Disampaikan pada Webinar Fisika Material

“Riset Fisika Material di Era Revolusi Industri 4.0”

Fisika UIN Sunan Kalijaga
Yogyakarta, 24 Oktober 2020

Nano Partikel Magnetik:

Peluang Aplikasi di Bidang Kesehatan

By Budi Purnama
Physics Department, Universitas Sebelas Maret
Jl. Ir. Sutami 36A Kentingan Surakarta 57126
Isi Presentasi
◼ Pengantar
◼ Prosedur Eksperimen
◼ Modifikasi nanopartikel magnetik cobalt Ferrite
◼ NPM cobalt ferrite berbasis pasir besi
◼ Fotokatalis NPM cobalt ferrite
◼ Antibakteria
◼ Kesimpulan
 Introduction
◼ Superparamagnetic limit adalah kata kunci guna aplikasi devais spintronic
seperti HDD, MRAM dan lainnya yang memerlukan memperkecil ukuran/the
donwn size hingga orde nanometer dengan lithography technique dan atau
prosedur sintesis. Fenomena superparamagnetik disumbang oleh kehadiran
single domain pada a defined pattern atau pada particle tunggal.
◼ Secara teori ukuran untuk realisai single domain → RSD = 36 AK  0 M S2
Theory → kurang dari 100 nm
Experimen → kurang dari 70 nm (Berkowitz and Schuele, 1959)
kurang 45 nm (Maaz et al, 2007) untuk cobalt ferrite
◼ Nano partikel cobalt ferrite : MS tinggi ~ 80 emu/cc, HC tinggi ~ 4,5 kOe,
stabil secara kimia.
◼ Karakteristik yang menarik ini membuka peluang aplikasisebagai contrast
agent for magnetic resonance imaging (Ahmad et al 2014), agen fotokatalis,
antibakteria serta sebagai diagnostic awal kanker dan drug delivery
system/targeted therapy procedures (Pasukoniene et al 2015).
Magnetisasi Relaksasi dari single domain magnetic

Energy barrier

Magnetisasi Medan Nol

(Relaksasi)
Reversal ditentukan oleh waktu relaksasi ()
Waktu relaksasi (∝ Blocking temperature TB)
Reciprocal requirement
Ukuran Partikel (∝ MS)
SINTESIS NANOPARTIKEL

Bahan-bahan NaOH
nanopartikel +
Co(NO3)2.6H2O

Fe(NO3)3.9H2O Aquades
Dititrasi @suhu tertentu
0,01 mol Diaduk dg magnetic stirrer dg tetap di stirrer

Penyiapan Homogenisasi Synthesis

Bahan

+ Endapan

Larutan
Sampel diannealing didiamkan
& endapan dipisahkan

Annealing Pencucian dan Pengendapan

Pengeringan
 Angka Gelombang k (1/cm) 20 40 60 80
2θ(degree)
Hasil & Diskusi: Suhu Sintesis
100 (311) 15000
(a) 8000 (
80 (111)
Transmitance (%)

Intensity (a.u.)
Intensity (a.u)
RT o
T = 95 C
60 (220) 10000
(511) (440)
6000 (111) (400)
40
(b)
20
4000 5000
Annealing at T = 600oC for 4 hr
0
4000 3000 2000 1000 0 20 40 60 80 20
Wave number (1/cm) 2θ(degree)
Gambar 2.Pola XRD cobalt ferrite hasil
Gambar 1. Modifikasi kurva FTIR dari sintesis (a) suhu ruangan dan (b) 95C.
sampel cobalt ferrite (a) suhu ruangan dan
(b) 95C .
No Suhu Synthesis (C) 2θ (°) Crystalite size D
(nm)
1. RT (28C) 35.665 7.59
2. 95C 35.665 37.90
3. 40C Stein et al 7.4
2018
 Hasil & Pembahasan
(a) (b)

[Ni80Fe20(800 nm)/Cu(y nm)] 3 "B"

1500 "
200
1000
Hc= 550 Oe
y = 300 nm
100

M (emu/cm3)
Mr= 96,9 emu/cm3
500
M (emu/cm3)

y = 400 nm

0 0
Gambar 3. Typikal SEM nano partikel cobalt
x = 300
feritte
Hc= 265 Oe
-500suhu T = 600C selama x4= 400
hasil anealling h dengan -100
Mr= 13,1 emu/cm3
suhu sintesis (a) RT dan (b) 95C
-1000 -200

-1500 -2000 -1000 0 1000 2000

-1000 -500 0 500 1000 H (Oe)
Magnetic field HGambar
(Oe) 4. Typikal kurva hysteresis untuk cobalt ferrite Hc = 5
Titrasi at 95oC-->RT 600oC(4 jam)
nanopartikel dg suhu sintesis suhu ruangan o
RT and 95oC . Mr = 9
Titrasi at RT 600 C(4 jam) Hc = 265 Oe
40 o Mr = 13.1 emu/cm3
Tann = 600 C 4 jam

20
u/gr)

40
 Results and Discussion: annealing times effect
Transmittance (a.u.)

11 h

6h (311)

Intensity (a.u)
2h
(220) (400) (511) (440)
0h (111) 11 h

6h

2h
4000 3000 2000 1000 0
Wavenumber k (1/cm)
Fig 5. The modified FTIR curve of cobalt
ferrite at different annealing time periods
100 20 40 60 80
i.e. 0, 2, 6 and 11 h 2θ(degree)
Fig 6. X-ray diffraction patterns for cobalt
crystallite sizes of 21.4, 21.6 and 21.7 nm
were obtained for the annealing80 times of ferrite nanoparticles at three annealing
times of 2, 6 and 11 h at 600°C
2, 6 and 11 h, respectively
60 8000
 (b)
(b) A Gaussian narrow size
distribution is obtained for a
long-time annealing:
2 h distribute 12.5 nm – 75 nm
11 h distribute 25.0 nm – 65 nm

Fig 7. Typical SEM images and partcilse size distribution

(inset) for cobalt ferrite after annealing at 600°C with two
different time durations of (a) 2 h and (b) 11 h

For the sample of 2 h; the MS = 110.5 emu/cm3. In

contrast, for a sample of 11 h; the MS = 140.5 emu/cm3.
Coercive fields HC of 307 and 381 Oe were obtained
for annealing times of 2 and 11 h, respectively. The
experimental results confirmed that the magnetic
property of the cobalt ferrite nanoparticles is dependent
Fig 8. A typical hysteresis curve for
on the modified crystallite sizes.
cobalt ferrite nanoparticles at two
different annealing time periods of 2
and 11 h
 Results and Discussion: synthesis temperature effect
The cations
1000-75 80 distribution for the tetrahedral
80 1000-85
and the octahedral sites are indicated by the
1000-95
ratios I220/I222 and I422/I222 .
Transmitance (%)

700 600 500 400 95 C

o 60
60 (311)

o
85 C 40 K
(440)
40 (220)
(400) (511)

Intensity (a.u.)
o (422)
75 C (222)
95oC
20
20
4000 3000 2000 1000 0 0 85oC
Wave number, k (1/cm) 4000 3000 2000 1000 0
Fig 9. FTIR results for the cobalt-ferrite
nanoparticles synthesized at three different 75oC
temperatures followed by annealing at
1000C for 5 h. 1200-75
1200-8530 40 o
50 60
0 I220/I222 @ 75C, 85C and 95C were 1200-95 2 teta ( )
3.43, 3.40 and 3.48 (theoretical ~ 3);
whereas I422/I222 ratios were 1.68, 1.52 Fig 10. XRD patterns of the CoFe2O4 nanoparticles
synthesized at temperatures of 75°C, 85°C and
and 1.24 (theoretical 1.0) → cation
0 distribution occur at octahedral cites
95°C and then annealed at 1000°C for 5 h.
 Fig Kurva
11. Typical SEM
Histerisis M images
vs H (suhu for
aniling cobalt-ferrite
1000 C) synthesized at temperatures of (a) 75oC, (b)
85oC, and (b) 95oC and then annealed at 1000°C for 5 h.
400
Magnetization, M (emu/cc)

Fig 12. Typical 75 hysteresis curves for cobalt-ferrite

nanoparticles synthesized
85 at temperatures of 75, 85, and
85oC 95
200 95oC and annealed at 1000°C for 5 h.

75oC
0 95oC

-200

-400
-4000-2000 0 2000 4000
Magnetic field, H (Oe)
 Results and Discussion: calcination temperature effect

Fig 13. Typical TG/DTA of cobalt ferrite

nanoparticle synthesised using the
coprecipitation method
D→ increase with the increasing
calcination temperature.
From the I220/I222 and I422/I222 ratios,
expected that the cation distribution Fig 14. X-ray diffraction patterns for cobalt ferrite
occur for both octahedral and nanoparticles at calcination temperatures, namely (a)
tetrahedral cites. 600 C, (b) 800 C and (c) 1000 C, for six hours.
Fig 14. Typical SEM images including particles size distribution analysis (inset) and VSM curves for
cobalt ferrite after calcination for six hours @ (a)600C, (b) 800 C and (c) 1000 C.

Magnetization: It is expected that Fe3+ dominantly

migrate to octahedral sites with the increase of
calcination temperature. So that MS increase with the
increase of the calcination temperature i.e. 38.58,
53.59 and 62.30 emu/g.
Coercive field confirmly depend on the particles size.
 -20 -10 0 10 20
20 30 40 50 60 70 80 Medan Magnet H (kOe)
Sudut 2θ(derajat)
Results and Discussion: cobalt ferrite based natural fine sediment
(A) Standar
(B) Kalsinasi
(C) Tanpa kalsinasi

o
800 C Tidak Aniling

Magnetization M (emu/g)
40
Intensitas (a.u)

20
o
Tan=800 C, 4 jam
0

(311) -20
Standar
(220) Aniling
(400) (511)(440) Standar -40
(222) (422) Tidak Aniling

0 1000 2000 3000 4000

20 30 40 50 60 70 80 -20 -10 0 10 20
2θ(o) Magnetic Field H (kOe)
Fig 15. (a) Typical XRD pattern and (b) VSM result of cobalt ferrite with natural fine sediment as
raw material.
 Magnetic Field, H (kOe)

Results and
MnDiscussion:
Mg Fe O NP's MnxMg1-xFe2O4 based natural fine sediment
1-x x 2 4

(311)
(a (b
(220) (511) (440) ) )
Intensity (a.u.)

Frequency
x=0.25

(%)
x=0.5 Particles diameter
(nm)
(c
)
x=0.75

20 30 40 50 60 70
o
Angle 2 θ ( )
Fig 16. XRD patterns for co-precipitated MnxMg1−xFe2O4 nanoparticles with x =
0.25, 0.50 and 0.75.
Results and Discussion: MnxMg1-xFe2O4 based natural fine sediment
Mn 1-x Mg xFe2O4 NP's
40 40

Magnetization, M (emu/g)
42 (a)
Magnetization, M (emu/g)

MS (emu/g)
o
Ta=300 oC
20 40 Ta=400 oC
20 Ta=500 oC
38 Ta=600 C
36
0 x=0.25 500
0 300 400 500 600
x=0.50 o
Ta ( C) 400
(b)

HC (Oe)
x=0.75
300
Fig 17. Typical VSM curve for co-
-20 200
precipitated
-20 MnxMg1−xFe2O4 100nanoparticles
with x = 0.25, 0.50 and 0.75. 0
300 400 500 600
-40 Ta (oC)
-4 -2 0 2 4 -40
Magnetic Field, H (kOe) -20 -15 -10 -5 0 5 10 15 20
Magnetic Field, H (kOe)

40 Mn1-xMgxFe2O4 NP's

(311)
20
(220) (511) (440)
(a.u.)

0 x=0.25
Kinerja Foto Katalis: Teori Dasar
Kinerja Foto Katalis

Fig 17. Photocatalyst performance results on the blue

methylene solution are represented in the UV-VIS curve for the
active ingredient CoFe2O4 (a) sample A (b) sample B and (c) Naik et. al, 2019
sample C. (d). Reduction ratio of the photocatalyst as a
function of times
Kinerja Anti-Bakteria
1. NM berinteraksi secara
elektrostatik dengan membran
bakteri
2. Kelahiran ROS (Reactive
Oxygen Spesies) yg merupakan
radikal bebas, menyerap pasokan
oksigen, efeknya
➢ memicu kerusakan membran
sekunder,
➢ menghambat fungsi protein,
➢ menyebabkan kerusakan
DNA,
➢ dan menghasilkan produksi
radikal berlebih
3. NM as antibacterials
complementary to antibiotics
 Samavathi et al, 2017

Fig 18 Performance of the actibacteria activity of the cobalt

ferrite based material
Naik et al, 2019
Kesimpulan & Riset masa depan

Telah disajikan prosedur sintesis nano partikel berbasis cobalt ferrite dan juga
memanfaatkan sumber daya lokal seperti pasir besi bengawan Solo maupun
pasir besi di daerah Padang.
Modifikasi nano partikel yang menjadi parameter utama aplikasi telah berhasil
di konfirmasi dari perubahan parameter sintesis.
Telah pula dikonfirmasi kinerja nano partikel untuk bidang kedokteran yaitu
foto katalis dan anti bakteri menggunakan sampel yang di sintesis
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Terima kasih