Supplementary Data
Synthesis of adenine mediated superparamagnetic colloidal βFeOOH nanostructure(s) – study of their morphological changes
and magnetic behavior
Anil Kumar and Sudhir Kumar Gupta
Absorbance
2.5
2.0
SP2
0.03M FeCl3 + 0.003M Adenine
(Sum spectra)
0.03M FeCl3
0.003M Adenine
1.5
1.0
0.5
0.0
200
300
400
500
600
700
800
Wavelength (nm)
Fig.S1.Electronic spectra of SP2 with the sum spectra of its precursors.
Fig. S2. ζ –potential distribution for SP5.
1
(I)
(II)
(I')
(II')
(III)(III')
Fig. S3.FESEM images and EDAX analysis of: SP2- (I) and (I'), SP3- (II) and (II') and SP4- (III)
and (III') respectively.
2
Fig.S4.EDAX analysis of the samples SP1 and SP5.
25
30
SP2 Diameter size distribution
SP2 Length distribution
25
No. of particles
No. of particles
20
15
10
5
20
15
10
5
0
20
25
30
35
Length (nm)
40
45
0
3
4
5
6
7
Diameter (nm)
(I)
9
(I')
30
25
SP5 Diameter size distribution
SP5 Length distribution
25
20
20
No. of particles
No. of particles
8
15
15
10
10
5
5
0
0
10
15
20
25
Length (in nm)
(II)
1
30
2
3
4
Diameter (nm)
5
(II')
Fig. S5.(a)Size histograms forlength and diameter of nanorodsof: SP2 (I, I') and SP5 (II, II').
3
20
SP5 Diameter of sphericle particles
SP2 Diamter of Spherical particles
15
No. of particles
No. of particles
30
20
10
10
5
0
0
4
5
6
Diameter (nm)
0
7
1
2
3
Diameter (nm)
4
(I) (II)
40 K
60 K
80 K
M (emu/g)
Fig. S5.(b)Size histogram of the spherical nanoparticles in samples: SP2 (I) and SP5 (II).
10 SP5
5
0
-600 -400 -200
0
-5
200 400 600
H/T (Oe/K)
-10
Fig. S6. M vs. H/T plots for SP5 at 80 K, 60 K and 40 K up to 20,000 Oe applied field.
4
5
Fig. S7. ζ –potential distribution for 3 months aged SP5.
Absorbance
2.5
Fresh SP5
3 months aged SP5
2.0
1.5
1.0
0.5
0.0
200
300
400
500
600
Wavelength (nm)
Fig. S8. Electronic spectra of fresh and 3 months aged SP5
5
700
800
%T
100
80
819
SP5 (b)
SB (a)
60
40
4000 3500 3000 2500 2000 1500 1000
-1
Wavenumber (cm )
Fig. S9. FTIR spectra of SB (a);SP5(b).
Fig. S10.HRTEM image of SP2 nanorod.
6
500
Scheme S1.Presenting the effect of adenine concentration on the morphology and size
distribution of β-FeOOH nanostructures.
7
Table S1. Effect of [adenine] on the crystallite size of different adenine mediated β-FeOOH
samples.
[Adenine]
Sample (mol dm-3)
Plane (hkl)
Avg. size*
from XRD
pattern (nm)
Particle size from TEM analysis
(nm) Length x width; diameter of
spherical nanoparticle
SP1
0.001
26.3
-
SP2
0.003
21.6
32.5 x 6.5; 5.5
SP3
0.005
19.3
22.5 x 4.5; 3.5
SP4
0.010
17.1
22.5 x 4.0; 3.5
SP5
0.020
(103), (112),
(512), (013),
(101), (114)
(103), (112),
(512), (013),
(101), (114)
(103), (112),
(512), (013),
(114)
(103), (112),
(512), (013),
(114)
(103), (112),
(512), (114)
13.9
17.5 x 3.5; 2.5
*Calculated using Debye-scherrer method for various reflections.
Table S2. Effect of adenine concentration on the hydrodynamic size of the colloidal β-FeOOH.
S. No. Sample
[Adenine] (mol dm-3)
1
2
3
4
5
6
0.000
0.001
0.003
0.005
0.010
0.020
SB
SP1
SP2
SP3
SP4
SP5
8
Hydrodynamic size
(nm)
98.3
60.8
29.8
32.3
29.7
10.1
Table S3. Brunauer-Emmett-Teller (BET) surface area analysis data.
S. No.
Sample
Specific Surface
Area (m2/g)
Pore Volume (cm3)
1
SB
82.8
27.1
2
SP1
96.3
31.5
3
SP5
194.4
63.7
Table S4.IR spectral data (cm-1) of β-FeOOH, adenine and SP5.
S. No. Vibration mode/
Fuctional group
β-FeOOH
(literature
data)
Adenine
SP5
(Observed) (Observed)
1
2
3
4
H2O stretching
H2O bending
O-H…Cl deformation
Fe-O-Fe stretching
-
5
6
C(8)N(9)
C(4)N(9)
3438
1634
833,
696,644,471,
420
-
7
8
N(9)H bending
C(6)N(1) bending
-
1370
1419
9
10
C(2)N(3)
N(7)C(8)stretching
-
1450
1510
9
1026
1123
3408
1632
819,
693, 637, 467,435,
422
1083
Intensity reduced
significantly
1383
1418 (peak almost
diminished)
disappeared
disappeared
Table S5. Raman spectra data for SB and SP5.
S. No.
1
Peaks observed in
SB (cm-1)
218
Peaks observed in
SP5 (cm-1)
216
2
284
280
3
390
390
4
604
589
5
1304 (br)
1290 (br)
10