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The Effect of Adding Zro Nanoparticles To Fe-18Al-15Cr Alloys With Mechanical Alloying Process For Oxidation Resistance

This document summarizes a study on the effect of adding ZrO2 nanoparticles to Fe-18Al-15Cr alloys produced using mechanical alloying for improved oxidation resistance at high temperatures. Intermetallic alloys like Fe3Al are promising high-temperature materials due to properties like high melting points, strength and oxidation resistance. The study produced Fe-18Al-15Cr alloy samples with 1%, 3% and 5% additions of ZrO2 nanoparticles via mechanical alloying. The samples were oxidized at 800-1000°C for 4 hours and analyzed. XRD analysis showed the formation of protective oxide layers including Cr2O3, Al2O3 and Fe2O3. The addition of Z

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0% found this document useful (0 votes)
25 views17 pages

The Effect of Adding Zro Nanoparticles To Fe-18Al-15Cr Alloys With Mechanical Alloying Process For Oxidation Resistance

This document summarizes a study on the effect of adding ZrO2 nanoparticles to Fe-18Al-15Cr alloys produced using mechanical alloying for improved oxidation resistance at high temperatures. Intermetallic alloys like Fe3Al are promising high-temperature materials due to properties like high melting points, strength and oxidation resistance. The study produced Fe-18Al-15Cr alloy samples with 1%, 3% and 5% additions of ZrO2 nanoparticles via mechanical alloying. The samples were oxidized at 800-1000°C for 4 hours and analyzed. XRD analysis showed the formation of protective oxide layers including Cr2O3, Al2O3 and Fe2O3. The addition of Z

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Fauzan Faried
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The Effect of Adding ZrO2 Nanoparticles to Fe-18Al-

15Cr Alloys with Mechanical Alloying Process for


Oxidation Resistance

Lolytah1, Djoko Hadi Prajitno2, Pawawoi3


{[email protected], [email protected] 2, [email protected]}

Universitas Jenderal Achmad Yani1, Badan Tenaga Nuklir Nasional2,


Universitas Jenderal Achmad Yani3

Abstract. The purpose of this study is to make a compatible material for the application
at high temperatures. Material that commonly used is superalloy but this material has low
melting point. One material that can replace superalloy material for the application at
high temperatures are intermetallic alloys and this alloys are very compatible to facing up
Industrial Revolution 4.0. The intermetallic alloys have several characteristics such as
high strength at high temperatures, high oxidation resistance, high melting points and low
densities. The specimens are made at this research are intermetallic alloys of Fe-18Al-
15Cr with variations in the addition of ZrO2 nanoparticles (1%, 3% and 5%). The process
of making specimens using one method of powder metallurgy. The process is
Mechanical Alloying (MA) which aims to reduce the particle size, increase homogeneity
and help to form new phases. In the high temperature oxidation process using a variable
temperature at 800°C, 900°C and 1000°C for 4 hours. The result of metallographic
testing showed the formation of the intermetallic phase Fe3Al. The result of XRD testing
showed the formation of oxide compounds on the surface of the specimen that are Cr2O3,
Al2O3 and Fe2O3. Addition of small amount of ZrO2 into the Fe-Al alloy is very effective
to enhance the oxidation resistance and hardness of the material.

Keywords: Fe3Al, Intermetallic, Mechanical Alloying, Oxidation, ZrO2 Nanoparticles,

1 Introduction

In the aircraft industry, there is an Aero gas turbine engine that has a exhaust system that
transmits turbine exhaust gases to the atmosphere at the speed, and in the direction needed, to
provide the thrust produced. The design of the exhaust system has a considerable influence on
jet engine performance. But, the exhaust system works if the combustion can works properly.
The combustion chamber has the difficult task of burning large quantities of fuel,
supplied through the fuel spray nozzles, with extensive volumes of air, supplied by the
compressor, and releasing the heat in such a manner that the air is expanded and accelerated to
give a smooth stream of uniformly heated gas at all conditions required by the turbine. This
task must be accomplished with the minimum loss in pressure and with the maximum heat
release for the limited space available.
The amount of fuel added to the air will depend upon the temperature rise required.
However, the maximum temperature is limited to within the range of 850 to 1700°C by the
materials from which the turbine blades and nozzles are made [1].

[Type here]
Fig. 1. An Early Combustion Chamber [1]

The air has already been heated to between 200 and 550°C by the work done during
compression, giving a temperature rise requirement of 650 to 1150°C from the combustion
process. Since the gas temperature required at the turbine varies with engine thrust, and in the
case of the turbo-propeller engine upon the power required, the combustion chamber must also
be capable of maintaining stable and efficient combustion over a wide range of engine
operating conditions. Therefore, it is necessary to use materials and forms of construction that
will withstand distortions and cracks, and prevent heat conduction in aircraft structures [1].

Fig. 2. Temperature, Axial Velocity and Total Pressure of Jet Engines [1]

The containing walls and internal parts of the combustion chamber must be capable of
resisting the very high gas temperature in the primary zone. In practice, this is achieved by
using the best heat resisting materials. The combustion chamber must also withstand corrosion
due to the products of the combustion [1].
The purpose of this study is to make a compatible material for the application at high
temperatures. High temperature material is a material that is able to maintain its properties or
does not decreasing it‘s quality at high temperatures and it‘s not easy to react with the
surrounding environment at high operating temperatures.
The type of material commonly used in high temperature operating environments is super
alloys. But this material has low melting point and it‘s quite expensive in terms of the material
and the manufacturing process so that further research is carried out to produce a new type of
material that is more efficient, the material is intermetallic alloy. Intermetallic alloys has high
strength characteristics at high temperatures, high resistant oxidation and corrosion, high
melting points and low density [2].

High temperature
Melting strength
point
Toughness

Ceramis
Super alloys

Intermetalics

Oxidation
resistance thermal Form ability
conductivity

Fig. 3. Comparison of Three Materials (Super Alloys, Intermetallic and Ceramic) [2]

Intermetallic alloys that are good for use at high temperatures are iron-aluminum alloys
(iron-aluminide) [3]. A material can be categorized as high temperature resistant if the
material is able to operate without protection at a temperature of 600°C continuously. In iron
and aluminum alloys, one of the phases formed is the Fe3Al phase. The intermetallic alloy
Fe3Al is a things that make the material can operating at high temperatures. The advantages of
using Fe-based are easy to get and cheap, low density, its durability increases with increasing
temperature and has excellent oxidation resistance [4]. Fe3Al-based intermetallic compounds
are a very promising alloy group for alternative steel substitutes in high temperature
applications and are open to future technology characterized with lower fuel consumption and
reduce environmental impact [5].
Fe-based if combined with Al will produces intermetallic Fe-Al alloys especially Fe3Al or
FeAl. The Fe-Al alloy is good if used at high temperatures because it has oxidation resistance
at high temperatures [6]. Fe3Al intermetallic compounds showed unique physical properties
and mechanical properties including high melting point (1540°C), high hardness (338 HV),
low density (6,72 g/cc) and have a good oxidation and corrosion resistance. Fe3Al retains the
corrosion by forming a Al2O3 layer on the surface [7].
In the intermetallic compound Fe-Al-Cr, Fe as a base metal, Al as an alloy that increases
toughness and tenacity and Cr (chromium) added to FeAl alloys can stabilizing the protective
layer Al2O3 and increase the hardness, strength, toughness and oxidation resistance properties
at high temperatures [2]. In addition ZrO2 has many advantages as nano alloys. These
advantages include having good corrosion resistance at temperatures above molten alumina
temperatures, stabilizing the protective layer of Al2O3, making a protective oxide thick layer
formed at high temperatures, increase hardness and reducing porosity [8].

2 Experimental Procedure

Elemental Fe (>99%), Al (>95%), Cr (>99%), ZrO2 (>99%) powders (Fe was supplied by
MERCK, Al by MERCK, Cr by MERCK and ZrO2 by Inframat Advanced
Material). The alloy of this study had a chemical composition of 67Fe-18Al-15Cr + % ZrO2
(1%, 3% and 5% ZrO2) (otherwise stated the composition is in weight percent). To obtain
chemical composition of the alloy, raw material proportion was set up as shown in Table 1,
Table 2 and Table 3.

Table 1. Calculation of Material Balance (67Fe-18Al-15Cr + 1%ZrO2)

Sample Vol Elements Vol ρ 5 pellets


Elements %wt Mass (gram)
(cm³) (cm³) (g/cm³) (gram)
Fe 67 0.285 0.191 7.860 1.501 7.505
Al 18 0.285 0.051 2.700 0.138 0.69
Cr 15 0.285 0.043 7.190 0.309 1.545
Sample Vol Element Vol ρ
Element %dopping Mass (gram) 5 pellets
(cm³) (cm³) (g/cm³)
ZrO2 1 0.285 0.003 5.680 0.017 0.085
Mass of each sample = 1.965 9.825

Table 2. Calculation of Material Balance (67Fe-18Al-15Cr + 3%ZrO2)

Sample Vol Elements Vol ρ 5 pellets


Elements %wt Mass (gram)
(cm³) (cm³) (g/cm³) (gram)
Fe 67 0.285 0.191 7.860 1.501 7.505
Al 18 0.285 0.051 2.700 0.138 0.69
Cr 15 0.285 0.043 7.190 0.309 1.545
Sample Vol Element Vol ρ
Element %dopping Mass (gram) 5 pellets
(cm³) (cm³) (g/cm³)
ZrO2 3 0.285 0.009 5.680 0.051 0.255
Mass of each sample = 1.999 9.995

Table 3. Calculation of Material Balance (67Fe-18Al-15Cr + 5%ZrO2)

Sample Vol Elements Vol ρ 5 pellets


Elements %wt Mass (gram)
(cm³) (cm³) (g/cm³) (gram)
Fe 67 0.285 0.191 7.860 1.501 7.505
Al 18 0.285 0.051 2.700 0.138 0.69
Cr 15 0.285 0.043 7.190 0.309 1.545
Sample Vol Element Vol ρ
Element %dopping Mass (gram) 5 pellets
(cm³) (cm³) (g/cm³)
ZrO2 5 0.285 0.014 5.680 0.080 0.4
Mass of each sample = 2.028 10.14
The alloy of this study were milled in a planetary ball mill. The milling operation was
performed at 1290 rpm for 3 hours. In all the experiments, nine hardened stainless steel balls
with a diameter of 10 mm and twenty hardened stainless steel balls with a diameter of 5 mm
were used with 9,8332 g powder mixture for alloy with 1% ZrO2; 10,0073 g powder mixture
for alloy with 3% ZrO2 and 10,1761 g powder mixture for alloy with 5% ZrO2 i.e. the ball-to-
powder weight ratio was 10:1.
The powders milled for 3 hours were compacted by a load of 100 Kg/mm2 to disks of 11
mm in diameter and 4,2 mm thickness. The milled powder was sintered in a sealed quartz
tubes evacuated for 2 hours at 1000°C. Sintering was performed in a Tube Furnace. After
sintering, the samples were cooled in the furnace to room temperature. Some samples are
oxidized and some are not oxidized. Non-oxidized samples must be characterized early.
Characterization that must be done consists of visual testing (measuring weight, height,
diameter), microscopy testing by optical, phase and compound testing by XRD and hardness
testing by Vickers.
Weighing and surface area measurement of each sample were carried out prior to
oxidation test. Isothermal oxidation tests were carried out by heating the samples at 800, 900
dan 1000°C for 4 hours in a tube heat resistance electric furnace. After oxidation, the samples
were cooled in the furnace to room temperature. Weighing of the oxidized samples was done
to obtain the weight change of each sample. The samples after oxidation must be characterized
by measuring height and diameter. Measuring the oxides thickness with an optical microscope
was used to determine oxidation resistance at high temperatures and the samples were tested
the hardness by indentation method using Zwick Hardness Vickers with a holding time of 10
seconds and the number of tests is 5 points.
To observe the microstructural changes during MA, the samples were polished to remove
any surface contamination and then etched in HNA solution (3,3 mL CH3COOH + 3,3 mL
HNO3 + 0,1 mL HF + 93,3 mL H2O) with the immersion method for 5-8 seconds.
Microstructure observation was carried out using an Olympus BX60M optical microscope
with 1000x (20m) magnification. The microstructural morphology of the compacted samples
was characterized by SEM. The phase and compound testing after oxidation process was
characterized by EDS.
Phase changes that occurred in the powders during milling and oxidation were
investigated by X-ray diffraction using Philips Analytical PC-APD with a CuK_ radiation (_ =
0.1542 nm). The step size and step time were 0.05◦ and 1 s/step, respectively. The lattice
parameter, long-range order parameter, crystallite size and lattice strain were calculated from
the XRD data.

3 Results and Discussion

3.1 Visual testing, weight gain formula and weight gain data

Visual testing. Samples weight before and after oxidation is weighed and measurements the
height and diameter from the samples using calipers and analytic balance.

Weight gain formula. Calculate the ∆weight of the oxidation samples before calculating the
weight gain with a formula like the following:

∆W = weight after oxidation – weight before oxidation = gram (1)


After ∆weight is obtained, calculate the surface area (Sa) of the samples with a formula
like the following:

Sa = 2Πr(t+r) = mm2 (2)

After the two things above have been obtained, then the weight gain can be calculated by
a formula like the following:

Weight gain = = gr/mm2 (3)

Weight gain data. The following data are weight gain datas from oxidation samples that show
weight before oxidation and weight after oxidation shown in Table 4.

Table 4. Dimension and Weight Observation Data Before and After Oxidation

Weight Weight
Radius Height Surface
Oxidation Before After ∆W Weight Gain
%ZrO2 (r) (t) Area
Temperature Oxidation Oxidation
(gram) (gram) (gram) mm mm mm² gram/mm²
1 2.0925 2.1153 0.0228 5.5 4.2 335.038 0.0000680520
3 800°C 2.0986 2.1612 0.0626 5.5 4.2 335.038 0.0001868445
5 2.1442 2.1895 0.0453 5.5 4.2 335.038 0.0001352085
1 2.0886 2.1239 0.0353 5.5 4.2 335.038 0.0001053612
3 900°C 2.0451 2.1685 0.1234 5.5 4.2 335.038 0.0003683164
5 2.1340 2.1894 0.0554 5.5 4.2 335.038 0.0001653544
1 2.0671 2.1175 0.0504 5.5 4.2 335.038 0.0001504307
3 1000°C 2.0821 2.2345 0.1524 5.5 4.2 335.038 0.0004548738
5 2.1013 2.1645 0.0632 5.5 4.2 335.038 0.0001886353

From the table of data above, it shows that there is a change in weight, the weight
increases after being oxidized. To clarify weight gain from all 9 samples, a weight gain curve
was made:

Weight Gain Measurement Results


WEIGHT GAIN
(GRAM/MM²)

0.0005300000
0.0004300000
0.0003300000
0.0002300000
0.0001300000
0.0000300000
1% ZrO2 3% ZrO2 5% ZrO2
800°C 0.0000680520 0.0001868445 0.0001352085
900°C 0.0001053612 0.0003683164 0.0001653544
1000°C 0.0001504307 0.0004548738 0.0001886353

Fig. 4. Weight Gain Measurement Results Curve of All 9 Samples


3.2 Microstructure and phase formed

Microstructure. The figure below is a micro-structure of Fe-18Al-15Cr alloy which added


ZrO2 nanoparticles before and after oxidation with oxidation temperature according to the
image below. Photographs of microstructure were carried out on the top surface of the sample
for non-oxidized samples and in cross sections for oxidized samples.

(a) (b)
Fig. 5. Microstructures of Fe-18Al-15Cr + 1% ZrO2 Alloy (a) and Fe-18Al-15Cr + 3% ZrO2 Alloy (b)

Fig. 6. Microstructures of Fe-18Al-15Cr + 5% ZrO2 Alloy


Phase formed. The phase formed consists of αCr, FeAl and Fe3Al and presence of porosity
between phases. The shape of αCr in the micro structure is square and there is a round with
white color and large in size. Porosity is marked in black color and it is located between
grains. The FeAl and Fe3Al phases are gray and their shape is like a cloud between αCr which
is round white or square white [9]. In the 9 test samples with variations in oxidation
temperature and the addition of ZrO2 nanoparticles, the difference was in the form of grain
changes in the microstructure. Oxidation temperature at 800ᴼC shows the sample has a fine
grain shape but at a higher oxidation temperature, the grain size tends to more increase.
Oxidation temperature at 1000ᴼC shows the sample has a coarse grains when adding just
a little ZrO2 nanoparticles that means the more ZrO2 added will make the grains of
microstructure more refined.

3.3 Hardness

Hardness. The Vickers hardness testing was carried out on 12 samples using 500 grams of
load with diamond pyramid identor. Vickers hardness testing is carried out on the top surface
of the sample for non-oxidized samples and on the cross section for oxidized samples. The
following data are hardness testing results on 12 samples (Fe-18Al-15Cr + variation of
%ZrO2) before and after oxidation process shown in Table 5.

Table 5. Hardness Vickers Number of All Samples

Oxidation Hardness (HVN)


Sample %ZrO2
Temperature 1 2 3 4 5 Average
1 1 225.00 230.00 228.00 205.00 205.00 218.60
2 3 Non-Oxy 225.00 227.00 223.00 221.00 215.00 222.20
3 5 260.00 229.00 228.00 225.00 220.00 232.40
4 1 185.00 180.00 182.00 180.00 180.00 181.40
5 3 800°C 188.00 211.00 184.00 208.00 191.00 196.40
6 5 202.00 194.00 218.00 188.00 188.00 198.00
7 1 203.00 204.00 201.00 203.00 194.00 201.00
8 3 900°C 184.00 211.00 211.00 215.00 190.00 202.20
9 5 193.00 209.00 203.00 205.00 208.00 203.60
10 1 203.00 215.00 193.00 220.00 209.00 208.00
11 3 1000°C 220.00 201.00 201.00 215.00 215.00 210.40
12 5 215.00 218.00 229.00 215.00 203.00 216.00

Based on the data obtained from the table above, it can be seen that the effect of adding
ZrO2 nanoparticles to the alloy of Fe-18Al-15Cr powder has the highest average hardness
value of 232.40 HVN. Hardness increases with increasing ZrO2 as a dopping and increasing
the oxidation temperature. This is analogous with the concept where in addition ZrO2 has
many advantages as nano alloys one of which is increasing the hardness number [8]. To
clarify the hardness number from all 12 samples, a hardness results curve was made:
Fig. 7. Hardness Comparison Curve of Unoxidized and Oxidized Samples at 800°C, 900°C, 1000°C with
Variations of ZrO2 (1%, 3% and 5%)

3.4 Oxidation Thickness

Oxidation thickness. The figure below is a micro-structure of Fe-18Al-15Cr alloy which


added ZrO2 nanoparticles after oxidation with oxidation temperature according to the image
below. Photographs of microstructure were carried out at cross sections.

(a) (b)
Fig. 8. Oxidation Thickness of Fe-18Al-15Cr (a) adding 1% ZrO2 (b) adding 3% ZrO2
Fig. 9. Oxidation Thickness of Fe-18Al-15Cr + 5% ZrO2 Alloy

The following data are oxide thickness measurement results on 9 samples (Fe-18Al-15Cr
+ variation of %ZrO2) after oxidation process shown in Table 6.

Table 6. Oxide Thickness Measurement Data

Oxidation Oxidation Thickness (m)


Sample %ZrO2
Temperature 1 2 3 4 5 Average
1 1 4.70 6.83 7.69 6.41 7.69 6.66
2 3 800°C 16.66 23.50 17.52 12.82 17.94 17.69
3 5 9.82 8.11 15.38 13.24 14.52 12.21
4 1 8.97 8.97 11.11 10.25 14.95 10.85
5 3 900°C 46.15 32.47 37.17 28.63 46.58 38.20
6 5 14.52 12.82 16.23 16.23 18.80 15.72
7 1 11.96 17.09 12.39 14.10 13.24 13.76
8 3 1000°C 45.29 38.46 46.58 38.88 56.83 45.21
9 5 13.67 21.79 24.78 16.66 9.82 17.34

Based on the data obtained from the table above, it can be seen that the effect of adding
ZrO2 nanoparticles to the alloy of Fe-18Al-15Cr powder has the highest average oxide
thickness value of 45.21 m. Oxides thickness increases with increasing the oxidation
temperature. Oxide thickness can determine the oxidation resistance of a material where the
thicker the oxide layer means the oxidation resistance of a material is low. From the data table
above, it can be seen that the oxidation resistance of the material decreases when added ZrO2
nanoparticles as much as 3% but when added as much as 5% the oxidation resistance
increases. This is because the addition of 3% ZrO2 has not been effective against the oxidation
resistance value of the material but will be very effective if the addition is as much as 5% ZrO2
which will increase the oxidation resistance.
The oxidation thickness data obtained is proportional to the weight gain value after the
oxidation process. This is analogous with the concept where the higher the weight gain value
the thicker the oxide thickness shown in Table 4. To clarify the oxidation thickness value from
all 9 samples, a oxide thickness measurement results curve was made:

Measurement of Oxidation Thickness Results


50.00
OXIDE THICKNESS (M)

45.00
40.00
35.00
30.00
25.00
20.00
15.00
10.00
5.00
0.00
1% ZrO2 3% ZrO2 5% ZrO2
800°C 6.66 17.69 12.21
900°C 10.85 38.20 15.72
1000°C 13.76 45.21 17.34

Fig. 10. Oxide Thickness Comparison Curve of Oxidized Samples at 800°C, 900°C, 1000°C with
Variations of ZrO2 (1%, 3% and 5%)

3.4 XRD and SEM-EDS Results

XRD. XRD testing was carried out on the surface of the sample to determine the compounds
formed in Fe-18Al-15Cr + %ZrO2 (1%, 3% and 5%) samples after oxidation which oxidation
for 4 hours at 1000°C. The XRD analysis results, shown in Figure 11, confirmed that oxides of
Fe2O3, Cr2O3 and Al2O3 were detected in all sample surfaces. It is believed that the outer parts
of the scale was dominated by iron oxide of Fe2O3. Iron oxides such as Fe2O3 begin to form at
temperatures around 570°C [3]. But the Fe2O3 oxide layer has properties not as a protective
layer. Iron oxide of Fe2O3 is believed to be formed at the first stage of oxidation at all
temperatures studied [10, 11], as the alloy rich in iron, even though these oxide are
thermodynamically less stable compared with Al2O3 and Cr2O3. With time, underneath iron
oxides depleted in Fe and consequently enrich the Al and Cr [10]. Enrichment of Cr in this
region would drive formation of Cr2O3. However, Cr2O3 is less stable than Al2O3.Therefore,
Al2O3 would form immediately bellow iron oxides scale [10]. Formation of this aluminium
oxide reduced inward diffusion of oxygen to the alloy surface as the Fen+ ions have larger size
compared with other anions [11], making the outward diffusion of iron ions to the oxygen rich
regions decrease. The growth of Al2O3 layer caused depletion aluminium content in the alloy
below the scale [12]. Consequently, as the Cr content increased, Cr2O3 would form. Formation
of reduces the possibility of iron oxides to form further [12]. Addition of Cr elements will
increase oxidation resistance and ductility properties of Fe3Al phase. In the formation of
protective layer Cr2O3, Cr will play a role in reducing O2 flux and reducing internal oxidation
and accelerating the growth of Al2O3 layers under the Cr2O3 layer [11]. The scale mainly
consist out of Fe2O3, Cr2O3 and Al2O3 with small amounts of ZrO2 scattered on the surface
[13], this makes the position of the ZrO2 peak in XRD patterns coincide with the major oxide
layer Fe2O3.

Fig. 11. XRD Patterns for Fe-18Al-15Cr + %ZrO2 (1%, 3% and 5%) Oxidation at 1000°C for 4 Hours

SEM-EDS. SEM-EDS testing, shown in Figure 12-13, was carried out on the cross sections of
the samples to determine percentage of Fe, Al, Cr, Zr and O elements in Fe-18Al-15Cr +
%ZrO2 (1% and 5%) samples after oxidation which oxidation at 900°C for 4 hours. EDS
testing was carried out at the results of SEM micrograph with overall mapping to determine
the percentage of the elements observation per position to see the distribution of elements to
oxides and substrates of the samples, shown in Figure 14-15. The percentage of Zr in all
points or positions has a stabil value according to the magnitude of the addition of ZrO2 at the
beginning of alloying. Al elements basically reacts with oxygen to form a protective layer of
Al2O3 on the surface [7] while Cr (chromium) and ZrO2 added to Fe Alloys can stabilize the
protective layer Al2O3 [2, 8]. This is the reason why the percentage of oxygen is higher on the
surface than in the middle of the sample because Al and Cr reacts with O2 to produce a
protective oxide layer on the surface. This also makes the percentage of Al and Cr higher on
the surface than in the middle of the sample. The things above make the Fe element on the
surface of the sample less than in the middle of the sample.

(1) (2) (3)

3
Fig. 12. SEM-EDS Micrograph For Fe-18Al-15Cr + 1% ZrO2 Which Oxidation For 4 Hours At 9000C
With 2000x Magnification (Positions 1 To 3 Are From The Area Near The Surface To The Middle Of
The Sample)

(1) (2) (3)

3
Fig. 13. SEM-EDS Micrograph For Fe-18Al-15Cr + 5% ZrO2 Which Oxidation For 4 Hours At 9000C
With 2000x Magnification (Positions 1 To 3 Are From The Area Near The Surface To The Middle Of
The Sample)

Fig. 14. Distribution Curve of Elements to Oxides and Substrates (Fe-18Al-15Cr + 1% ZrO2 Oxidation
at 900°C for 4 Hours)
Fig. 15. Distribution Curve of Elements to Oxides and Substrates (Fe-18Al-15Cr + 5% ZrO2 Oxidation
at 900°C for 4 Hours)

4 Conclusion

The oxidation behaviour of Fe–18Al–15Cr + %ZrO2 (1%, 3% and 5%) alloys designed for
applications at high temperatures has been evaluated between 800, 900 and 1000°C. While all
three alloys showed a very good oxidation resistance at 800°C, which compared favourably to
those of other Fe3Al-based alloys, they show increasing weight gains and oxide thickness at
higher temperatures due to ingress of the oxidation into the sample. Scale formed on the
surface of the samples consisted of oxides of Fe2O3, Al2O3 and Cr2O3 but dominated by Fe2O3.
For the investigated alloys has beneficial effect from alloying the samples with 5 wt% ZrO2.
Addition of 3% ZrO2 make a phenomenon of decreasing oxidation resistance that make the
addition of ZrO2 becomes ineffective. The addition of ZrO2 made oxidation resistance increase
when added 5% ZrO2. Addition of small amount of ZrO2 into the Fe-Al alloy has only
insignificant effect on the mechanical properties, but it is worth to notice, that the addition of 5
wt% ZrO2 is very effective to enhance the oxidation resistance and hardness of the material.
Hardness increases with increasing oxidation temperature and %wt ZrO2 as a doping. Oxide
layer stability of Al2O3 is increased in Fe–18Al–15Cr + %wt ZrO2 (1%, 3% and 5%) alloys.
Because the compound element in the form of zirconium has dissolved in the Fe matrix. Non-
oxidized samples have phase formed consists of αCr, FeAl and Fe3Al and presence of porosity
between phases. Fe3Al intermetallic compounds showed unique physical properties and
mechanical properties including high melting point and have a good oxidation and corrosion
resistance [7] this is what makes it become a high temperature oxidation resistant material.
Acknowledgments
The authors gratefully acknowledge the support of National Nuclear Energy Agency of
Indonesia (BATAN) and Degree Program of Metallurgical engineering, Jenderal Achmad
Yani University Bandung Indonesia (UNJANI) for the research facilities. The first author
would like to thank Mr Dr. Ir. Djoko Hadi Prajitno, MSME and Mr Pawawoi, ST. MT who
supported the powders and for the help and valuable advice.

References
[1] Rolls Royce, “Rolls Royce - The Jet Engine,” The Jet Engine. 1996.
[2] E. A. Basuki, Paduan Logam Untuk Aplikasi Temperatur Tinggi Dan Penghematan Energi.
Bandung: ITB, 2016.
[3] G. S. Upadhyaya, “Powder Metallurgy Technology,” Cambridge Int. Sci. Publ., 2014, doi:
10.1073/pnas.0703993104.
[4] J. R. Davis, “ASM Specialty Handbook: Heat-Resistant Materials,” in ASM Specialty
Handbook: Heat-Resistant Materials, 1997.
[5] E. Airiskallio et al., “High temperature oxidation of Fe-Al and Fe-Cr-Al alloys: The role of Cr
as a chemically active element,” Corros. Sci., 2010, doi: 10.1016/j.corsci.2010.06.019.
[6] S. E. Haghighi, K. Janghorban, and S. Izadi, “Structural evolution of Fe-50 at.% Al powders
during mechanical alloying and subsequent annealing processes,” J. Alloys Compd., 2010, doi:
10.1016/j.jallcom.2010.01.145.
[7] Z. B. Jiao, J. H. Luan, M. K. Miller, C. Y. Yu, and C. T. Liu, “Group precipitation and age
hardening of nanostructured Fe-based alloys with ultra-high strengths,” Sci. Rep., 2016, doi:
10.1038/srep21364.
[8] J. M. A. Hotařa, P.Kejzlara, M.Palmb, “The Effect of Zr on High-Temperature Oxidation
Behaviour of Fe3Al-Based Alloys,” Corros. Sci., vol. 100, pp. 147–157, 2015, doi:
10.1016/j.corsci.2015.07.016.
[9] M. Mhadhbi, J. J. Suñolb, and M. Khitouni, “Influence of heat treatments on the structure of
FeAl powders mixture obtained by mechanical alloying,” in Physics Procedia, 2013, doi:
10.1016/j.phpro.2012.12.005.
[10] E. A. Basuki, D. C. Nababan, F. Muhammad, A. A. Korda, and D. H. Prajitno, “Isothermal
Oxidation Behaviour of 69.5Fe-14Ni-9Al-7.5Cr Alloy at High Temperatures,” Int. J. Corros.,
2019, doi: 10.1155/2019/8517648.
[11] P. Kofstad, High Temperature Corrosion in Materials at High Temperatures Corrosion and
Anti-Corrosives. New York, USA: Elsevier Applied Science Publishers Ltd, 1988.
[12] N. K. Othman, N. Othman, J. Zhang, and D. J. Young, “Effects of water vapour on isothermal
oxidation of chromia-forming alloys in Ar/O2 and Ar/H2 atmospheres,” Corros. Sci., 2009, doi:
10.1016/j.corsci.2009.08.032.
[13] A. Hotař, M. Palm, P. Kratochvíl, V. Vodičková, and S. Daniš, “High-temperature oxidation
behaviour of Zr alloyed Fe 3Al-type iron aluminide,” Corros. Sci., 2012, doi:
10.1016/j.corsci.2012.05.027.

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