Ftir Dan XRD Analysis

X-Ray Diffraction
DEPARTEMEN TEKNIK MATERIAL, FAKULTAS TEKNOLOGI INDUSTRI- ITS
Theoretical Background of Diffraction
Bragg’s Law
X-rays are electromagnetic waves, as are visible light, but the X-ray wavelength is much
shorter than visible light, only in the order of 0.1 nm.
We normally set n=1 and adjust Miller indices, to give

2dhkl sin  = 
2d sin   n
n=1 :  = 39.9°
 n 
  sin   1
n=2 : X (n/2d)>1
 2d 
Combining Bragg and d-spacing equation

X-rays with wavelength 1.54 Å are “reflected” from the (1 1 0) planes of a cubic
crystal with unit cell a = 6 Å. Calculate the Bragg angle, , for all orders of
reflection, n.
1 h k l 2 2 2
11 0
2
  2
 0.056
d a2 6
d  18 
2
d = 4.24 Å
1.How to identify phase?

2.How to determine crystal structure?
3.How to determine the interaction of
mixture?
4.How to analyze crystallinity?
5.etc
identify phase
crystal structure
the interaction of mixture

Phase content, using highscore software

crystallinity
Another uses:
Small Angle X-Ray Scattering (SAXS)

Only for nanomaterial: measure the distance between
nanoparticle using small angle
VIBRATIONAL SPECTROSCOPY
Vibrational spectroscopy uses electromagnetic waves with much
longer wavelengths, in the order of 10−7 m, than the X-rays which are
also electromagnetic waves but with wavelengths in the order of
10−10 m.
• Two spectroscopic methods: Fourier transform infrared

spectroscopy (FTIR) and Raman microscopy (also called micro-
Raman), which are the vibrational spectroscopy techniques most
commonly used by scientists and engineers for materials
characterization.
PRINCIPLES OF VIBRATIONAL SPECTROSCOPY
• Infrared spectroscopy is based on the phenomenon of infrared absorption by

molecular vibrations. When a molecule is irradiated by electromagnetic waves
within the infrared frequency range, one particular frequency may match the
vibrational frequency of the molecule. Consequently, the molecular vibration
will be excited by waves with the frequency.
• Raman spectroscopy is based on the Raman scattering phenomenon of

electromagnetic radiation by molecules. When irradiating materials with
electromagnetic radiation of single frequency, the light will be scattered by
molecules both elastically and inelastically. Elastic scattering means that the
scattered light has the same frequency as that of the radiation. Inelastic
scattering means that the scattered light has a different frequency from that of
the radiation. Elastic scattering is called Rayleigh scattering while inelastic
scattering is called Raman scattering.
THEORITICAL BACKGORUND
The electromagnetic radiation in near visible light is able to change

status of molecular vibrations and produce vibrational spectra of
molecules
• Molecules in solids are always in vibration at their equilibrium positions, except at the
temperature of absolute zero
• Molecular vibrations can be simply modeled as massless springs connecting nuclei in a

molecule.
Illustration the potential energy of harmonic motion as a parabolic function of

displacement from the equilibrium position of nuclei.
Normal modes of vibrations in a CO2 molecule.
• Nuclei in a molecule vibrate at the same frequency and in the same phase (passing their
equilibrium positions at the same time); and
• Nuclear motion does not cause rigid body movement (translation) or rotation of
molecules.
It is possible to categorize the various modes of molecular vibration

modes into four types:
1. Stretching vibration (ν);

2. In-planar bending vibration (δ);
3. Out-of-planar bending vibration (γ); and
4. Torsion vibration (τ).
Introduction
• FT-IR stands for Fourier Transform InfraRed
• The preferred method of infrared spectroscopy
• Vibrational spectroscopy for molecular analysis
So, what information can FT-IR provide?
• It can identify unknown materials

• It can determine the quality or consistency of a
sample
• It can determine the amount of components in a
mixture
Background
Polystyrene
Poly (acrylonitrile-co-methyl methacrylate) nanoparticles
Disappearance of
peak at 1629 or
1631 cm-1
Tabel daerah gugus fungsi

Cara membaca spektra FTIR :
1. Tentukan sumbu X dan Y-sumbu dari spektrum. X-sumbu dari spektrum IR diberi
label sebagai "bilangan gelombang" dan jumlahnya berkisar dari 400 di paling
kanan untuk 4.000 di paling kiri. X-sumbu menyediakan nomor penyerapan. Sumbu
Y diberi label sebagai "transmitansi Persen" dan jumlahnya berkisar dari 0 pada
bagian bawah dan 100 di atas.
2. Tentukan karakteristik puncak dalam spektrum IR. Semua spektrum inframerah

mengandung banyak puncak. Selanjutnya melihat data daerah gugus fungsi yang
diperlukan untuk membaca spektrum.
3. Spektrum IR dapat dipisahkan menjadi empat wilayah. Rentang wilayah pertama

dari 4.000 ke 2.500. Rentang wilayah kedua dari 2.500 sampai 2.000. Ketiga wilayah
berkisar dari 2.000 sampai 1.500. Rentang wilayah keempat dari 1.500 ke 400.
4. Tentukan kelompok fungsional diserap di wilayah pertama. Jika spektrum

memiliki karakteristik puncak di kisaran 4.000 hingga 2.500, puncak sesuai dengan
penyerapan yang disebabkan oleh NH, CH dan obligasi OH tunggal.
5. Tentukan kelompok fungsional diserap di wilayah kedua. Jika spektrum memiliki

karakteristik puncak di kisaran 2.500 hingga 2.000, puncak sesuai dengan penyerapan
yang disebabkan oleh ikatan rangkap tiga.
6. Tentukan kelompok fungsional diserap di wilayah ketiga. Jika spektrum memiliki

karakteristik puncak di kisaran 2.000 sampai 1.500, puncak sesuai dengan penyerapan
yang disebabkan oleh ikatan rangkap seperti C = O, C = N dan C = C.
7. Membandingkan puncak di wilayah keempat spektrum IR lain. Yang keempat dikenal

sebagai daerah sidik jari dari spektrum IR dan mengandung sejumlah besar puncak serapan
yang account untuk berbagai macam ikatan tunggal. Jika semua puncak dalam spektrum IR,
termasuk yang di wilayah keempat, adalah identik dengan puncak spektrum lain, maka Anda
dapat yakin bahwa dua senyawa adalah identik.

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X-Ray Diffraction

DEPARTEMEN TEKNIK MATERIAL, FAKULTAS TEKNOLOGI INDUSTRI- ITS

Theoretical Background of Diffraction

We normally set n=1 and adjust Miller indices, to give

Combining Bragg and d-spacing equation

1.How to identify phase?

the interaction of mixture

Phase content, using highscore software

Small Angle X-Ray Scattering (SAXS)

• Two spectroscopic methods: Fourier transform infrared

PRINCIPLES OF VIBRATIONAL SPECTROSCOPY

• Infrared spectroscopy is based on the phenomenon of infrared absorption by

• Raman spectroscopy is based on the Raman scattering phenomenon of

The electromagnetic radiation in near visible light is able to change

• Molecular vibrations can be simply modeled as massless springs connecting nuclei in a

Illustration the potential energy of harmonic motion as a parabolic function of

Normal modes of vibrations in a CO2 molecule.

It is possible to categorize the various modes of molecular vibration

1. Stretching vibration (ν);

So, what information can FT-IR provide?

• It can identify unknown materials

Poly (acrylonitrile-co-methyl methacrylate) nanoparticles

Tabel daerah gugus fungsi

Cara membaca spektra FTIR :

2. Tentukan karakteristik puncak dalam spektrum IR. Semua spektrum inframerah

3. Spektrum IR dapat dipisahkan menjadi empat wilayah. Rentang wilayah pertama

4. Tentukan kelompok fungsional diserap di wilayah pertama. Jika spektrum

5. Tentukan kelompok fungsional diserap di wilayah kedua. Jika spektrum memiliki

6. Tentukan kelompok fungsional diserap di wilayah ketiga. Jika spektrum memiliki

7. Membandingkan puncak di wilayah keempat spektrum IR lain. Yang keempat dikenal

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