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DAFTAR ISI

KATA PENGANTAR .................................................................................. i


DAFTAR ISI ................................................................................................. iii
DAFTAR GAMBAR .................................................................................... iv
DAFTAR TABEL ........................................................................................ v
BAB I PENDAHULUAN ............................................................................. 1
1.1 Latar Belakang ............................................................................... 1
1.2 Rumusan Masalah .......................................................................... 3
1.3 Batasan Masalah ............................................................................ 4
1.4 Tujuan Penelitian ........................................................................... 4
1.5 Manfaat Penelitian ......................................................................... 4
1.6 Sistematika Penulisan .................................................................... 5
BAB II TINJAUAN PUSTAKA.................................................................. 6
BAB III LANDASAN TEORI ..................................................................... 10
3.1 Dasar-dasar Kemagnetan Bahan .................................................... 10
3.2 Sifat Kemagnetan Bahan ............................................................... 11
3.3 Konsep Domain dan Histerisis ...................................................... 14
3.4 Metode Kopresipitasi ..................................................................... 17
3.5 Teknik Pengukuran ........................................................................ 17
3.5.1 Transmission Electron Microscopy (TEM).............................. 17
3.5.2 X-Ray Diffraction (XRD) ......................................................... 18
3.5.3 Fourier Transform Infrared (FTIR) ......................................... 19
3.5.4 Vibrating Sample Magnetometer (VSM) ................................. 22
BAB IV METODE PENELITIAN ............................................................. 26
4.1 Alat ................................................................................................ 24
4.2 Bahan ............................................................................................. 24
4.3 Uji Analisis .................................................................................... 24
4.4 Prosedur Penelitian ........................................................................ 24
4.5 Teknik Analisis Data ..................................................................... 28
4.6 Jadwal Penelitian ........................................................................... 34
BAB V PEMBAHASAN .............................................................................. 35
5.1. Hasil Sintesis Mg1-xNixFe2O4 ........................................................ 35
5.2. Analisis X-Ray Diffrcatometer (XRD) ........................................... 35
5.3. Analisis TEM ................................................................................. 53
5.4. Analisis FTIR ................................................................................ 55
5.5. Analisis Sifat Kemagnetan ............................................................ 59
BAB VI KESIMPULAN DAN SARAN...................................................... 66
6.1. Kesimpulan ................................................................................... 66
6.2. Saran .............................................................................................. 67
DAFTAR PUSTAKA ................................................................................... 68
LAMPIRAN-LAMPIRAN
DAFTAR GAMBAR

Gambar 3.1 Arah domain magnetik pada material diamagnetik sebelum dan
sesudah diberi medan magnet eksternal .........................................11
Gambar 3.2 Arah domain magnetik pada material paramagnetik sebelum dan
sesudah diberi medan magnet eksternal .........................................12
Gambar 3.3 Arah domain magnetik pada ferromagnetik ...................................13
Gambar 3.4 Arah domain magnetik pada antiferromagnetik .............................14
Gambar 3.5 (a) domain magnet; (b) dinding domain .........................................15
Gambar 3.6 Hysteresis loop pada material ferro/ferrimagnetik .........................16
Gambar 3.7 Skema TEM ....................................................................................18
Gambar 3.8 Ilustrasi hukum difraksi Bragg .......................................................19
Gambar 3.9 Skema FTIR....................................................................................20
Gambar 3.10 Vibrasi streching dan vibrasi bending ............................................20
Gambar 3.11 Komponen dari VSM .....................................................................22
Gambar 3.12 Proses terjadinya flux oleh pergerakan sampel magnet .................23
Gambar 4. 1. (a) Perangkat XRD Shimadzu-XD,
(b)Perangkat TEM Jeol Jem-1400,
(c) Perangkat VSM Riken Denshi Co Ltd ......................................26
Gambar 4.2 Skema Penelitian ............................................................................27
Gambar 4.3 Ilustrasi Spektrum Puncak Mg1-x NixFe2O4 ....................................28
Gambar 4.4 Ilustrasi Gambar TEM ....................................................................29
Gambar 4.5 Ilustrasi Grafik Hubungan Dengan Ukuran Butir
Yang Terukur Dengan Frekuensi Kemunculannya ........................30
Gambar 4.6 Contoh pola cincin difraksi ............................................................30
Gambar 4.7 Ilustrasi kurva hysteresis hasil pengujian VSM .............................31
Gambar 4.8 (a) kurva histeresis; (b) setelah pembesaran skala ..........................33
Gambar 4.9 Contoh Hasil Analisa FTIR ............................................................34
Gambar 5.1 Proses sintesis nanopartikel Mg1-xNixFe2O4 ...................................35
Gambar 5.2 Spektrum data XRD .......................................................................39
Gambar 5.3 Grafik pengaruh konsentrasi X terhadap parameter kisi dan ukuran
butir.................................................................................................43
Gambar 5.4 Grafik pengaruh konsentrasi X radius ionik ..................................47
Gambar 5.5 Grafik pengaruh konsentrasi X terhadap panjang ikatan ...............49
Gambar 5.6 Grafik perbandingan parameter kisi secara teoritik dengan parameter
kisi secara eksperimen ....................................................................51
Gambar 5.7 Hasil TEM .....................................................................................54
Gambar 5.8 Distribusi Ukuran Sampel ..............................................................55
Gambar 5.9 Spektrum FTIR ...............................................................................57
Gambar 5.10 Kurva histersis hasil VSM ..............................................................60
Gambar 5.11 Grafik pengaruh komposisi X terhadap koersivitas
dan ukuran butir ..............................................................................62
Gambar 5.12 Hubungan Koersivitas dengan ukuran partikel ..............................63
DAFTAR TABEL

Tabel 4.1 Variasi Massa MgCl2 dan NiCl2 .....................................................25


Tabel 4.2 Rincian Jadwal Peneltian ................................................................34
Tabel 5.1 Estimasi persentase fasa α-Fe2O3 dan 𝜸-Fe2O3 ..............................41
Tabel 5.2 Komposisi X, parameter kisi, ukuran butir didalam Mg1-xNixFe2O4
........................................................................................................42
Tabel 5.3 Informasi Distribusi Kation ............................................................46
Tabel 5.4 Informasi bond lenghts cation-anion ...........................................48
Tabel 5.5 Perbandingan parameter kisi secara teoritik(ath) dan ekperimen (aexp)
........................................................................................................50
Tabel 5.5 X-Ray Density ................................................................................53
Tabel 5.6 Gugus fungsi dan bilangan gelombang pada analisa FTIR. ...........58
Tabel 5.7 Pengaruh subsitusi Nikel kedalam Mg1-xNixFe2O4 terhadap
magnetisasi saturasi (Ms), Magnetisasi remanen (Mr), dan
koersivitas (Hc) ..............................................................................61
Tabel 5.8 Informasi persentase α-Fe2O3, Hmax pada Hc 15 kOe, magnetik
anisotropi ........................................................................................64
ABSTRACT

FABRICATION OF Mg1-xNixFe2O4 (x=0.2 ,0.3, 0.4, 0.5, 0.6, 0.7, 0.8)


USING COPRECIPITATION METHOD AND CHARACTERIZATION OF
THEIR CRYSTAL STRUCTURE AND MAGNETIC PROPERTIES

By
Rachmad Almi Putra
14/372362/PPA/4674

The Mg1-xNixFe2O4 nanoparticles have been successfully synthesized by


coprecipitation method at temperature of 90oC with various x = 0.2, 0.3, 0.4, 0.5,
0.6, 0.7, 0.8. The addition of Ni content into MgFe2O4 gives significant effect to the
average grain size, lattice parameter and magnetization of nanoparticles. The grain
size increase as the increase of Ni content. The values varie from 8.6 to 10.4 nm.
The lattice parameter decrease as Ni content increase which values varie from 8.53
Å to 8.58 Å for Ni2+rich and 8.51 Å to 8.53 Å for Mg2+rich. The Transmission
Electron Microscopy (TEM) image showed that nanoparticles are polydisperse
which morphology is not perfectly spherical. The average grain size was 5.9 nm
different to the XRD based schereer calculation result. The Infra-red spectra
confirmed the presence of five absorption peaks in the frequency range of 400 –
4000 cm-1 due to the tetrahedral (A) and octahedral (B) stretching vibration.
Through magnetic measurement conducted by a Vibrating Sampel Magnetometer
(VSM) revealed that samples are ferrimagnetic nanoparticles. The maximum
magnetization appers in sampel Mg0.8Ni0.2Fe2O4 of 16,9 emu/g. The magnetization
decreases with increasing Ni content and the presence of α-Fe2O3 phase. The
coercivity increases from 22.7 to 36.4 Oe with increasing Ni content due to
increasing grain size of nanoparticles. The result revealed that the magnetic
properties and microstructure of nanoparticles strongly depend on cations
composition, their distribution in crystal lattice, and the presence impurity phases
in sample nanoparticles.
ABSTRAK

FABRIKASI NANOPARTIKEL MAGNETIK Mg1-xNixFe2O4 (X= 0,2; 0,3;


0,4; 0,5; 0,6; 0,7; 0,8) MENGGUNAKAN METODE KOPRESIPITASI
SERTA KARAKTERISASI STRUKTUR KRISTAL DAN SIFAT
KEMAGNETANNYA

Oleh
Rachmad Almi Putra
14/372362/PPA/4674

Nano partikel Mg1-xNixFe2O4 telah berhasil disintesis pada suhu 900 C


menggunakan metode kopresipitasi dengan memvariasi x = 0,2; 0,3; 0,4; 0,5; 0,6;
0,7; 0,8. Mensubsitusikan unsur Ni kedalam MgFe2O4 memberikan pengaruh yang
signifikan terhadap ukuran butir, parameter kisi dan magnetisasi dari nanopartikel.
Ukuran butir meningkat seiring dengan meningkatnya unsur Ni. ukuran butir yang
dihasilkan bervariasi dari 8,6 sampai dengan 10,4 nm. Parameter kisi menurun
ketika unsur Ni dinaikkan. Ukuran parameter kisi yang dihasilkan bervariasi dari
8,53 Å hingga 8,58 Å ketika Ni2+rich dan 8,51 hingga 8,53 ketika Mg2+rich. Hasil
pengamayan Transmission Electron Microscopy (TEM) menunjukkan nanopartikel
bersifat polidispersi dengan morfologi tidak bulat sempurna. Rerata ukuran butir
yang dihasilkan 5,9 nm. Hasil pengukuran ini berbeda dengan hasil pengukuran
XRD yang menggunakan persamaan Schereer. Spektrum infra merah menunjukkan
lima puncak serapan pada frekuensi 400 hingga 4000 cm-1 yang menggambarkan
terjadinya vibrasi pada sub kisi tetrahedral (A) dan oktahedral (B). Pengukuran
magnetisasi menggunakan Vibrating Sample Magnetometer (VSM). Hasil dari
VSM menunjukkan sampel bersifat ferrimagnetik. Magnetisasi maksimum terdapat
pada sampel Mg0.8Ni0.2Fe2O4 yaitu sebesar 16,9 emu/g. Magnetisasi menuun seiring
dengan meningkatnya unsur Ni dan kehadiran fasa α-Fe2O3. Koersivitas meningkat
dari 22,7 hingga 36,4 Oe dengan meningkatnya unsur Ni. meningkatnya nilai
koersivitas disebabkan karena meningkatnya ukuran butir nanopartikel. Sehingga
dapat disimpulkan sifat kemagnetan dan mikrostruktur nanopartikel dipengaruhi
oleh komposisi kation dan distribusinya, kisi kristal, dan munculnya fasa pengotor
pada sampel nanopartikel.