( - 91(

By:

Instructor of Physical Chemistry

Faculty of Science(Girls) Al-Azhar University

Supervisors
Prof. Dr. Inas Abd El-Aziz El- Sabbagh Prof. Dr. Magda Mohamed El-Fass Prof. Dr. Asrar Gomaa Emam

Dr. Fatma Abd El-Rahman Taher

 Among various metallic nanopowders the magnetic nanoparticles have been the focus of much research recently because they possess attractive properties which could see magnetic potential use in resonance
data storage biomedicine catalysis environmenta l remediation imagining

Many efficient synthetic routes have been described to shape-controlled, highly stable and monodisperse magnetic nanoparticles.

Chemical reduction in solution method was advantageous over other processes, because of its
low reaction tempera ture

solubility of metal salts in water

simplicity

So that, Ni and Co, have been extensively prepared via reduction of metal salts in solution by hydrazine monohydrate corresponding to the formation of pure metals.

Preparation of Nickel nanoparticles

2Ni2+ + N2H4 + 4OH- = 2Ni + N2 + 4H2O

spherical

wire

Cottonlike structure

Thin film

Flower like structure

Applications of the as prepared Ni and Co nanoparticles

Industrial

Catalysis

Electrode
synthesis

Cancer treatment

Pink nickel hydrazine complexes.

Pure black nickel

Not pure black nickel

44.5

51.8 76.4

90 80

100oC

70

11 nm 26 nm 32 nm

45 nm

(A)

(B)

Logarithmic plots of remaining concentration(A), concentration of nickel versus time at different temperatures (B).

(a)

(b)
SEM micrographs of the sample obtained at (a) 70, (b) 80, (c) 90 and (d) 100 oC.

(c)

(d)
SEM micrographs of the sample obtained at (a) 70, (b) 80, (c) 90 and (d) 100 oC.

(a)

16 nm

TEM micrographs of the sample obtained at (a) 70 (b) 80 (c) 90 and (d) 100 oC .

32 nm

(b)

(c)
34 nm

(d)
51 nm

(e) (f) (g) (h)

SEM

13 nm 32 nm

(e) (f) (g) (h)

76 nm 132 nm

TEM

17 nm

XRD patterns of the nanonickel sample obtained at 90 oC and [Ni+2] = 0.08M using ethanol as solvent at pH 10-12

(i) (ii)

19 nm

SEM (i) & TEM (ii) micrographs of sample obtained at 90 oC, pH 10-12 and [Ni+2] = 0.08M.

Comparison between % yield and particle size of nanonickel in ethanol and water.

Sample
index

[Ni+2]
(mol L-1)

Average
particle size (nm)

Morphology
% yield

e f g h

0.05 0.08 0.1 0.15

13 32 76 132

Spherical Spherical Spherical Nonspherical

82.8 95.8 89.3 88.2

0 1:1

2:1 4:1
SDS: Ni+2

(i)

(j)
SEM patterns of ultrafine nickel powder: (i) without SDS, (j) SDS: [Ni+2] = 1:1, (k) SDS: [Ni+2] = 2:1 and (l) SDS: [Ni+2] = 4:1

(i)

(l) (k) (j)

SEM patterns of ultrafine nickel powder: (i) without SDS, (j) SDS: [Ni+2] = 1:1, (k) SDS: [Ni+2] = 2:1 and (l) SDS: [Ni+2] = 4:1

(i)
32 nm

TEM patterns of ultrafine nickel powder: (i) without SDS, (j) SDS: [Ni+2] = 1:1, (k) SDS: [Ni+2] = 2:1 and (l) SDS: [Ni+2] = 4:1

9 nm

(j)

(k)

145 nm

(l)
TEM patterns of ultrafine nickel powder: (i) without SDS, (j) SDS: [Ni+2] = 1:1, (k) SDS: [Ni+2] = 2:1 and (l) SDS: [Ni+2] = 4:1

Sample index

SDS: Ni+2

Average particle size (nm) 32 9 145 -

Morphology

i j k l

0 1:1 2:1 4:1

Spherical Spherical
Agglomerated

Thin film

(m)

(n)

XRD

(o)

(p)

(m)

(n)

SEM

(o)

(p)

(m)
32 nm

TEM

67 nm

(n)

113 nm

(O)

(p)

SDS:PVA
1:1 1:5 1:9

(q)

SEM
(r)

(s)

XRD patterns of sample obtained by using mixture of SDS and PVA in molar ratio (1:5)

TEM image of sample obtained by using mixture of SDS and PVA in molar ratio (1:5)

0.1 M

0.2 M

0.4 M

0.8 M

(t)

(u)

(v)

(w)

13 nm

18 nm

Ni (s)

The variation in optical absorption spectra of Orange G with reaction time using: Ni (s) spherical Ni, Co (s) spherical Co, Ni (w) Ni wire, Ni (c) Ni with cotton-like structure and Ni (f) Ni nanocones with flower-like structure

Co (s)

The variation in optical absorption spectra of Orange G with reaction time using: Ni (s) spherical Ni, Co (s) spherical Co, Ni (w) Ni wire, Ni (c) Ni with cotton-like structure and Ni (f) Ni nanocones with flower-like structure

Ni (w)

The variation in optical absorption spectra of Orange G with reaction time using: Ni (s) spherical Ni, Co (s) spherical Co, Ni (w) Ni wire, Ni (c) Ni with cotton-like structure and Ni (f) Ni nanocones with flower-like structure

Ni (c)

The variation in optical absorption spectra of Orange G with reaction time using: Ni (s) spherical Ni, Co (s) spherical Co, Ni (w) Ni wire, Ni (c) Ni with cotton-like structure and Ni (f) Ni nanocones with flower-like structure

Ni (f)

The variation in optical absorption spectra of Orange G with reaction time using: Ni (s) spherical Ni, Co (s) spherical Co, Ni (w) Ni wire, Ni (c) Ni with cotton-like structure and Ni (f) Ni nanocones with flower-like structure

Ni (s)

UV-Vis spectra for the reduction reaction of p-nitrophenol by NaBH4 catalyzed by: Ni (s), Co (s), Ni (w), Ni (c) and Ni (f)

Co (s)

UV-Vis spectra for the reduction reaction of p-nitrophenol by NaBH4 catalyzed by: Ni (s), Co (s), Ni (w), Ni (c) and Ni (f)

Ni (w)

UV-Vis spectra for the reduction reaction of p-nitrophenol by NaBH4 catalyzed by: Ni (s), Co (s), Ni (w), Ni (c) and Ni (f)

Ni (c)

UV-Vis spectra for the reduction reaction of p-nitrophenol by NaBH4 catalyzed by: Ni (s), Co (s), Ni (w), Ni (c) and Ni (f)

Ni (f)

UV-Vis spectra for the reduction reaction of p-nitrophenol by NaBH4 catalyzed by: Ni (s), Co (s), Ni (w), Ni (c) and Ni (f)

0.012 0.011 0.010

Current (A)

0.009 0.008 0.007 0.006 0.005 0.006 0.008 0.010 0.012 0.014 0.016 0.018 0.020 0.022

= 0.2

= 0.158 S

Voltage (V)

0.005

Specific Capacitance (s A /m kg)

0.004

0.003

0.002

0.001

0.000

0.006

0.008

0.010

0.012

0.014

0.016

0.018

0.020

0.022

Voltage (V)

52.7Am2/kg.

700 to 1300W/g.

Parameter

Symbol

Parameter levels Low Mid High level point level (-) (0) (+)
0.05 0.08 0.15

Nickel concentration (molL-1) Time (min) Temperature (oC )

B C

10 70

20 90

30 100

Run 1 2 3 4 5 6 7

A 0.05 0.05 0.05 0.05 0.05 0.08 0.08

B 10 20 30 10 20 30 10

C 70 70 90 90 100 100 70

% Yield 47 63 82 75 73 93 67

8 9 10 11 12 13 14 15

0.08 0.08 0.08 0.15 0.15 0.15 0.15 0.15

20 30 10 20 30 10 20 30

70 90 90 100 100 70 70 90

77 96 80 87 94 70 77 95

RESULTS & DISCUSSION

(1)

(2)
(3)

(4) (5) (6)

(7)

(8)
(9)

mol L-1

76

77