BS

c/S
ixt
hse
mes
ter
/De
ptofc
hemi
str
y-S
AC,
shi
ll
ong
/S.
Dia
mai 2021

Sy
nthesi
sofgol
d,pl
ati
num andsi
lv
ernanopar
ti
cles:

Gol
dnanopar
ti
cles:

Ther
ear
emanymet
hodst
osy
nthesi
zenanopar
ti
cles.Thef
ir
stexampl
eismet
all
i
c
nanopar
ti
cl d.TheCi
es,suchasgol tr
ater
educt
ionmet
hoddev
elopedbyTur
kev
ichi
n
1951wast
hemostf
oll
owedpr
ocedur
efort
hesy
nthesi
sofgol
dnanopar
ti
cles.I
nthi
s
met
hodt
hedeepwi
ner
edgol
dhy
drosol
swasobt
ainedbyt
heboi
l
ingchl
oroaur
icaci
d
wi
thsodi
um ci
tr
atesol
uti
ons.

boi
l
ing
HAuCl
4 +Na3C6H5O7 Au

Aqueous [
deepwi
ner
ed]
-
I
n1957,Mi
chaelFar
adayf
oundt
hatr
educt
ionofanaqueoussol
uti
onof[
AuCl
4]wi
th
phosphor
usi
nCS2pr
oducedadeepr
edsuspensi
ont
hatcont
ainednanopar
ti
cles of
gol
d.
-
[
AuCl4] + P CS2 AuNPs
Aqueous [
deep-r
ed]

Becausesul
phurf
orm chemi
calbondst
ogol
d,sul
phurcont
aini
ngspeci
esar
egood
st
abi
l
izi
ngagent
sandt
hemostwi
del
yusedst
abi
l
izerf
orgol
dnanopar
ti
clescont
aini
ng
at
hiol
group(
-SH)
.

Anappr
oachhasbeendev
elopedf
oll
owi
ngt
hef
aradaymet
hodt
ocont
rolt
hesi
zeand
-
di
sper
sit
yofgol
dnanopar
ti
clesbyusi
ng[
AuCl
4] andt
hiolst
abi
l
izer
s.Thi
sist
heso
ed Br
cal
l ust
-Schi
ff
ri
n met
hod i
n 1994,i
n whi
ch ai
rst
abl
e gol
d nanopar
ti
cleswi
th
-
di
amet
ersi
ze1.
5and5.
2nm ar
ebei
ngpr
oduced.I
nthi
smet
hod,AuCl
4i st
ransf
err
ed
f
rom aqueousphaset
otol
ueneusi
ngt
hesur
fact
antt
etr
aoct
ylammoni
um Br
omi
de
(
TOAB)andr
educedbysodi
um bor
ohy
dri
de(
NaBH4)i
npr
esenceofdodecanet
hiol
.
S

HAuCl
4 NaBH4/
TOAB S Au S
HS S

Onaddi
ti
onofNaBH4,aqui
ckcol
orchangef
rom or
anget
odeepbr
ownt
akespl
acei
n
or
gani
cphase.TheAuNPsar
egener
atedi
ntol
uenewi
thcont
rol
l
eddi
amet
ersi
nthe

1
 BS
c/S
ixt
hse
mes
ter
/De
ptofc
hemi
str
y-S
AC,
shi
ll
ong
/S.
Dia
mai 2021

r
ange1.
5-5nm.

Ref
erences:
1.I
nor
gani
cChemi
str
y:Shr
iver&At
kinsf
if
thedi
ti
on:
page660
2.Chem.Rev
.2012,
112,
2739-
2779.
Ot
hermet
hodsofpr
epar
ati
on:
1.Sy
nthesi
sofgol
dnanopar
ti
clesusi
ngami
noaci
ds

Anaqueoussol
uti
onofgol
d(I
II
)chl
ori
deaci
d(1mL,1.
0mM)andanaqueous
sol
uti
onofanami
noaci
d(Hi
sti
dine,
1mL,
100mM)wer
emi
xedandi edat80oC
ncubat
f
or20mi
nusi
nganoi
lbat
h,f
oll
owedbypHadj
ust
mentusi
ng1M NaOHor1M HClt
o
pH7.
1–7.
8.

[
Ref
:Jour
nal
ofCol
l
oidandI
nter
faceSci
ence447(
2015)254–257]

2.Sy
nthesi
sofci
tr
atecappedAuNPs

Ci
tr
ate-
cappedAuNPswer
epr
epar
edbymeansoft
hechemi
calr
educt
ionofHAuCl
4

i
nthel
i
qui
dphase.A200mLaqueoussol
uti
onof1mM HAuCl
4wasbr
oughtt
oboi
lwi
th
v
igor
ousst
ir
ri
ng i
n ar
ound-
bot
tom f
laskf
it
ted wi
th ar
efl
uxcondenser
.38.
8 mM
t
ri
sodi
um ci
tr
ate(
20mL)wast
henaddedr
api
dlyt
othesol
uti
on,andt
hemi
xtur
ewas
heat
edunderr
efl
uxf
oranot
her15mi
n,dur
ingwhi
cht
imei
tscol
orchangedf
rom pal
e
y
ell
owt
odeepr
ed.

[
Ref
:ACSAppl
.Mat
er.I
nter
faces2011,
3,1568–1573]

3.Sy
nthesi
sofAqueousLy
sine-
CappedGol
dNanopar
ti
cles.

Onehundr
edmi
l
li
li
t sof10-4 M aqueoussol
er uti
onofchl
oroaur
icaci
d(HAuCl
4)was
r
educedby0.
01gofsodi
um bor
ohy
dri
de(
NaBH4)atr
oom t
emper
atur
etoy
iel
dcol
l
oidal
gol
dpar
ti
cles.Thecol
l
oidalgol
dpar
ti
cleswer
ecappedbyaddi
ti
onof10mLofan
aqueoussol
utonof10-3M l
i ysi
net
o90mLoft
hegol
dhy
drosol
.Af
teraddi
ti
onofl
ysi
ne
and agi
ng t
he gol
d col
l
oidalsol
uti
on f
or12 h,t
his sol
uti
on was subj
ect
ed t
o
ul
tr
acent
ri
fugat
iont
orecov
erapel
l
etofl
ysi
necappedgol
dnanopar
ti
cles.Tof
urt
her
pur
if
ythegol
dnanopar
ti
clesol
uti
onbyr
emov
alofuncoor
dinat
edl
ysi
nemol
ecul
es,t
he

2
 BS
c/S
ixt
hse
mes
ter
/De
ptofc
hemi
str
y-S
AC,
shi
ll
ong
/S.
Dia
mai 2021

pel
l
etwasr
edi
sper
sedi
ndei
oni
zedwat
erandanot
hercy
cleofcent
ri
fugat
ionwas
car
ri
edout
.Thepel
l
etwast
henr
edi
sper
sedi
ndei
oni
zedwat
erf
orUV-
visspect
roscopy
measur
ement
sandi or1H1NMRanal
nD2Of ysi
s.Theconcent
rat
ionofgol
dint
he
r
edi
sper
sedaqueoussol
utonwas10-2M.
i
[
Ref
:Langmui
r2003,
19,
3545-
35493545]

Si
lv
ernanopar
ti
cles:

TheLee-
Mei
selmet
hodi
sthemostcommonappr
oachesf
ort
hesy
nthesi
sofAgNPs.
Thr
eedi
ff
erentki
ndsofAgsol
swer
epr
epar
edbyt
hei
rappr
oaches.
1.Ag2SO4 wasmi
xedwi
thPVA(
pol
yvi
vyl
alcohol
)andH2 gaswasbubbl
edt
hrough
t
hemi
xtur
etoobt
ainedbr
ownsol
swi
thabsor
pti
onmaxi
maat400nm
H2
Ag2SO4 + PVA AgNPs(
brown)
.
2.AgNO3 sol
uti
onwasr
educedbyi
ce-
col
dNABH4 andt
henst
abi
l
izedbyPVAt
o
y
iel
dbr
ownsol
swi
thabsor
pti
onmaxi
maposi
ti
onedat400nm.

PVA
AgNO3 +NaBH4 Ag
3.
4.Thet
hir
dappr
oachesar
etheci
tr
ater
educt
ionmet
hodi
nwhi
chAgsol
swer
e
obt
ainedbyboi
l
ingAgNO3sol
uti
onwi
th1%sodi
um ci
tr
ate(
Na3C6H5O7).Thesol
s
obt
ainedwer
egr
eeni
sh-
yel
l
owwi
thabsor
pti
onmaxi
maat420nm.
AgNO3+Na3C6H5O7 Ag

Ot
hermet
hodsofpr
epar
ati
on:
1.Gr
eensy
nthet
icappr
oachedf
orAgNPs
i
) Pr
epar
ati
onoft
het
eaext
ract
Dr
ygr
eent
eal
eav
es(
400mg)wer
eaddedt
o30mLwat
eri
n150-
mLEr
lenmey
erf
lask.
Themi
xtur
ewasv
igor
ousl
yst
ir
redov
eramagnet
icst
irpl
atef
or30mi
natr
oom
t
emper
atur
eandf
il
ter
edwi
thWhat
man1f
il
terpaper
.Thef
reshl
ypr
epar
edt
eaext
ract
wast
henusedf
ort
hesy
nthesi
sofAgNPsasdescr
ibedbel
ow.
3
 BS
c/S
ixt
hse
mes
ter
/De
ptofc
hemi
str
y-S
AC,
shi
ll
ong
/S.
Dia
mai 2021

i
i
) Sy
nthesi
sofAgNPsusi
nggr
eent
eaext
ract
Wel
l
-def
ined si
l
vernanopar
ti
cleswer
esy
nthesi
sed usi
ng f
reshl
ypr
epar
ed aqueous
sol
uti
onsofgr
eent
eal
eafext
racti
nthef
oll
owi
ngmanner
.Thest
ocksol
uti
onoft
het
ea
l
eafext
ractwasdi
l
utedt
o5%,
10%,
20%,
30%,
and40%(
V/V)wi
thdei
oni
sedwat
er.Next
,
1.
00mLofsi
l
verni
tr
ate(
1mM)and0.
25mLofNaOH(
0.10M)sol
uti
onswer
eadded
dr
opwi
sei
nsequencei
ntot
hedi
l
utet
eaext
ractsol
uti
ons.Thecont
ent
soft
her
eact
ion
v
essel
s wer
e combi
ned wi
th gent
le swi
rl
ing,and br
own AgNPs wer
e pr
oduced
i
mmedi
atel
yatr
oom t
emper
atur
e underambi
entl
i
ghtcondi
ti
ons.[
Ref:Journalof
Exper
iment
alNanosci
ence,
2015,
Vol
.10,
No.16,
1242_
1255]

2.Si
l
vernanopar
ti
clespr
epar
ati
on
Fort
hepr
epar
ati
onofaqueoussol
uti
ons,dei
oni
zedwat
erwasdeoxy
genat
edby
bubbl
i
ngwi
thni
tr
ogengasf
or30mi
nbef
oreuse.Thesodi
um ci
tr
atewasaddedt
oan
aqueoussol
uti
onofsi
l
verni
tr
atewi
thr
api
dst
ir
ri
ng.Thenaf
reshl
ypr
epar
edsodi
um
bor
ohy
dri
desol
uti
onwasaddedbydr
op-
wiseaddi
ti
ont
othemi
xtur
eunderv
igor
ous
st
ir
ri
ng,t
hesol
uti
onchangedt
oyel
l
ow col
ori
mmedi
atel
y.Af
terst
ir
ri
ngf
or30s,t
he
r
eact
ionsol
uti
onwasi
rr
adi
atedwi
thaSodi
um l
amp(
OSRAM NAV- W λ=589nm)
T70- .
[
Ref
:Spect
rochi
micaAct
aPar
tA64(
2006)956–960]

3.Mi
crowav
eassi
stedsy
nthesi
sofPVP-
sil
vernanopar
ti
clecomposi
tes.
Fort
hesy
nthesi
sofAgnanopar
ti
clesSHARPmakemi
crowav
eov
en(
model
:R-
259)
wasused.I
nat
ypi
cal
procedur
e,10mlof1%(
w/v
)et
hanol
i
csol
uti
onofPVPand0.
2ml
of0.
1M AgNO3 wer
etakeni
na25mlcl
osedconi
calf
laskandpl
acedi
nami
crowav
e
ov
ent
hatwasoper
atedatt
he100%powerof800W andf
requency2450MHzf
or5s.
Thecol
our
lesssol
uti
oni
nst
ant
aneousl
ytur
nedt
othechar
act
eri
sti
cpal
eyel
l
owcol
our
,
i
ndi
cat
ingt
hef
ormat
ionofsi
l
vernanopar
ti
cles.Theadv
ant
ageofmi
crowav
e-medi
ated
sy
nthesi
s ov
ert
he conv
ent
ionalheat
ing i
sthe i
mpr
oved ki
net
ics oft
he r
eact
ion
gener
all
ybyone ort
wo or
derofmagni
tude,due t
orapi
dini
ti
alheat
ing and t
he
gener
ati
onofl
ocal
i
zedhi
gh-
temper
atur
ezonesatr
eact
ionsi
tes.
[
Ref
:Mat
eri
alsChemi
str
yandPhy
sics114(
2009)530–532]

4.SDScappedsi
l
vernanopar
ti
cles.
SDS-
cappedAgNPswer
epr
epar
edbymeansoft
hechemi
calr
educt
ionofmet
al

4
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ixt
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mes
ter
/De
ptofc
hemi
str
y-S
AC,
shi
ll
ong
/S.
Dia
mai 2021

sal
tpr
ecur
sor(
sil
verni
tr
ate,AgNO3)i
nwat
erwi
thNaBH4 i
nthepr
esenceofsodi
um
dodecy
lsul
fat
e(SDS)asast
abi
l
izer
.Br
ief
ly,
0.0038gofNaBH4and0.
0085gSDSwer
e
di
ssol
ved i
n 50 mLdei
oni
zed wat
erand st
ir
red f
or30 mi
natr
oom t
emper
atur
e.
Separ
atel
y,50mLAgNO3 2×10-4 molL-1,sol
uti
onwaspr
epar
edbydi
ssol
vi
ng0.
0017g
AgNO3i
n50mLdei
oni
zedwat
er.AgNPswer
epr
oducedbydr
opbydr
opaddi
ti
onoft
he
AgNO3sol
uti
oni
ntot
heNaBH4–SDSmi
xtur
efol
l
owedbyst
ir
ri
ngf
or1h.
[
Ref
:Anal
.Met
hods,
2011,
3,2599]

5
 BS
c/S
ixt
hse
mes
ter
/De
ptofc
hemi
str
y-S
AC,
shi
ll
ong
/S.
Dia
mai 2021

Sy
nthesi
sofpl
ati
num nanaopar
ti
cles:

1.Chemi
calr
educt
ionmet
hod
I
nthesy
nthesi
spr
ocess,
thePtmet
alpr
ecur
sor
,ei
theri
nani
oni
coramol
ecul
arst
atei
s
t
aken.
Chemi
calchangesar
eini
ti
atedt
oconv
ertt
hepr
ecur
sort
oPtmet
alat
omsbyt
he
r
educi
ngagent
,thesemet
alat
omst
henmer
gei
ntosui
tabl
esuppor
tedmat
eri
als/
or
st
abi
l
izert
ofor
m nanopar
ti
cles.Forexampl
einchemi
calr
educt
ion,H2Pt
Cl6i
sreduced
byNaBH4 ( kandet
Par .al
.2002)orZn(
Jiangandet
.al
.2003)t
ogi
ver
iset
opl
ati
num
nanopar
ti
cles;

H2Pt
Cl6+NaBH4 Pt + Ot
herr
eact
ionpr
oduct
.
Par
ti
cle gr
owt
his usual
l
yconf
ined byt
he pr
esence ofa conf
ini
ng suppor
tora
pr
otect
ion agent
/st
abi
l
izer
.Suppor
ted and si
ze-
cont
rol
l
ed nanopar
ti
cles ar
ethen
f
ormed.
Forexampl
e,sur
fact
ant
-st
abi
l
izedcol
l
oidalPtNPswasobt
ainedi
nwhi
chH2Pt
Cl6 was
empl
oyed as t
he pr
ecur
sor
s ofPtnanopar
ti
cles,zwi
tt
eri
oni
c sur
fact
ant3-
(N,N-
di
met
hyl
dodecy
lammoni
o)pr
opanesul
fonat
e(SB12)wasaddedast
hest
abi
l
izerand
met
hanol
ast
her
educt
ant(
LiandHsi
ng2006)
.
[
Ref
:Asi
aPaci
fi
cJour
nal
ofEner
gyandEnv
ironment
,Vol
ume1,
No2(
2014)
]

2.Shapecont
rol
l
edsy
nthesi
sofPtnanopar
ti
cles.

Asol
utonof1X10-4M K2Pt
i Cl4waspr
epar
edi
n250mlofwat
er,
towhi
chwasadded0.
2
mlof0.
1M sodi
um pol
yacr
ylat
e(set1)
.ThePti
onswer
ereducedbybubbl
i
ngH2gasat
ahi
ghf
low r
atet
hrought
hesol
uti
on.Ther
eact
ionv
esselwast
henseal
ed,andt
he
sol
uti
onwasl
eftov
erni
ght
.Af
ter12hour
scol
l
oidalPtNPswer
efor
med.Thei
nit
ial
concent
rat
ionr
ati
ooft
hecappi
ngmat
eri
alt
othemet
alcat
ioni
nthesol
uti
onswas1:
1.
TEM i
magesshowscubi
cPtNPsf
ormed.

Anot
herset(
set2)waspr
epar
edbyaddi
ngt
othest
art
ingsol
uti
on1.
0mloft
he0.
1M
pol
yacr
ylat
esol
uti
on,r
espect
ivel
y,andf
oll
owi
ngt
hesamepr
ocedur
e.Her
ether
ati
oof
t
hecappi
ngmat
eri
alt
othatoft
hemet
alcat
ioni
nthesol
uti
onwer
e5:
1wi
tht
he

6
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c/S
ixt
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mes
ter
/De
ptofc
hemi
str
y-S
AC,
shi
ll
ong
/S.
Dia
mai 2021

f
ormat
ionoft
etr
ahedr
alPtNPs.
[
A.L.St
epanov
,A.
N.Gol
ubev
,S.
I.Ni
ki
ti
nandY.
N.Osi
n
Rev
.Adv
.Mat
er.Sci
.38(
2014)160-
175]