MINI RESEARCH (MR)
SOLID STATE PHHYSICS
“X-RAY DIFFRACTION ANALYSIS OF STEEL AND CRYSTAL LaMnO”
NAME OF GROUP 3 : 1. CHAIRIN GHILLANDA (4202421018)
2. FADHILLA ANANDA (4203121054)
3. PUTRI AMALIA (4201121004)
4. TIARA SYAHDILA (4202121002)
LECTURER : Prof. Dr. MAKMUR SIRAIT, M.Si
BILINGUAL PHYSICS 2020
FACULTY OF MATH AND SCIENCE
MEDAN STATE UNIVERSITY
2023
PREFACE
Thanks be to God Almighty for His mercy and grace so that we can finish the paper
about x-ray diffraction analysis of steel and crystal LaMnO well despite the many flaws in it.
And also we thank to Prof. Dr. Makmur Sirait, M.Si as the lecturer in solid state physics subject
who gave this assignment to us.
Hopefully this paper can be useful in order to increase our insight and knowledge. We
are also fully aware that this paper has flaws and is far from perfect. Therefore, we hope that
there are criticisms and suggestions for improving the papers that we will make in the future,
considering that nothing is perfect without constructive suggestions.
Hopefully this paper can be understood by anyone who reads it. We hope that the report
prepared will be of use to us and for those who read it. Previously, we apologize if there are
errors in words that are not pleasing and we ask for constructive criticism and suggestions for
future improvements to this paper.
Medan, 20 May 2023
Group 3
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TABLE OF CONTENTS
PREFACE ................................................................................................................................... i
TABLE OF CONTENTS ...........................................................................................................ii
CHAPTER I ............................................................................................................................... 3
INTRODUCTION ..................................................................................................................... 3
1.1 Background ...................................................................................................................... 3
1.2 Formulation of the Problem ............................................................................................. 4
CHAPTER II.............................................................................................................................. 5
CONCEPTS AND HYPOTHESES ........................................................................................... 5
CHAPTER III ............................................................................................................................ 6
TECHNIQUES AND DATA COLLECTION........................................................................... 6
3.1 RESEARCH METHODS ............................................................................................ 6
3.2 RESEARCH TIME AND PLACE .............................................................................. 6
3.3. RESEARCH SUBJECT .............................................................................................. 6
3.4 DATA ANALYSIS TECHNIQUE ............................................................................. 7
CHAPTER IV ............................................................................................................................ 8
DATA ANALYSIS .................................................................................................................... 8
CHAPTER V ........................................................................................................................... 16
CLOSING ................................................................................................................................ 16
5.1 Conclusion ...................................................................................................................... 16
5.2 Suggestion ...................................................................................................................... 16
REFERENCES ........................................................................................................................ 17
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CHAPTER I
INTRODUCTION
1.1 Background
The development of Science and Technology today encourages a more detailed
understanding and use of X-rays. In 1895 Wilhelm Roentgen discovered X-rays which are
high-energy photons with a wavelength of the order . Since that discovery, research and
understanding of X-rays has continued to develop until now, one of its applications in the field
of life is X-Ray Diffraction (XRD) which is then widely used as a method for analyzing the
crystal structure of solids (Wiyatno, Yusman, 2003).
X-rays that interact with matter will experience optical phenomena such as scattering,
diffraction, reflection, and transmission. If the material has a crystalline structure, then X-rays
hitting the crystal planes will be diffracted or scattered at a certain scattering angle and will
provide direct information in the form of scattering angle (2θ), intensity (I) and distance
between atomic planes (dhkl). By knowing the distance between the atomic planes, it can then
be used to calculate the values of the Miller index (hkl) and the lattice parameters. Every
material in nature that has a crystalline structure has a certain crystal structure, meaning that it
has certain planes, distances between planes, and lattice parameters. Thus X-ray diffraction
technique can be used for the detection of elements or compounds contained in a compound.
The crystal structure of a material is closely related to the properties of the material, such as
optical, mechanical, electrical, and thermal properties. By knowing the crystal structure of a
material, indirectly the properties of the material can also be known, so X-ray diffraction
technique is a very important technique todetermine the type of material and its properties. In
this study, the authors tried to analyze the accuracy of crystal structure analysis (solids) using
X-ray analysis. In this mini research, there are two journals used or analyzed, namely journal
I entitled Analysis of X- Ray Diffraction in Austenitic and Ferritic Stainless Steels and journal
II entitled Crystal Structure Analysis By knowing the crystal structure of a material, indirectly
the properties of the material can also be known, so X-ray diffraction technique is a very
important technique to determine the type of material and its properties. In this study, the
authorstried to analyze the accuracy of crystal structure analysis (solids) using X-ray analysis.
In this mini research, there are two journals used or analyzed, namely journal I entitled Analysis
of X-Ray Diffraction in Austenitic and Ferritic Stainless Steels and journal II entitled Crystal
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Structure Analysis By knowing the crystal structure of a material, indirectly the properties
of the material can also be known, so X-ray diffraction techniqueis a very important technique
to determine the type of material and its properties. In this study, the authors tried to analyze
the accuracy of crystal structure analysis (solids) using X-ray analysis. In this mini research,
there are two journals used or analyzed, namely journal I entitled Analysis of X-Ray
Diffraction in Austenitic and Ferritic Stainless Steels and journal II entitled Crystal Structure
Analysis In this study, the authors tried to analyze the accuracy of crystal structure analysis
(solids) using X-ray analysis. In this mini research, there are two journals used or analyzed,
namely journal I entitled Analysis of X- Ray Diffraction in Austenitic and Ferritic Stainless
Steels and journal II entitled Crystal Structure Analysis In this study, the authors tried to
analyze the accuracy of crystalstructure analysis (solids) using X-ray analysis. In this mini
research, there are two journalsused or analyzed, namely journal I entitled Analysis of X-Ray
Diffraction in Austenitic andFerritic Stainless Steels and journal II entitled Crystal Structure
Analysis LaMnO3 With X-Ray Diffraction Technique And Rietveld Method.
1.2 Formulation of the Problem
The formulation of the problem from this mini research is:
1. How the diffraction patterns that arise in austenitic and ferritic stainless steels have been
successfully analyzed by X-ray diffraction techniques
2. How has the crystal structure of LaMnO3 been successfully analyzed using the Rietveld
method of X-ray diffraction?
3. How is the accuracy level of crystal structure analysis using X-ray diffractiontechnique from
the results of the analyzed journal research?
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CHAPTER II
CONCEPTS AND HYPOTHESES
Austenitic stainless steels are non-magnetic and have an FCC crystalline structureand
can transform to BCC at or below room temperature due to plastic deformation. metastable
which can return to phase when annealed at a temperature of 400-800 oC5. On the other hand,
ferritic stainless steel is magnetic and has a BCC crystalstructure so that it is more difficult to
slip than the FCC crystal structure.
The testing procedure is as follows:
1. Estimating the diffraction angle
The diffraction angle that will appear from the test object is estimated in advance
based on the main components in stainless steel (Fe)dancelight x
monochromatic Cu
2. Preparation of the test object
Powdered austenitic stainless steel and ferritic stainless steel are made by filing a test
object that is still a plate. Each powder obtained was mixed with vaseline and placed
on the test object plague, then mounted on a diffractometer.
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CHAPTER III
TECHNIQUES AND DATA COLLECTION
3.1 RESEARCH METHODS
The research method used is a quantitative approach with descriptive and evaluative
methods. The descriptive method used in this research is to take two journals containing research
on crystal analysis using x-rays to collect and present data about the conditions of crystal analysis.
The evaluative method was used to evaluate the research data obtained from the results of crystal
analysis research in the two journals that had been taken. The resulting data are observations using
the x-ray diffraction method in two journals. The resulting data is in the form of research results
from observations of two journals which then obtained measurement results figures and research
data from two journals with two compounds, namely Iron and LaMnO3 with the x-ray diffraction
method. After the data was collected, the measurement data and research data from two journals
with two compounds namely Iron and LaMnO3 with the x-ray diffraction method were analyzed,
which were then compared with existing standards and criteria. Then after that, the results of the
analysis are evaluated to determine the extent of the results of the crystal analysis.
3.2 RESEARCH TIME AND PLACE
This research was conducted on Sunday at 18.00 in the house of each student.
3.3. RESEARCH SUBJECT
The research subjects of this mini research are having two subjects, namely:
1. Journal with the title, "Analysis of LaMnO3 Crystal Structure with X-Ray Diffraction
Technique and Rietveld Method".
2. Journal with the title, "X-Ray Diffraction Analysis with Austenitic and Ferritic Stainless
Steels".
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3.4 DATA ANALYSIS TECHNIQUE
Data collection techniques in this mini research are carried out by:
1. Looking for two journals on crystal analysis using the x-ray diffraction method
2. The crystalline compounds sought in the two journals must be different but both use the X-
ray diffraction method. This aims to make a comparison of the first journal analysis with
LaMnO3 and Iron compounds.
3. Then the researchers conducted research on both journals, by looking at the resultsof the
discussion in the first journal and the second journal.
4. The researcher concludes the research results obtained from the two journals and then the
results are compared.
5. Researchers make reports on research results.
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CHAPTER IV
DATA ANALYSIS
The X-ray diffraction pattern as a result of the analysis is shown in Figure 2. It can
be seen in the figure that the observed profile is indicated by data points and the calculated
profile is represented by a malar line; short vertical lines indicate the positions of the
Bragg peaks, the first and second rows (Fig. 2b), for the positions of the Bragg peaks of the
Pnma phase and the R3c phase, respectively. Below the short vertical lines is the deviation
profile between the observed and calculated intensity prices.
Refinement of the X-ray diffraction pattern of the LaMnO3 sample was carried out,
first assuming that the crystal structure of the sample corresponds to the R3c phase (Model
1), second assuming that the sample consists of a mixture of Pnma+R3c phases (Model 2);
and thirdly by assuming that the sample contains only the Pnma phase (Model 3). Crystal
structure parameter input refers to the results of previous studies [7].
The first step (iteration-1), smoothing the background count parameters (b0, b1, b9)
and the scale factor (s). In iteration-2, the FWHM parameters (U, V, W) and Lorentzian
factors (X, Y) were refined. The lattice parameters (a, b, c) are smoothed in iteration-3. Then
in iteration-4, smoothing the scale factor (s) and preferred orientation factor (p), then in
iteration-5, smoothing the occupancy factor parameter (g), atomic coordinate fraction (x, y,
z) and temperature parameter (B) . Simultaneous iteration as a whole is carried out starting
from iteration-6. The final results of refinement are shown in Table 1.
During the calculation process, several atomic occupancy factor values of g>1.0 were
found, so the parameter was fixed at 1.0; means the point where the atom (site) is filled
(occupied) completely (100%). So, the value of g> 1.0 has no physical meaning. The value
of g for the oxygen atom in the R3c phase, Model 2, is greater than 1.0. However, when g is
assigned a fixed number of 1.0, the iteration stops. In the refinement, it was also found that
the value of the temperature parameter B was negative, namely B for the oxygen atom in
the R3c phase, Model 2; actually the negative temperature parameter also has no physical
meaning. The existence of data that has no physical meaning is an indication that the
assumption of the Model 2 structure is not correct.
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It can be seen in Table 1 that all the crystal structure parameters in Model 1 and
Model 3 have normal values. However, Model 3 has a better fitting quality, characterized
by a smaller S factor price (1.42) compared to the S Model 1 factor (1.59).Besides, it can
be seen in Figure 2(c) that Model 3 displays the best fitting quality, where the
calculated profile coincides with the observed profile. And therefore, the deviation profile
of the calculated-observation intensity almost resembles a straight line. This means that
the phase formed in the samples synthesized by the high energy milling method in this
study is single-phase LaMnO3+d where d = 0.000, has an orthorhombic crystal structure
with Pnma No space group. 62 with the structural parameters as shown in Table 1. Valence
of La and O in LaMnO3, The 0s are +3, and -2, respectively. Therefore the valence of the
Mn ions is +3.
The electron configuration of a neutral Mn atom is 4S23d5, this means that Mn+3
has 4 electrons in the d shell. So the configuration of the Mn+3 ion in LaMnO3,0 is 4S23d
4. These four electrons in the d shell will determine the electrical and magnetic properties
of this material. Based on the crystal field theory, the 3d orbital of manganese splits into
five orbitals, namely degenerate three, t2g and degenerate two, tg and according to Hund's
rule, all spins of Mn+3 have the same direction to minimize the repulsive force Coulomb,
as shown in Figure 3.
Based on previous research, it was shown that there was a relationship between
strain and the electric magnetic properties of LaMnO3+ [8]. Therefore, in this study,
measurements of lattice strain were carried out to determine the electric-magnetic
properties of LaMnO3+ . The lattice strain is determined by Hall's equation [10]:
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cos / =2 .sin /+0.9/D(2)...............................
The data of the reflection plane (hkl), Bragg angle (2), distance between crystal
planes (d), observed intensity (IO), calculated intensity (IC) and the half-width of the
maximum peak height ( ) from the Rietveld analysis are shown in Table 2. Based on the
data in the table, a graph of the relationship between the parameter .cos / and sin is
made, the results are shown
Table. Crystal structure parameters and reliability indices Rwp, Rp, S, RF and RI in
Model 1, Model 2, and Model 3 of LaMnO3+ samples refined using X-ray diffraction
technique Rietveld method. The number in brackets is the precision applied to the last digit
after the comma.
Parameter Model-1 Model-2 Model-3
smoothing
R3c PnmaR3c Pnma
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RI 21.46 24.09 25,72 17.57
RF 13.82 17.11 15.90 16.69
Weight fraction
(%)100 82.82 17.18 100
In Figure 3. Next, with the help of the EXCEL program, the equation of the line: y
= -0.0104x + 0.005 is plotted. Thus, the lattice strain, e = -0.5% and the crystallite size of
LaMnO3+d is D = 17 nm. Thus LaMnO3.0 crystals undergo compressive strain andaccording
to Nanda [8], LaMnO3.0 behaves as an insulating material, antiferromagnetic type G.
The event that occurs in high energy milling is a ball-assault collision. Assault particles
are framed on the colliding tar abol ab o la baja. Furthermore, the powders undergo a fracture
process, so that the size of the constituent oxide grains decreases. Furthermore, when the
constituent oxide grains are pelleted and sintered, a solid reaction occurs to form a new phase,
namely the LaMnO3 phase. The lattice strain in LaMnO3 is
Table 2. Reflection plane data (hkl), Bragg angle (2 ), distance between crystal planes
(d), observed intensity (IO), calculated intensity (IC) and the width of half the maximum
peak height ( ) Rietveld analysis results from the sample LaMnO3+
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23.02 0.321
2. 020 8 3.8589 1,135 1,383 7
32.30 0.267
3. 002 9 2.7685 11.09810.806 2
32.69 0.265
4. 121 9 2.7363 100,00097,653 1
32.89 0.264
5. 200 8 2.7202 11.11710.873 0
40.04 0.228
6. 022 9 2.2495 12,53213,099 5
40.54 0.226
7. 220 0 2.2233 12.98214.003 3
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compressive strain. Thus, LaMnO3.0 crystals experience compressive strain, this isin
accordance with the results of previous studies, where it was found that the lattice parameters a
and c in the LaMnO3 unit cell display negative temperature expansion. MR measurements of
samples as a function of the external magnetic field H were carried out in the range of -7.6 kOe
to +7.6 kOe. The results of the MR measurement as a function of the external magnetic field on
LaMnO3 are shown in Figure 4. It can be seen in the figure that the sample shows negative MR
properties. A material is said to have positive/negative MR properties when the resistance of the
material increases/shrinks when exposed to an external magnetic field. The MR value at
LaMnO3.0 is 7%. Meanwhile, the MR response of CMR materials (ie R1-xAxMnO3) can reach
100,000% at temperatures around the Curie temperature (Tc = 200 K to 220K) [1]. MR response
value on LaMnO3.0 is very small compared to MR on CMR. When a CMR material is subjected
to amagnetic field at a temperature around Tc.
Then there is a phase transition from insulator-paramagnetic to conductor-
ferromagnetic. This phase transition is accompanied by a very sharp reduction in resistance. This
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is because the material that was originally an insulator has turned into a metal, so the change in
resistance of the material is very large, the material which was originally in a state of random
spin direction (paramagnetic) changes to a state of regular spin direction (ferromagnetic). The
spin disorder causes charge carriers with different spin orientations to scatter each other, thereby
increasing the electrical resistance. When a magnetic field is applied to the material, the electron
spins are directed. Thus the scatteringof charge carriers by spin irregularity no longer occurs, so
the electrical resistance decreases. Therefore the shrinkage of the total electrical resistance
becomes very large.
In the case of LaMnO3,0, the MR measurement is carried out at room temperature, where
at that temperature the material is an insulator or semiconductor, even though it is subjected to a
magnetic field. So the change in electrical resistance when subjected to anexternal magnetic field,
is only due to a change in the state of the spin direction of the electron, from a random state to a
regular state. Therefore the change in resistance of the material to the magnetic field, MR is
small. The emergence of magnetic interactions between electrons is explained by a theory called
exchange interaction. The relative directions of the two interacting spins (S1 and S2) cannot be
changed except by changing the spatial charge distribution. As a result there is a direct coupling
between the spin directions and there is an interaction energy between the spin vectors whose
magnitude is proportional to S1 dot S2.
To understand the phenomenon of exchange interactions in La+3Mn+3O3, suppose two
Mn+3 ions are separated by an oxygen anion as shown in Figure 6. The first Mn+3 ion and the
eg electron are labeled A and A1 respectively. The second Mn+3 ion and the eg electron are
labeled B and B1 respectively. The electron spins of oxygen close to A and B are labeled O1 and
O2, respectively. Since the exchange interaction between the manganese and oxygen atoms is
negative, the spin of oxygen O1 is anti-parallel to A1 and the spin of oxygen O2 is anti-parallel
to the spin of oxygen O1. Also because of the negative exchange interaction, the spin of B1
becomes antiparallel to the spin of oxygen O2. In the conduction process, the eg electrons from
A will replace the O2 electrons and the O2 electrons will jump to the manganese ion B in a state
that the spin direction remainsup (up). However, according to Hund's rule, there should be no
spin of the conduction electron that is anti-parallel to the local spin of B1. That is why the
compound LaMnO3,0 is an insulator-antiferromagnetic.
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CHAPTER V
CLOSING
5.1 Conclusion
The crystal structure of LaMnO3.0 has been successfully analyzed using the Rietveld
method of X-ray diffraction. The snippet synthesized by the high energy milling method has
crystallized to form a single phase compound LaMnO3,0, the crystal system = orthorhombic
and space group = Pnma No. 62, lattice parameter a = 5.444(1) ; b = 7,709(1) ; c = 5.540(1)
, = = = 90°, MR response = 7%, crystallite size, D = 17 nm and strainlattice,= -0.5%. The
material is subjected to compressive strain and based on the strain model, LaMnO3.0 material
is an insulator, antiferromagnetic type G. The MR response is only due to the transition from
an irregular spin state to a regular spin state, not accompanied by an insulator phase transition
to a metal phase. Therefore at room temperature, LaMnO3.0 displays a small MR response.
Austenitic stainless steels and ferritic stainless steels exhibit different diffraction
patterns. It is seen that the austenitic stainless steel at temperature chamber can be transformed
from phase to phase by the presence of a shear mechanism, and this can be proven by the
appearance of peaks from the FCC and BCC fields. The results of the diffraction pattern
associated with the Hanawalt method can show the phases contained in the material.
5.2 Suggestion
This paper is a paper that still has many shortcomings, I hope the reader can give
suggestions or criticism. This paper may also be useful for readers and add insight or media
for readers. Hopefully the author can add better information in the future.
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REFERENCES
Sukirman, Engkir., et al. (2010). Analysis of Lamno3 Crystal Structure With X-Ray
Diffraction Technique And Rietveld Method. Jurnal SainsMateri Indonesia, vol
1,2, ISSN: 1411-1098, pp: 70-74
Triaminingsih, Siti. (1998). X-Ray Diffraction Analysis on Austenitic And Ferritic Stainless
Steels (laboratory test). Journal of Dentistry, University of Indonesia, vol 5, 1,
pages:17-24
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