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Preparation of high surface area

tin oxide powders by a


homogenous precipitation method

DTA
DTA merupakan adalah analisis termal
yang melibatkan pemanasan atau
pendinginan antara sampel dan
referensi (inert) dibawah kondisi
yang sama saat merekam perbedaan
temperatur antara sampel dan
referensi.
Data
kurva
yang
diperoleh
memberikan
informasi
tentang
transformasi yang terjadi seperti

TGA
Analisis TGA adalah metode analisis termal dimana
perubahan dalam sifat fisik dan kimia dari bahan
yang diukur sebagai fungsi dari meningkatnya suhu
(dengan laju pemanasan konstan), atau sebagai
fungsi waktu (dengan suhu konstan dan / atau
kehilangan massa konstan). Metode
ini dapat
mengkarakterisasi suatu bahan atau cuplikan
yang dilihat dari kehilangan massa atau terjadinya
dekomposisi, oksidasi atau dehidrasi. Mekanisme
perubahan massa pada TGA ialah bahan akan
mengalami kehilangan maupun kanaikan massa.

TEM
Analisis
TEM
digunakan
untuk
menganalisa morfologi dan topografi
suatu materi.
Sampel yang disiapkan sangat tipis
sehingga elektron dapat menembusnya
kemudian hasil dari tembusan elektron
tersebut yang diolah menjadi gambar

Abstract
Tin oxide powders were synthesized by a homogeneous
precipitation method using urea from SnCl4 solution. This
method resulted in the formation of nanoscale precursor
powders in the range of 3 to 4 nm in diameter together
with a narrow particle size distribution, while the
conventional precipitation method led to the formation of
precursor powder of not only larger particles 46 nm. but
also wider particle size distribution. When these
precursor powders were calcined at 600 oC for 2 h, the
powders from the homogeneous precipitation method
showed higher specific surface areas 2444 m 2/g. On the
other hand, the powders from the precipitation method
exhibited lower specific surface areas 1518 m 2/g.

Purpose
In this paper writer report the
successful synthesis of high surface
area tin oxide powders using the
homogeneous precipitation method.
For comparison, tin oxide powders
synthesized by the direct ammonia
method the precipitation method
were also prepared.

Material
Tin chloride pentahydrate 99%
ammonia water 28%
Urea99%

Preparation of tin oxide powder


Conventional presipitation method
In the precipitation method, aqueous NH3 solution was
added directly to 0.1M aqueous SnCl4 solution until
the pH of the mixture reached desired values
(4,10,12), where white tin hydroxide precipitates were
produced. The powders prepared under these
conditions are named as samples A, B, and C in Table
1, respectively. The products were separated by use of
a high-speed centrifuge at 8500 rpm for 30 min. The
precipitates were then dried in a drying oven at 100 oC
for 24 h. The dried precipitates were calcined in air for
2 h at constant temperatures in an electric furnace.

Homogeneous precipitation method


For the homogeneous precipitation method, ureas
of different concentrations (0.11.0 M) were dissolved in SnCl4.5H2O aqueous solutions (0.01
M). The reacting solutions were hydrolyzed at
90oC for 4h and then cooled with ice water. The
powders
prepared
with
different
urea
concentrations are termed as samples D to G in
Table 1, respectively. The products were
separated using a high-speed centrifuge at 8500
rpm for 30 min. The precipitates were then dried
at 100oC for 24 h. The dried precipitates were
then calcined at constant temperatures for 2 h to
completely convert the hydroxide into tin oxide

Samp
el

Preparation
Method

pH

Precipitation

Urea
concentra
tion (M)

Calcination
Temperature
(oC)

BET surface
area (m2/g)

600

18,18

Precipitation

10

600

15,09

Precipitation

12

600

17,72

Homogeneou
s
precipitation

0,1

600

23,67

Homogeneou
s
precipitation

0,2

600

29,00

Homogeneou
s
precipitation

0,5

600

44,44

Homogeneou
s
precipitation

1,0

600

27,72

Characterization
TEM >> Philips CM20
were taken to observe the size and shape of the dried particles
SEM >> Philips 535M
were taken to examine the microstructural evolution and particle
size of the calcined particles
DTA/TGA (STD2960,TA instrument)
The thermal behavior of the powders was investigated at a
heating rate of 108C/min in flowing air
FT-IR (FTS155, Bio-Rad)
The IR spectra of the powders were measured in the wave
number range from 400 to 4000 cm-1
BET >> ASAP2010, Micromeritics
The specific surface areas of the calcined powders

Result and Discussion


1. TEM
.Metode presipitasi homogen
Terbentuk bubuk berukuran nano
dengan
range
3-4
nm,
dan
distribusi
ukuran
partikelnya
sempit.
.Metode presipitasi konvensional
Terbentuk bubuk precursor yang
ukuran partikelnya tidak hanya
berukuran lebih besar yaitu 4-6
nm, tapi juga distribusi ukuran
partikelnya lebih luas

2. TGA
Kurva TGA menunjukkan kehilangan berat
seiring meningkatnya suhu kalsinasi.
The weight loss is due to the elimination of
ammonia, physically adsorbed water, and
chemically bonded water.
3. DTA
Pada kurva DTA, terbentuk 2 puncak
endoterm yaitu pada suhu 90 dan 180 oC.
Puncak
ini
menunjukkan
peristiwa
evaporasi air yang teradsorpsi dan
dekomposisi
karbonat.
Selain
itu,
terbentuk juga puncak endoterm pada
suhu 240 oC. Puncak ini menunjukkan
dekomposisi NH4+ pada serbuk.

Conclusion
1. Serbuk precursor yang diperoleh dari
metode presipitasi homogen lebih baik
daripada metode presipitasi konvensional
2. Serbuk hasil kalsinasi pada suhu 600 oC
selama 2 jam dengan metode presipitasi
homogen memiliki luas area yang lebih
besar yaitu 24-44 m2/g dari pada metode
presipitasi konvensional yaitu 15-18 m 2/g
3. Metode presipitasi homogen lebih efektif
daripada metode presipitasi konvensional