Physico-chemical properties of metal nanopowders prepared for advanced technological applications

7/29/2019 Physico-chemical properties of metal nanopowders prepared for advanced technological applications

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(-19(


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By:

Instructor of Physical ChemistryFaculty of Science(Girls)Al-Azhar University


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Supervisors


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Among various metallic nanopowders the

magnetic nanoparticles have been the focusof much research recently because they

possess attractive properties which could see

potential use in

Many efficient synthetic routes have been

described to shape-controlled, highly stable

and monodisperse magnetic nanoparticles.

catalysis

biomedicine

data storage

environmental remediation

magneticresonance

imagining


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Chemical reduction in solution method wasadvantageous over other processes, because of its

lowreaction

tempera

ture

simplicity

solubilityof metalsalts in

water

So that, Ni and Co, have been extensivelyprepared via reduction of metal salts in solutionby hydrazine monohydrate corresponding to the

formation of pure metals.


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Preparation of Nickel nanoparticles2Ni2+ + N2H4 + 4OH- = 2Ni + N2 + 4H2O

spherical

wire Cotton-

likestructure

Thinfilm

Flower

like

structure


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Industrial Catalysis

Electrodesynthesis

Cancertreatment

Applications of the as prepared Ni and Co

nanoparticles


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Pinknickel hydrazinecomplexes.

Pure blacknickel

Not pureblacknickel


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44.5

51.876.4


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70

80

90100oC


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26 nm

32 nm

45 nm

11 nm


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

temperatures (B).

(A)

(B)


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(a)

(b)SEM micrographs

of the sampleobtained at (a) 70,(b) 80, (c) 90 and

(d) 100 oC.


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(c)

(d)SEM micrographs

of the sampleobtained at (a) 70,(b) 80, (c) 90 and

(d) 100 oC.

( )


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TEM micrographs of thesample obtained at (a)70 (b) 80 (c) 90 and (d)

100 oC .

(a)

(b)

16 nm

32 nm

(c)


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(c)

(d)

34 nm

51 nm


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

SEM


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

TEM

13 nm

32 nm

76 nm

132 nm


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XRD patterns of the nanonickel sample obtainedat 90 oC and [Ni+2] = 0.08M using ethanol as

solvent at pH 10-12

17 nm


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SEM (i) & TEM (ii) micrographs of sample

obtained at 90 oC, pH 10-12 and [Ni+2] =

0.08M.

(i) (ii)

19 nm


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Comparison between % yield andparticle size of nanonickel in ethanol

and water.


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Sample

index

[Ni+2]

(mol L-1)

Average

particle size

(nm)

Morphology

% yield

e 0.05 13 Spherical 82.8

f 0.08 32 Spherical 95.8

g 0.1 76 Spherical 89.3

h 0.15 132 Non-

spherical

88.2


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0

1:1

2:1

4:1

SDS: Ni+2


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(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


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(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

(k)(l)

(i)


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TEM patterns of ultrafinenickel powder: (i)

without SDS, (j) SDS:


[Ni+2] = 4:1

(i)

(j)

32 nm

9 nm

(k)


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TEM patterns of ultrafinenickel powder: (i)

without SDS, (j) SDS:


[Ni+2] = 4:1

(l)

(k)

145 nm


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Sample

index

SDS: Ni+2Average

particle

size

(nm)

Morphology

i 0 32 Spherical

j 1:1 9 Spherical

k 2:1 145 Agglomerated

l 4:1 - Thin film


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(m) ( ) XRD


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(m) (n)

(o) (p)

XRD

(m) (n) SEM


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(m) (n)

(o) (p)

SEM

TEM(m)


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TEM( )

(n)

(O) (p)

32 nm

67 nm

113 nm


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1:9

1:5

1:1

SDS:PVA

(q)


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(q)

(r)SEM

(s)


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XRD patterns of sample obtained by using

mixture of SDS and PVA in molar ratio 1:5


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TEM image of sample obtained by using

mixture of SDS and PVA in molar ratio (1:5)


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0.1 M 0.2 M 0.4 M 0.8 M

(t) (u)


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( ) (u)

(v) (w)


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13 nm


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18 nm


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Ni (s)

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


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Co (s)

The variation in optical absorption spectra of Orange G withreaction 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


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Ni (w)




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Ni (c)




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Ni (f)




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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)


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Co (s)


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Ni (w)


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Ni (c)


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Ni (f)


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0.006 0.008 0.010 0.012 0.014 0.016 0.018 0.020 0.022

0.005

0.006

0.007

0.008

0.009

0.010

0.011

0.012

Current(A

)

Voltage (V)

= 0.2 = 0.158 S


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.

0.006 0.008 0.010 0.012 0.014 0.016 0.018 0.020 0.022

0.000

0.001

0.002

0.003

0.004

0.005

SpecificCapacitance(s4

A2/m2

kg)

Voltage (V)


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52.7Am2/kg.


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700 to 1300W/g.


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Parameter Symbol Parameter levels

Low

level(-)

Mid

point(0)

High

level(+)

Nickel

concentration

(molL-1

)

A

0.05

0.08

0.15

Time

(min)

B

10

20

30

Temperature

(oC )

C

70

90

100


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Run A B C % Yield

1 0.05 10 70 47

2 0.05 20 70 63

3 0.05 30 90 82

4 0.05 10 90 75

5 0.05 20 100 73

6 0.08 30 100 93

7 0.08 10 70 67

8 0.08 20 70 77

9 0.08 30 90 96

10 0.08 10 90 80

11 0.15 20 100 87

12 0.15 30 100 94

13 0.15 10 70 70

14 0.15 20 70 77

15 0.15 30 90 95

RESULTS & DISCUSSION


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(1)

(2)

(3)


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(4)

(5)

(6)


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(7)

(8)

(9)


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mol L-1


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76


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Physico-chemical properties of metal nanopowders prepared for advanced technological applications