PENGOLAHAN DATA XRD

APLIKASI METODE XRD

1. Penentuan struktur kristal :
1. Pengideks-an bidang kristal,
2. Bentuk dan ukuran sel satuan kristal,
3. Jumlah atom per-sel satuan
2. Analisis kimia :
1. Identifikasi/Penentuan jenis kristal
2. Penentuan kemurnian hasil sintesis
3. Deteksi senyawa baru
4. Deteksi kerusakan oleh suatu perlakuan
Jenis Sampel :
 Bentuk: serbuk, lembaran, plat
 Jenis: logam, oksida logam, polimer,
mineral, seny.organik

Perlakuan sampel:
◼ Sampel padatan dari alam (lempung, zeolit, dsb)
 Dibersihkan dari kerikil, ranting, daun, dsb
 Dikeringkan
 Dihaluskan: 10-250 mesh
 Dimasukkan ke dalam sample holder

◼ Sampel lembaran:
 Langsung dianalisis
Data XRD

◼ Kondisi Pengukuran
 Nama alat dan Serinya
 Rentang 2 (5-100)
 Sumber radiasi (CuKa), celah (slit).
◼ Data Gambar
◼ Data Text (.txt)
◼ Data Olahan (parameter kristal, kisi, indeks)
◼ Data pembanding (JCPDS card or ICDD files)
JCPDS= Joint Committee on Powder Diffraction Standard
ICDD= The International Center for Diffraction Data
 X-Ray Diffraction Pattern
z z z
c c c

y (110) y y
a b a b a b
Intensity (relative)

x x x (211)

(200)

Diffraction angle 2

Diffraction pattern for polycrystalline a-iron (BCC)

 DATA DIFRAKSI = POLA DIFRAKSI

Intensitas

Sudut difraksi 2 
Data text ------> data Gambar dan parameter
kristal

◼ Excel
◼ Origin----------→
◼ Igor-------------→
◼ Phasanx
◼ Retica
◼ Etc…
Data Text
FILEN kyousei12/Ni2Sn1400
BLOCK 0
FILES 0 0:RAW 1000:PEAK 3100:POLE-TRANS 3200:POLE-REFLECT
SAMPL Ni2Sn1400
MDATE 2011/01/25 18:37
OPERT rodian
GONIO 12
ATACH 100 6:POLE
TARGT Cu
XWAVE 1.54056
VOLTG 40 Kv
CURNT 200 mA
MODE1 1 1:Theta Scan 2:d* Scan 4:Mennai
MODE2 1 1:CS 2:FT 3:FC
MODE3 3 1:Repeat 2:Integ 3:Normal
SAXIS 1 1:2Theta/Theta 2:2Theta 3:Theta
START 5.020 deg
STOPA 80.000 deg
STEPW 0.020 deg
SPEED 4.000 deg
CTIME 1.00 sec
CUNIT 1
DSLIT 1.00 deg
SSLIT 1.00 deg
RSLIT 0.30 mm
DATAN 3750
MAXCN 14156
HIGHV 780
BASEL 1.16
WINDW 1.90
XGSHU 3 1:3Kw 2:18Kw
POS2T 0.000
DTSRT
5.020 1136
5.040 1123
5.060 1220
5.080 1193
5.100 1130
5.120 1110
5.140 1103
5.160 1160
Average Particle Sizes : Scherrer Equation

◼ τ is the mean size of the ordered (crystalline) domains, which may be

smaller or equal to the grain size;
◼ K is a dimensionless shape factor, with a value close to unity. The
shape factor has a typical value of about 0.9, but varies with the actual
shape of the crystallite;
◼ λ is the X-ray wavelength;
◼ β is the line broadening at half the maximum intensity (FWHM), after
subtracting the instrumental line broadening, in radians. This quantity
is also sometimes denoted as Δ(2θ);
◼ θ is the Bragg angle.
Identifikasi fase kristal
JCPDS card of Ni3Sn alloy
JCPDS card of SnO