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Mc lc

M u 1
Chng 1. Tng quan
2
1.1.
Cng ngh nano v vt liu nano
2
1.1.1. Cng ngh nano (nanotechnology) 2
1.1.2. Vt liu nano
2
1.1.2.1. nh ngha
2
1.1.2.2. c im, tnh cht ca vt liu nano
2
1.1.3. Cc phng php tng hp vt liu nano 5
1.1.3.1. Phng php t trn xung (top-down) 5
1.1.3.2. Phng php t di ln (bottom-up)
5
1.1.4. Tnh cht ca ht nano kim loi 8
1.1.5. ng dng ca vt liu nano v cc ht nano kim loi
10
1.2. BC V NANO BC
13
1.2.1. Gii thiu v kim loi bc
13
1.2.2. Bc nano v tnh u vit ca bc nano so vi bc ion v bc khi
1.2.3. Cc phng php iu ch nano bc
14
1.2.4. ng dng ca nano bc 17
1.3. Gii thiu v CuO v xc tc Ag/CuO
20
1.4. Mt s phng php nghin cu vt liu nano
21
1.4.1. Phng php nhiu x tia X
21
1.4.2. Phng php phn tch nhit
23
1.4.3. Knh hin vi in t truyn qua (TEM)
23
1.4.4. Knh hin vi in t qut (SEM) 25
1.4.5. Ph tn x nng lng (EDS)
25
CHUNG 2. THC NGHIM 26
2.1. i tng, ni dung v phng php nghin cu
26
2.2. ha cht - dng c
26
2.2.1. Ha cht
26
2.2.2. Dng c 27
2.3. Phn tch c trng ca vt liu 27
2.3.1. Phng php nhiu x tia X (XRD)
27
2.3.2. Phng php chp nh SEM, EDS
27
2.3.3. Phng php chp TEM
27
2.3.4. Phng php phn tch nhit
27
2.4. tng hp xc tc Ag/CuO
28
2.4.1. Xc nh nhit nung cho qu trnh tng hp
28
2.4.2. Tng hp vt liu Ag/CuO t CuSO4 v AgNO3
30
2.4.3. Tng hp vt liu Ag/CuO t Cu v AgNO3
34
2.5. Th hot tnh xc tc
42
2.5.1. Th hot tnh xc tc phn ng phn hy vi H2O2 42
2.5.2. Th hot tnh khng khun
43
2.5.3. Th xc tc quang
44
CHNG 3. KT QU V THO LUN
45
3.1. kt qu nghin cu vt liu bng phng php nhiu x tia X
45
3.2. Kt qu chp nh SEM
52
3.3. Kt qu chp nh TEM
54
3.4. Kt qu chp ph tn x nng lng (EDS) 55
3.5. Kho st hot tnh xc tc ca vt liu Ag/CuO
56
3.5.1. Th hot tnh xc tc vi H2O2 56
3.5.2. Kt qu th hot tnh khng khun
62
3.5.3. Kt qu th xc tc quang
64
Kt lun
66
Ti liu tham kho
67

14

M u

Nu th k 20 c coi l th k ca cuc cch mng cng ngh thng tin th th k 21


h nano ang pht trin vi mt tc bng n v ha hn em li nhiu thnh tu k diu ch
i tng ca cng ngh nano l nhng vt liu c kch c nano mt (10-9 m). Vi kch
g tnh cht v cng c o m nhng vt liu c kch c ln hn khng c c nh bn c

in quang ni tri Chnh nhng tnh cht u vit ny m ra cho cc vt liu nano nhiu
hng, nng lng n cc vn sc khe, y t, mi trng, t cng ngh thm him v tr n
dng to ln nh vy, cng ngh nano c cc nh khoa hc d on s thay i c bn th gi
Nhn thc c vai tr, tm quan trng ca cng ngh nano v khng b tt hu so v
nc ta coi vic pht trin cng ngh nano l mt nh hng mi nhn v khoa hc cng ngh
ngh thng tin, cng ngh sinh hc, cng ngh vt liu, cng ngh mi trng Do vy, trong
v cng ngh nano Vit Nam cng pht trin v thu c nhng thnh cng bc u nh l
oxit phc hp, ng nano cacbon v ang nghin cu a cc sn phm ny vo ng dng trn
Trong s cc vt liu nano, ht nano ca cc kim loi qu c nghin cu nhiu hn c
nano bc nhn c s quan tm ch ca nhiu nh khoa hc cng nh cc nh doanh nghip. N
nano, ht bc kch thc nano cn c nhng tnh cht th v ring nh: tnh quang, tnh dn
i ho, kh nng dit khun, ty trng...V nhu cu v ht bc nano ngy cng cao nn nhiu ng
ano vi qui trnh n gin, hiu qu cao, kch thc ht nh mong mun.
Trong lun vn ny, chng ti chn ti Nghin cu tng hp, tnh cht v kh nn
trn cht mang ng oxit.
Chng 1. Tng quan
1.1. Cng ngh nano v vt liu nano
1.1.1. Cng ngh nano (nanotechnology)
Thut ng cng ngh nano xut hin t nhng nm 70 ca th k XX. C nhiu cch k
.
T in bch khoa ton th a ra nh ngha Cng ngh nano l ngnh cng ngh lin quan n
dng cc cu trc, thit b v h thng bng vic iu khin hnh dng kch thc trn cp
Cng ngh nano l mt khoa hc lin ngnh, l s kt tinh ca nhiu thnh tu khoa hc trn n
o gm ton hc, vt l, ha hc, y dc hc, sinh hc) v l ngnh cng ngh c nhiu tim n
Cng ngh nano bao hm mt s vn sau:
Tm hiu c s khoa hc ca ngnh cng ngh nano.
Nghin cu thit k, ch to cc cng c v phng php quan st, thao tc cp nan
Ch to v kim sot kch thc v tnh cht ca cc loi vt liu nano.
ng dng vt liu nano.
1.1.2. Vt liu nano
1.1.2.1. nh ngha [1]
Vt liu nano c nh ngha l vt liu c kch c t 1- 100 nm t nht mt chi
Vt liu nano c th tn ti ba trng thi: rn, lng, kh. Trong , vt liu na
ht, sau n vt liu lng v kh.
C th phn chia vt liu nano thnh 3 loi da trn hnh dng:
+ Vt liu nano ba chiu (hay cn gi l vt liu nano khng chiu) l vt liu c b
o mt. V d: m nano, dung dch keo nano, ht nano
+ Vt liu nano hai chiu l vt liu trong ch c hai chiu c kch thc nano m
+ Vt liu nano mt chiu l vt liu trong ch duy nht c mt chiu c kch th
nano
Vt liu nanocomposit l vt liu trong ch c mt thnh phn ca vt liu c k
n c nano ba chiu, hai chiu v mt chiu an xen nhau. V d: nanocomposit bc/silica, bc
trn cc cht nn.
1.1.2.2. c im, tnh cht ca vt liu nano
Mt c im quan trng ca vt liu nano l kch thc ht v cng nh b, ch
. Do vy, s nguyn t nm trn b mt ca vt liu nano ln hn rt nhiu so vi cc vt li
Nu vt liu khi thng thng, ch mt s t nguyn t nm trn b mt, cn phn
b cc lp ngoi che chn th trong cu trc vt liu nano, hu ht cc nguyn t u c
vy, din tch b mt ca vt liu nano tng ln rt nhiu so vi vt liu thng thng. Ni
mt, mi nguyn t c t do th hin ton b tnh cht ca mnh trong tng tc vi mi tr
no nhiu c tnh ni tri, c bit l tnh cht in, quang, t, xc tc
Kch thc ht nh b cn l nguyn nhn xut hin vt liu nano 3 hiu ng: hi
h thc.
+ Hiu ng lng t
i vi cc vt liu v m gm rt nhiu nguyn t (1m3 th tch vt liu c khon
ng bnh cho tt c cc nguyn t, v th v ta c th b qua nhng khc bit ngu nhin ca t
rung bnh ca chng. Nhng i vi cu trc nano, do kch thc ca vt liu rt nh, h c r
r hn v khng th b qua. iu ny lm xut hin vt liu nano cc hin tng lng t k
ht quang phi tuyn ca vt liu, hiu ng ng ngm

+ Hiu ng b mt [23, 30]


vt liu nano, a s cc nguyn t u nm trn b mt, do vy m din tch b mt ca v
truyn thng. V th, cc hiu ng c lin quan n b mt nh: kh nng hp ph, hot n
g khi. iu ny m rng ng dng k diu cho lnh vc xc tc v nhiu lnh vc khc m c
Kch thc ca vt liu nano c tri rng. V d nu ta c mt qu cu c bn knh bng qu
hc 10 nm. Nu ta xp cc ht thnh mt hng di k tip nhau th di ca chng bng
+ Hiu ng kch thc
Cc vt liu truyn thng thng c c trng bi mt s cc i lng vt l, ha
, tnh axit Tuy nhin, cc i lng vt l v ha hc ny ch l bt bin nu kch thc c
kch thc ca vt liu xung n thang nano (nh hn 100 nm) th cc i lng l, ha tr
ay i theo kch thc. Hin tng ny gi l hiu ng kch thc [2]. Kch thc m , v
tr ca mt kim loi kch c v m m ta thy hng ngy tun theo nh lut Ohm. Nu ta gim
qung ng t do trung bnh ca in t trong kim loi (thng t vi nano mt n vi trm
Lc in tr ca vt liu c kch thc nano s tun theo cc qui tc lng t.
Cc nghin cu cho thy cc tnh cht in, quang, t, ha hc ca cc vt liu u
1 nm n 100 nm nn cc tnh cht ny u c biu hin khc thng th v vt liu nano so

1.1.3. Cc phng php tng hp vt liu nano [1, 2]


Hai phng php c bn tng hp vt liu nano v nano compozit l phng php t
php t di ln (bottom-up). Phng php t trn xung l phng php to ht kch thc na
ln l phng php hnh thnh ht nano t cc nguyn t hoc ion.
1.1.3.1. Phng php t trn xung (top-down)
Phng php t trn xung l phng php dng k thut nghin v bin dng bin v
a. Phng php nghin
Vt liu dng bt c trn ln vi nhng vin bi c lm t cc vt liu rt cn
hin rung, hoc nghin quay. Cc vin bi cng va chm vo nhau v ph v bt n kch thc n
o khng chiu.
b. Phng php bin dng
Phng php bin dng c th l n thy lc, tut, cn, p. Nhit c th c i
it phng th gi l bin dng nng, cn nhit nh hn hoc bng nhit phng th gi
hoc 2 chiu.
Nhn chung, phng php t trn xung l phng php n gin, r tin nhng hiu qu
hin, tnh ng nht ca vt liu khng cao v do vy, phng php t trn xung t c dng
1.1.3.2. Phng php t di ln (bottom-up)
Ngc li vi phng php t trn xung, phng php t di ln hnh thnh vt li
u im ca phng php ny l tng hp c vt liu nano vi kch thc nh ng
ny. N c th l phng php vt l, ha hc hoc kt hp c hai phng php.

a. Cc phng php vt l
y l phng php to vt liu nano t nguyn t hoc chuyn pha.
+Phng php chuyn pha
Vt liu c un nng ri lm ngui vi tc nhanh thu c trng thi v nh hn
hnh sang cu trc tinh th. Phng php ny cn c gi l phng php lm ngui nhanh.
+ Phng php bc bay nhit
Vt liu c t, hoc dng tia bc x hay phng h quang lm bay hi vt liu. Sau
h c kch c nano. V d, trong phng php phng in h quang, ngi ta dng mt bnh chn
, trong bnh c hai in cc ni vi mt in th ln. Khi mi cho phng in s xy ra hin
ant b in t bn ph lm cho cc nguyn t y bc bay ln (bc bay nhit), b mt in
lp vt liu bay sang t ant. Thnh phn ca cht lm in cc nh hng n thnh phn cu
yu dng bt mn.
Cc phng php iu ch vt liu nano nh trn thng yu cu nhng thit b phc tp,
c kch thc ht phc v cho nhng ng dng khc nhau.
b. Phng php ha hc
Phng php ha hc l phng php ch to vt liu nano t cc ion hoc nguyn t. y l
v nano compozit. u im ca phng php ny l c th tng hp c tt c cc dng vt li
thm ch l cc cu trc nano phc tp m phng sinh hc. Hn na, phng php ny cn cho
ano vi kch thc nh hn nh mong mun vi ng u cao.
+ Phng php kh ha hc
phng php kh ha hc, mui ca kim loi tng ng c kh vi s c mt ca c
keo t ca chng [13, 14, 16].

u im ca phng php ny l qui trnh thc hin n gin, khng i hi cc thi


v cho php vt liu vi lng ln.
Phng php ny ch yu to ra cc ht nano kim loi.
+ Phng php s dng ht nano c sn trong t nhin
Cc cht c sn trong t nhin nh zeolit, cc ht st, cc phn t sinh hcc rt
nano compozit.
+ Phng php s dng mng a in ly (Polielectrolyte)
Mt s mng cc cht a in ly thng c dng tng hp vt liu nano v nano
AA), polyanlylamin hiroclorua (PAH), polietylenimit (PEI). Cc mng ny c cc nhm cacbonyl
hoc cc nguyn t nit mang in tch m nn s hp th v to vi cc ion kim loi cc phc
kh thch hp s c s dng kh cc ion kim loi. Cc sn phm thu c l cc mng cu
+ Phng php sol-gel [1, 25]
Phng php sol-gel do R.Roy xut nm 1956. u im ca phng php ny l d i
ht nh.
Phng php sol-gel thng c dng tng hp cc vt liu nano dng bt, si,
Phng php sol-gel trong nhng nm gn y pht trin rt a dng, qui t thnh mt
Phng php sol-gel theo con ng thy phn cc mui.
Phng php ny xut pht t cht u l cc mui nitrat, cloruaCc ion kim loi t
hc aquo. Phc aquo b thy phn to aquohidroxo.
[M(H2O)n]z+ + hH2O
[M(OH)h(H2O)n-h](z-h)+ + hH3O+
Cc phc aquohidroxo n nhn ngng t thnh phc a nhn ri tip tc pht trin m
Phng php sol-gel theo con ng thy phn cc alkoxit.
Trong phng php ny, cc hp cht alkoxit thng ha tan vo dung mi hu c khan
o thm vo mt lng nc.
S to thnh sol, gel rt phc tp nhng c th tm tt bng ba qu trnh sau:
- Thy phn cc alkoxit kim loi M(OR)n
M(OR)n
+
xH2O
M(OH)x(OR)n-x
+
xROH
- Qu trnh trng ngng
+ Phn ng loi nc
- M-OH
+
HO- M-M-O- M+
H2O
+ Phn ng loi ru
-M-OH
+
RO-M-M-O-M
+
ROH
- Qu trnh gel ha
Cc on polime ni vi nhau thnh khung ba chiu. n mt lc no , nht tn
h gel, nc v ru nm trong cc l ca gel.
Phn ng phn hy gel s xy ra nhit thp, cho sn phm c ng nht v tinh k
iu chnh tc thy phn v tc ngng t, c th khng ch c kch thc ht v hnh
Phng php ny c bit thun li trong vic ch to vt liu oxit.
1.1.4. Tnh cht ca ht nano kim loi [4]
Nh phn u ni, ht nano kim loi c hai tnh cht khc bit so vi vt liu khi l
do c im cc ht nano c tnh kim loi, tc l c mt in t t do ln nn cc tnh ch
mt in t t do cao.
a. Tnh cht quang hc
Tnh cht quang hc ca ht nano vng, bc trn trong thy tinh lm cho cc sn phm t thy
au c ngi La M s dng t hng ngn nm trc. Cc hin tng bt ngun t hin t
nce) do in t t do trong ht nano hp th nh sng chiu vo. Kim loi c nhiu in t t
dng ca in t trng bn ngoi nh nh sng. Thng thng cc dao ng b dp tt nhanh c
nt mng tinh th trong kim loi khi qung ng t do trung bnh ca in t nh hn kch th
oi nh hn qung ng t do trung bnh th hin tng dp tt khng cn na m in t s d
cht quang ca ht nano c c do s dao ng tp th ca cc in t dn n t qu trnh t
phn b li trong ht nano lm cho ht nano b phn cc in to thnh mt lng cc in. Do
vo nhiu yu t nhng cc yu t v hnh dng, ln ca ht nano v mi trng xung quanh
ht nano cng nh hng n tnh cht quang. Nu mt long th c th coi nh gn ng
rnh tng tc gia cc ht.
b. Tnh cht in
Tnh dn in ca kim loi rt tt, hay in tr ca kim loi nh nh vo mt in t t d
trn cu trc vng nng lng ca cht rn. in tr ca kim loi n t s tn x ca in t
o ng nhit ca nt mng (phonon). Tp th cc in t chuyn ng trong kim loi (dng in
vi nhau thng qua nh lut Ohm: U = IR, trong R l in tr ca kim loi. nh lut Ohm

h. Khi kch thc ca vt liu gim dn, hiu ng lng t do giam hm lm ri rc ha cu tr


ny i vi ht nano l I-U khng cn tuyn tnh na m xut hin mt hiu ng gi l hiu
de) lm cho ng I-U b nhy bc vi gi tr mi bc sai khc nhau mt lng e/2C cho U v e
in t, C v R l in dung v in tr khong ni ht nano vi in cc.

c. Tnh cht t
Cc kim loi qu nh vng, bc,... c tnh nghch t trng thi khi do s b tr cp in
r trn s khng ton din na v vt liu c t tnh tng i mnh. Cc kim loi c tnh s
, coban, niken th khi kch thc nh s ph v trt t st t lm cho chng chuyn sang trn
trng thi siu thun t c t tnh mnh khi c t trng v khng c t tnh khi t trng b
g.
d. Tnh cht nhit
Nhit nng chy Tm ca vt liu ph thuc vo mc lin kt gia cc nguyn t trong mn
guyn t c mt s cc nguyn t ln cn c lin kt mnh gi l s phi v. Cc nguyn t tr
uyn t bn trong nn chng c th d dng ti sp xp c th trng thi khc hn. Nh
s gim. V d, ht vng 2 nm c Tm = 500C, kch thc 6 nm c Tm = 950C.
1.1.5. ng dng ca vt liu nano v cc ht nano kim loi [5]
a. Cng ngh in t cng ngh thng tin
S ra i ca my tnh in t m ra cuc cch mng khoa hc cng ngh thng tin vi nhng
ui th k XX cho n nay. Tuy nhin, cc linh kin my tnh s dng cng ngh ny tim c
, chng tr nn qu t . Nu khng tm ra c bin php thay th hu hiu, cc linh kin
heo tc pht trin rt nhanh ca cng ngh thng tin. Cng ngh nano a ra mt gii ph
hnh l chm lng t. Chm lng t l mt ht (bn dn, kim loi, polyme) c bn knh c v
my tnh vi cc chm lng t gi l chp nano c tch hp rt cao, trin vng cho php
cha thng tin t tt c cc th vin trn th gii trong mt thit b nh nh mt vin ng
b. C kh, vt liu
Cc ng nano cacbon l loi vt liu nano c rt nhiu ng dng trong thc t. Do c cu trc
on cc k vng chc, c bn c hc gp 10 ln thp v c bit c tnh bn nhit rt cao,
hch hp sn xut cc thit b cho ngnh sn xut xe hi, my bay tu v tr. Cng do c
dy tc tng tui th cho bng n ln n vi chc nm. Cc ng nano cacbon ang c ngh
mn hnh my tnh, mn hnh in thoi di ng...
Mt s vt liu nh gng, knh, sn, gch men... khi c trng mt lp mng nano TiO2 s c
kh nng xc tc quang ha ca TiO2 s lm cho cc cht bm bn d dng b oxi ha bi oxi kh
b ra tri.
Do tnh cng, kh nng chu mi mn, bn cao nn cc vt liu nano c dng ch to nh
hng.
Vi din tch b mt ln, cc ht nano ZnS, CdS c dng lm cht pht quang trong cc mn h
loi t him kch thc nano nh Yt, Sm, Co c dng trong nam chm t tnh to t trng
c. Y t v sc khe
Mt trong nhng ng dng c mong ch nht ca cng ngh nano l ch to c cc thit b
on ngi, m bo thuc khng gy nh hng n nhng t bo khe mnh khc gy ra tc dn
vic ny. Cc ht nano t ny c th c ch to sao cho c th lin kt vi cc phn t c
tr l xe ti ko r - mooc l cc phn t thuc. Sau ch cn dng t trng hng cc
g Quc tuyn b pht minh ra v th nghim thnh cng trong phng th nghim mt thit b
huyn trong mch mu ngi v th thuc vo ng ni thy thuc quy nh. Thit b sau tho
M v tp ch c Angew. Chemie cng b v nh gi cao pht minh ny.
Cc nh khoa hc M cng ang ch to ra cc phng th nghim siu nh c th nm gn trong l
g phng th nghim ny c th cho ngay nhng kt qu phn tch ni bnh.
d. Nng lng, mi trng
Nh cng ngh nano, nhng loi pin mi c kh nng quang hp nhn to s gip con ngi sn x
no, ngi ta cng c th to ra nhng thit b t tiu tn nng lng hn do s dng nhng lo
Cc mng nano (vi chi ph sn xut thp) ha hn c th hp th c nhiu nng lng mt tr
hi u cho mt cuc cch mng trong vic s dng nng lng mt tri.
Cc cht lm sch mi trng cng ang l vn c quan tm. Cc my lc to bi ng cacbo
mt b ngang c kh nng lc c cc vi khun v vi rt trong nc ung. Cng ngh nano gi
e. An ninh quc phng
Cng ngh nano cng ng vai tr rt quan trng trong lnh vc quc phng. Nhng thit b k
kh nguy him hn c bom nguyn t. Vi mt i qun nh b khng th pht hin bng mt th
th tiu dit c k th ch trong chp nhong. y cng l mt vn ht sc thn trng tr
Ngoi nhng ng dng c bn trn, cng ngh nano cn c nhiu ng dng quan trng trong nhiu

nng nghip... Trn c s khoa hc v thc tin thu c, ta c th thy rng chc chn c
ha tng c trong khoa hc v i sng.

1.2. bc v nano bc
1.2.1. Gii thiu v kim loi bc
Bc (Ag) nm th 47 trong bng tun hon cc nguyn t ha hc, thuc nhm IB [10]. Cu
t bc cc phn lp ngoi cng l 4d105s1.
Bc kim loi kt tinh dng lp phng tm din, c bn knh nguyn t l 1,44Ao.
Bc l kim loi nng, mm, c nh kim, mu trng, c hai ng v bn l 107Ag(51,9%) v 109Ag
Nhit si, nhit nng chy v nhit thng hoa ca bc cao hn nhiu so vi hu ht c
ng s tt c cc kim loi. Bc cng vt xa cc kim loi khc v tnh do, d dt mng v d
V mt ha hc, bc l kim loi rt km hot ng. Bc khng tc dng vi xi khng kh k c
Bc c bit n nh mt kim loi c kh nng dit khun t kh sm. Trong lch s
nc ung, x l mi trng, y t v ngn chn s pht tn dch bnh. Cch y khong vi tr
nh l mt dch keo, v vy keo bc c s dng lm cht khng khun ngay trong c th con n
dit khun mnh nht tn ti trong t nhin, c s dng rng ri bng cch ung hoc tim v
thng, vt bng, cc bnh ng tiu ha v rng ming, lm thuc nh mt v.v... c rt
in y hc, trong c th nu ra mt s ch phm in hnh nh collargol hoc protargol. Cc
r cc bnh nhim trng thng gp nh thng hn, dch t, vim mng no, bnh tai mi hng,
dy v cc bnh lin quan n phu thut nh nhim trng vt thng, p xe, rut tha, vim t
k XX sau khi thuc khng sinh c pht minh v a vo ng dng vi hiu qu cao hn, ng
i tr cha bnh ca bc na. Nhng nhng nm gn y do ngy cng xut hin nhiu loi vi kh
s ch vo kh nng dit khun c bit ca bc do n c ph tc dng rng v khng b rng
1.2.2. Bc nano v tnh u vit ca bc nano so vi bc ion v bc khi
Nano bc l tp hp ca cc nguyn t bc c kch thc t 1 ti 100 nm thng c ch to
Nano bc mang y tnh cht ca bc khi nh dn in, dn nhit, kh nng xc tc, tnh
nano c nhiu tnh khc bit so vi bc kim loi nh cc c tnh ca nano nh din tch b
cc dung mi. in hnh nh kh nng dit khun, xc tc tt hn h n so vi bc kim loi hay
rt nhiu gp phn tit kim chi ph sn xut [12].
Kh nng khng khun xut hin c bc kim loi, bc ion v bc nano bi chng u c th gi
nhng ion ny ng vai tr l cht dit khun [28]. Nhng khi trng thi bc khi, lng io
s dng dung dch ion bc dit khun th thi gian tc dng ngn do tnh khng bn ca io
din tch b mt ring rt ln l mt h gii phng ion bc tt, cc ion bc c gii phng
lu di [18, 24].
1.2.3. Cc phng php iu ch nano bc
Ngi ta c th s dng cc quy trnh khc nhau cng nh cc iu kin khc nhau:
, sy, nung iu ch bc nano vi kch c khc nhau phc v cho nhng mc ch khc nha
cc vt liu nano khc, bc nano ch yu c tng hp bng hai phng php vt l v phng
h c bit kh rng ri trn th gii.
Phng php kh ho hc
- Phng php kh ho hc l phng php ph bin trong vic iu ch cc ht keo b
- Nguyn tc kh mui bc (thng l AgNO3) di s c mt ca mt tc nhn bo v t
v cc cht hot ng b mt) khng ch qu trnh ln ln v tp hp ca cc ht keo bc.
nhn bo v v cc iu kin th nghim (nng dung dch, nhit ) [13].
- Tc nhn kh ng vai tr quan trng trong qu trnh iu ch. mnh yu ca tc
ca ht nano to thnh. Nu cht kh qu mnh, qu trnh kh din ra nhanh, s lng ht keo
c bo v th d dng bin keo t thnh cc ht c kch thc ln. Nu cht kh s dng qu
h ra nhiu qu trnh trung gian v cc sn phm khng mong mun. Cc tc nhn kh thng dng
ormanhit, natribohydrua, hydrazin, gluco [23].
Cc tc nhn kh va l cht bo v va l cht kh li ng vai tr dung mi l thch hp nh
Cht bo v thng c s dng l cc polime mch di, cc cht hot ng b mt, thiol mch
VA, PEG [27] Cc cht bo v ny c th l cht c lp khi thm vo hn hp phn ng nhng
h ra trong qu trnh phn ng hoc cc mui bc ban u cha phn ng ht. Vai tr ca chng
cc ht bc nano to thnh [16].
C nhiu kin gii thch khc nhau v vai tr ca cht bo v nhng im chung u cho l c
v ngoi vi cc tc nhn ny, lm gim nng lng t do b mt ht nano. Phn t cc tc nh
PVA, xenluloz gn trn cc polime c i lc mnh vi Ag+ hay nguyn t Ag kim loi. Cc h
h thnh trn khun polime nh vy c ngn cch vi nhau v khng th kt t c vi nha
, do d to kch thc nh v ng u.
Ngoi ra, cc ht bc nano cn c bo v theo quy ch lm bn ca cc ht keo. Khi ion Ag+

h trn b mt ht v c to thnh cc mixen gm nhn bc, mt lp cht bo v v lp m k


ang in tch tri du v y nhau trnh hin tng keo t.
Ngoi ra cc yu t nh pH, nng cht tham gia phn ng, nhit ca phn ng, tc , th
to thnh. V d khi pH qu ln s xy ra qu trnh to thnh Ag2O nn kh khng ch phn ng
lm mng lp in kp bao ngoi ht nano lm cc ht nano d tp hp. Khi nng thp, tc
to thnh thng nh v ng u hn.
Phng php ny c u im l d thc hin, d khng ch cc iu kin phn ng nhng ch th
bt mn. Dng bt mn khi thu li cng khng bn bng dung dch keo ca n.
Phng php s dng mng cht a in ly
Lp mng ca cht a in ly c c im c nhiu nhm mang in tch tri du. Mt s cht
Polyallylamin hidroclorua (PAH), Polyetylenimit (PEI) [19, 25]. Do c im ca cc mch cht
ly l mch di nn chng c th hnh thnh cc h tch in m kch c nano mt bi cc nhm
h ion Ag+ to thnh phc bn trn mng. Sau ta s dng cc cht kh thch hp kh ion
hc ht c ng u cao v nh.
Phng php Polyol
C th dng etylen glycol (PEG) v cc iol lm cht kh nhit cao trong s c mt ca
[11]. Qua nghin cu ngi ta thy rng kh nng kh PEG nhy hn, n li c mch cacbon di
ht bo v trong qu trnh phn ng.
Phng php phn hu nhit.
Trong phng php ny ngi ta thng s dng mt mui ca bc v axit hu c thng l cc h
mui nhit di 3000C trong vng 2 gi ta s thu c tinh th bc nano vi kch c
Phng php ny n gin, t c, tn t ho cht, thi gian phn ng thp, d dng to ra l
mt khong hp v thng di dng tinh th.
Ngoi cc phng php trn cn c phng php khc nh dng sng siu m, quang ho hay phn
1.2.4. ng dng ca nano bc
Vt liu bc nano va kt hp c nhng tnh cht u vit ca vt liu nano, va
im loi nn c rt nhiu ng dng trong i sng nh:
a. ng dng trong cng nghip in t (kh nng dn in, truyn quang)
Do kh nng dn in tt m nano bc c s dng lm cht truyn dn trong nhng vi mch i
nh xung v cht lng th ngy cng tt hn.
b. ng dng hot tnh dit khun
c nhiu cng trnh khoa hc nghin cu gii thch hot tnh khng khun ca bc [18,28].
v ion bc tn cng vo vi sinh vt nh th no vn ang c tip tc nghin cu. Hin nay t
khun ca bc. Cc quan im ny ch yu da trn s v hiu ha nhm thiol trong men vn chu
n s ime ha pyridin v cn tr qu trnh sao chp DNA ca t bo vi khun. Cc nh khoa
Quc [5] cho rng bc tc dng ln mng bo v ca t bo vi khun. Mng ny l mt cu trc
cu ni axit amin to cng cho mng: cc protein c gi l peptidoglican. Cc ion bc
ican v c ch kh nng vn chuyn oxy ca chng vo bn trong t bo dn n lm t lit vi
ngay sau th kh nng hot ng ca vi khun c th li c phc hi. Cc t bo ng v
i sinh vt vi hai lp lipoprotein giu lin kt i c kh nng cho in t, do khng cho
chng khng b tn thng khi tip xc vi cc ion ny.
Ngoi ra, cc ion bc cn c kh nng c ch qu trnh pht trin ca vi khun bng cch s
b mt ca ht bc:
2Ag+
+
O22Ago
+
Oo
Theo cc nh khoa hc Nga, hin nay c nhiu l thuyt v c ch tc dng dit vi khun c
ph c nhiu ngi chp nhn hn c. Bn cht ca thuyt ny l ch t bo vi khun b v
mt mang in tch m ca t bo v ion Ag+ c hp ph ln , cc ion ny sau xm nhp
Cho n nay mi ch c mt quan im lin quan n c ch tc ng ca nano bc l
a hc tha nhn. l kh nng dit vi khun ca ht nano bc, l kt qu ca qu trnh chuy
ion Ag+ t do v cc ion t do ny sau tc dng ln v tr mang in tch m trn vi khun
ln vi sinh vt vn cha hon ton sng t, nhng a s cc nh nghin cu c cng quan im
hp hoc ph hy chc nng ca t bo, hoc lin kt vi DNA ca t bo vi sinh vt v ph h
Nano bc c th s dng dng dung dch lm cht dit khun trc tip hay a vo
phm mi c kh nng khng khun rt tt. Chng c ph dit khun rng v khng nh hng ti
h vc khc nhau.
Trong y hc ngi ta dng nano bc lm cc loi bng gc y t (gc cha
g c phu thut, dung dch ty trng v mt s dc phm.
Trong may mc ngi ta c th to ra vi c cha nano bc gip cho loi vi mi ny c kh n
g gim kh nng bm bn ca vi. [9]
Nh tnh nng kh khun ca nano bc v tc dng lc mi, lc kh c ca t

ano bc c sn xut ha hn ngn nga cm A/ H1N1.

Hnh 1.1: Khu trang nano bc nga cm H1N1.


Trong xy dng s dng sn nano bc c kh nng t dit khun chng bm bn, d lau
Trong nng nghip ngi ta to ra dung dch thuc bo v thc vt t nano bc c
hng ti sc khe con ngi.
ng dng ca ht bc nano sn xut hng tiu dng: trong sinh hot hng ngy cc
nh t lnh, iu ha nhit , bnh lc nc, bnh sa... vi tc dng chnh l chng khun.
Mt s hnh nh ng dng thc t ca nano bc [9]:
Hnh 1.2. Bnh sa ph nano bc.
Hnh 1.4. ng thc phm ph nano bc.

Hnh 1.3. Dung dch ra nano bc.


Hnh 1.5. Kem m phm cha nano bc.

Hnh 1.6. Vi tm nano bc.


Hnh 1.7. Tt khng mi (ph nano bc).
1.3. Gii thiu v CuO v xc tc ag/cuo
Trong cng trnh nghin cu [29] cc tc gi cho bit CuO c iu ch bng vic
lm kt ta Cu(OH)2. Ngi ta nghin cu qu trnh lm kh v qu trnh nung ca kt ta
ot tnh xc tc ca n nu phi ra ngoi khng kh, do nh hng ca s hp th hi nc.
CuO l cht bn dn vi di gii hn 1,2 eV, CuO c cc tnh cht quang, in, xc
c s dng trong mt s lnh vc nh:
- Phn ng oxi ha CO thnh CO2 c tin hnh bi xc tc CuO[31].
- Vi din tch b mt ln, n nh cao, gi thnh sn xut thp do tnh cht dn i
cho vic lm vt liu catt ca t bo pin mt tri [29].
- H2O2 c kh nng phn hu ra oxi nhit thng nn c s dng nh nhin liu sc
phn hu H2O2 l CuO kch thc nano [20].
Tuy vy, nhiu nghin cu cn cho thy CuO nguyn cht c hot tnh xc tc khng
compozit nh CuO/Fe2O3 v Cu2(OH)3Cl/CuO, Ag/CuO c hot tnh xc tc cao hn [21]. Tuy nhi
rnh tng hp l qu trnh phc tp v s kt ta ca cc ht nano iu chnh khng d dng.
Qu trnh tng hp ca nano Ag/CuO l s kt hp cc hp cht ng trong dung dch
qu trnh tng hp l loi b cc anion, kt qu l thi gian thc hin di v gi sn phm c
nion kch thc cc tiu phn tng v s kt t ca sn phm v do lm kh nng xc tc b
iu nano Ag/CuO c iu ch t ng kim loi, oxi khng kh v NH3 l tc nhn phi tr. Tr
rong mi trng NH3, sau thm Ag2CO3 v NH4HCO3 kt ta ng thi c ng v bc di d
ny khng a thm anion vo dung dch h phn ng, v vy khng cn qu trnh lm sch sn p
1.4. Mt s phng php nghin cu vt liu nano
1.4.1. Phng php nhiu x tia X [3]
Phng php nhiu x tia X cung cp cc thng tin v thnh phn pha v cu trc ca vt liu.
i vi kch thc v hm lng cc cht c trong vt liu.
Khi chiu mt chm tia X vo tinh th, in t trng ca tia X s tng tc vi
tinh th. Cc tia khuych tn t tng tc ny c th giao thoa vi nhau. Nu gi gc ti ca
h l th s giao thoa ch c th xy ra nu phng trnh Bragg c tha mn:
2dsin = n
Trong : d l khong cch gia hai mt ph ng mng (hkl) lin tip
,
l bc sng v gc nghing ca tia phn x

Hnh 1.8. S phn x tia X trn b mt tinh th.


Nh vy, vic o cc cc i nhiu x tia X theo gc
khc nhau s cho php xc nh c h
Trn my chp ph nhiu x tia X, mt chm in t c tng tc trong in trng v p vo
tot l mt di c vch c trng. Mt vch s c tch ra bng knh lc v tia X thu c co
hm song song chiu vo mu. Mu c mang ln cc tm trn v c gn ln gi. Gi ny c t
hng gc xc nh. My m ghi nhn nhiu x (detector) c kt ni vi gi ng mu bng m
hng ng b vi nhau detector c th ghi nhn c tt c cc tia nhiu x di cc gc
iu x . Sau khi ghi ph, my s so snh vi th vin cc ph chun xc nh cc pha tro
C th tnh c kch thc tinh th trung bnh ca ht bng cng thc Debye- Scherrer:
Trong :
d l kch thc ht trung bnh (nm).
 bc sng tia X.
 gc ti pc cc i.

l rng na vch ph ca pc cc i (rad).


Cng thc Deye- Scherrer thng c p dng i vi cc ht hnh cu. y ch l cng thc
hc ht. Tuy nhin, cng thc trn vn c th s dng hiu qu trong vic nghin cu an u
1.4.2. Phng php phn tch nhit [8]
Phng php phn tch nhit cung cp nhng thng tin v tnh cht nhit v thnh p
Trn gin phn tch nhit c n ng c n.
ng T: ghi li s bin i n thun v nhit ca mu theo thi gian. N ch
ng TG: cho bit bin thin khi lng ca mu trong qu trnh nung nng. N c
phn ca mu khi xy ra hiu ng nhit.
ng DTG: ghi li o hm s thay i khi lng ca mu theo nhit . N ch
l s thay i khi lng ca mu.
DTA: ghi li s bin i nhit ca mu theo thi gian so vi mu chun. N c
hit) v cc cc tiu (ng vi hiu ng thu nhit).
Kt hp cc d liu thu c t vic phn tch 4 ng trn, ta s c cc thng tin
nghin cu.
1.4.3. Knh hin vi in t truyn qua
(Transmission electron microscope TEM)
Hin vi truyn qua (TEM) [1] l phng php cho php s dng chm tia electron n
uan st cc vt th rt nh. phng i ca TEM l 400.000 ln i vi nhiu vt liu v th
h v phng x rt ln, TEM l cng c c lc trong vic nghin cu cc vt liu nano.

Hnh 1.9. S nguyn l hot ng ca knh hin vi in t truyn qua.


Nguyn l lm vic ca my TEM c m t nh sau: chm electron c to ra t ngun sau khi
li thnh mt dng electron hp. Dng electron ny tng tc vi mu v mt phn s xuyn qu
mt thu knh v to nh. nh sau s c truyn n b phn phng i. Cui cng tn hi
php ngi dng quan st c nh. Phn ti ca nh i din cho vng mu cn tr, ch ch
cao). Phn sng ca nh i din cho nhng vng mu khng cn tr, cho nhiu electron tru
nhit thp).
nh TEM thu c s l hnh nh mt ct ngang ca vt th. nh TEM c th cung cp
, kch thc ca vt liu nano.
Tuy c u im l phng i v phn gii cao nhng TEM khng th hin c
hp vi knh hin vi in t qut (SEM) pht huy u im ca c hai phng php ny.
1.4.4. Knh hin vi in t qut (Scanning electron Microscope SEM) [1, 8]
So vi TEM th SEM c phng i nh hn, ch vo khong 100.000 ln. Tuy nhi
l n cho php thu c hnh nh ba chiu ca vt th v do vy thng c dng kho st

Hnh 1.10. S nguyn l hot ng ca knh hin vi in t qut.


Chm electron hp sau khi i ra khi thu knh hi t s c qut ln b mt mu. Cc electr
tp hp cc ht th cp i ti detector. Ti y cc electron s c chuyn thnh tn hiu
tia catot v c qut ln nh. Cc vng ti v sng trn nh ph thuc vo s cc ht th c
ra ca cc electron sau khi tng tc vi b mt mu. Chnh v th m nh SEM thu c phn
1.4.5. Ph tn x nng lng (EDS)
Trong cc my chp SEM, ngi ta thng ghp thm mt modun tn x nng lng E
lectron tng tc vi mu s pht ra cc tia X c trng ca cc nguyn t. My o ph tn x
cng ca ph tn x nng lng cho php xc nh cc nguyn t v hm lng ca chng c
CHUNG 2. THC NGHIM
2.1. i tng, ni dung v phng php nghin cu
Mc tiu ca lun vn l nghin cu cc qu trnh tng hp xc tc Ag/CuO c kc
ca n. Do vy, chng ti s tin hnh tng hp xc tc Ag/CuO theo mt s qui trnh khc nh
.
Tng hp bt xc tc Ag/CuO kch thc nano t mui CuSO4 v AgNO3 theo cc phng ph
- Phng php ng kt ta (quy trnh 1).
- Phng php tm (quy trnh 2).
Tng hp bt xc tc Ag/CuO t Cu kim loi v AgNO3 theo ba quy trnh sau:
- Phng php ng kt ta (I) (quy trnh 3).
- Phng php ng kt ta (II) (quy trnh 4).
- Phng php tm (quy trnh 5).

Cc sn phm thu c theo 5 qui trnh iu ch c:


Nghin cu c trng ca vt liu bng cc phng php vt l khc nhau.
Nghin cu kh nng xc tc ca cc sn phm thu c.
Th hot tnh khng khun ca mt s mu i din.
2.2. ha cht - dng c
2.2.1. Ha cht
Bng 2.1. Ha cht s dng trong qu trnh thc nghim.
Ha cht
Xut x c im
AgNO3 Nga
Dng tinh th, ha cht tinh khit
CuSO4 Trung Quc
Dng tinh th ngm nc.
Na2CO3 Trung Quc
Dng tinh th, ha cht tinh khit.
Cu
Trung Quc
Dng bt tinh khit.
NH4HCO3 Trung Quc
Dng tinh th, ha cht tinh khit.
(NH4)2CO3
Trung Quc
Dng tinh th, ha cht tinh khit.
Dung dch NH3 Trung Quc
Nng 28%.
Dung dch H2O2 Trung Quc
Nng 30%.
Xanh metylen
Trung Quc
Dng tinh th, ha cht tinh khit.
2.2.2. Dng c
Cc chu nhit 100ml.
Pipet 5ml, 10ml, 15ml, 20ml.
a thy tinh.
Chn nung.
ng li tm.
Ci nghin m no.
Cn phn tch Mettler Toledo.
My li tm Hettich EBA 8 (Prolado- Php).
My khuy t HC 502 (Anh).
T sy chn khng.
L nung.
2.3. cc phng php nghin cu tnh cht ca vt liu
2.3.1. Phng php nhiu x tia X (XRD)
xc nh thnh phn pha ca mu sau khi tng hp c, chng ti dng phng php
ADVANCE (Brucker, c) ti phng th nghim Ho Vt liu, Khoa Ho Hc, Trng HKHTN HQGH
g ng, gc 2 quay t 30o 70o, vi tc 0,030o/step.
2.3.2. Phng php chp nh SEM, EDS
nh SEM ca mu c chp trn my JMS 5810 ca hng Jeol (Nht Bn) v EDS ca h
Ha Hc Vin Khoa Hc v Cng ngh Vit Nam.
2.3.3. Phng php chp TEM
xc nh hnh dng v kch thc ca mu, chng ti tin hnh chp nh TEM trn
o ti Vin V Sinh Dch T Trung ng.
2.3.4. Phng php phn tch nhit
Gin phn tch nhit ca mu c ghi trn my phn tch DTA, TG - labsys TG/DSC
ung tm Ha Hc Vt liu, Khoa Ha Hc -Trng HKHTN vi tc t nng 10oC/pht trong mi
2.4. tng hp xc tc ag/cuo
2.4.1. Xc nh nhit nung cho qu trnh tng hp
Trong tt c cc qui trnh iu ch, chng ti u chuyn v dng hp cht Ag2CO3
hp cht trn phn hy nhit to thnh Ag/CuO. Do vy, tm nhit nung ti thiu chng t
g Cu2(OH)2CO3 v hai mu c bc M 2.1.6 nung cc kt ta dng Ag2CO3 vi Cu2(OH)2CO3, M 2.
g kt ta dng AgNO3 v Cu2(OH)2CO3 ghi li gin phn tch nhit.
Kt qu nh sau:

Hnh 2.1. Gin phn tch nhit ca mu MT1


Nhn vo gin phn tch nhit ca mu MT 1 ch cha Cu2(OH)2CO3
hnh 2.1 thy:
+ Trn ng DTA c mt hiu ng thu nhit yu 84,13o C, l hiu ng mt n
+ Trn ng DTA c mt hiu ng thu nhit mnh 285,04oC, tng ng vi hiu ng ny l hi
it Cu2(OH)2CO3.
Nhn vo ng TG thy khong 2000C bt u xy ra qu trnh phn hy, trn 300oC qu trnh
trnh phn hy 400oC nhng v tc gia nhit nhanh nn thc t nhit phn hy ca mu
+ Phng trnh phn ng phn hy.

Cu2(OH)2CO3

2CuO + H2O + CO2

Hnh 2.2. Gin phn tch nhit ca mu M 2.1.6


Nhn vo gin phn tch nhit ca mu M 2.1.6 c cha Ag2CO3 v Cu2(OH)2CO3 hnh 2.2
+ Trn ng DTA ch c mt hiu ng thu nhit mnh 309,410C tng ng vi hiu ng ny l
+ Trn ng TG gn 2000C xy ra s phn hy ca sn phm v trn 2000C qu trnh phn h
0C .
Phng trnh phn ng phn hy.
Ag2CO3
2Ag + CO2 + O2
Cu2(OH)2CO3 2CuO + H2O + CO2
Hnh 2.3. Gin
Nhn vo
+ Trn
+ Trn ng TG
0C .
Nh vy,
AgNO3

phn tch nhit ca M 2.3.5


gin phn tch nhit ca mu M 2.3.5 c cha AgNO3 v Cu2(OH)2CO3 hn
ng DTA ch c mt hiu ng thu nhit mnh 203,730C tng ng vi hiu
gn 2000C xy ra s phn hy ca sn phm v trn 2000C qu trnh phn h

qu trnh phn hy nhit ca cc cht.


Cu2(OH)2CO3
2CuO + H2O + CO2
Ag + NO2 + O2
T cc hnh 2.1, 2.2 v 2.3 c th thy d mu c cha bc hay khng, nhit phn h

V vy, kho st nh hng ca nhit nung ti tnh cht ca vt liu chng ti


2.4.2. Tng hp vt liu Ag/CuO t CuSO4 v AgNO3 [13]
T cc nguyn liu ban u l mui ng sunfat v mui bc nitrat chng ti tng hp x
php khc nhau:
Quy trnh 1: Phng php ng kt ta
tng hp Ag/CuO theo phng php ng kt ta chng ti thc hin nh sau:
Cn AgNO3 vi khi lng ln lt l: 0,05 gam; 0,057 gam v 0,098 gam trn cn ph
trong 10 ml nc ct (dung dch A).
Cn 1,76 gam CuSO4.5H2O, ho tan trong 10 ml nc ct (dung dch B).
Cn 1,12 gam Na2CO3 , ho tan trong 10 ml nc ct (dung dch C).
dung dch B vo dung dch A khuy u ri t t dung dch C vo ta thu c k
dung dch NaNO3, Na2SO4. Khuy dung dch hn hp thu c trong 1 gi bng my khuy t. Sau
nhiu ln bng nc ct m loi ht ion Na+. Ri tch pha rn ra khi pha lng. Phn kt t
i trong t sy chn khng. Sn phm sau khi sy c ly mt phn em i chp XRD, phn t
, 500oC v 600oC trong 2 gi.
Sn phm sau khi nung chp XRD, chp ph tn x nng lng EDS, chp nh SEM, TEM. th hot t
H2O2.
Bng 2.2. K hiu cc mu tng hp theo qui trnh 1
Hm lng
AgNO3
Nhit
0,05 gam
0,056 gam
0,099 gam
400OC M 1.1.4 M 1.2.4 M 1.3.4
500OC M 1.1.5 M 1.2.5 M 1.3.5
600OC M 1.1.6 M 1.2.6 M 1.3.6
C th tm tt qu trnh tng hp Ag/CuO theo phng php ng kt ta theo s hnh 2.4

Hnh 2.4. S qui trnh 1 tng hp v nghin cu xc tc Ag/CuO.


Quy trnh 2: Phng php tm
tng hp vt liu theo phng php tm chng ti thc hin nh sau:
Cn 1,76 gam CuSO4.5H2O ho tan trong 15ml nc ct (dung dch A).
Cn 1,12 gam Na2CO3 ha tan trong 15ml nc ct (dung dch B).
hai dung dch A vo dung dch B ta thy kt ta mu xanh ca Cu-2(OH)2CO3 c h
a thu tinh khuy u sau t ln my khuy t v khuy trong mt gi phn ng xy r
v kt ta ra khi nhau. Ra kt ta bng nc ct loi b ion CO32- d (th bng giy ch
chn nung.
Cn AgNO3 vi cc khi lng ln lt l: 0,05 gam; 0,057 gam v 0,098 gam. Ha tan A
thiu sau trn u vi kt ta Cu2(OH)2CO3 trong chn. Sn phm em sy trong t sy ch
gi sau ly ra nghin bng ci m no. Ly mt t mu em i phn tch nhit; phn cn li
2 gi v na cn li em nung 6000C trong 2 gi.
Sn phm sau khi nung c: chp XRD, chp nh SEM, TEM, th hot tnh xc tc phn
Bng 2.3. K hiu dy mu theo qui trnh 2.
Hm lng
AgNO3
Nhit
0,05 gam
0,056 gam
0,099 gam
500OC M 2.1.5 M 2.2.5 M 2.3.5
600OC M 2.1.6 M 2.2.6 M 2.3.6
C th tm tt qu trnh tng hp Ag/CuO theo phng php tm theo s 2.5 di y:

Hnh 2.5. S qui trnh 2 tng hp v nghin cu xc tc Ag/CuO.


2.4.3. Tng hp vt liu Ag/CuO t Cu v AgNO3 [13]
Trong hai qui trnh (1) v (2) trn ngun cung cp ion Cu2+ l mui CuSO4. Do v
phi qua giai on ra ht ion sunfat bm dnh vo cc kt ta Cu2(OH)2CO3 , Ag2CO3. Giai o

iu khi gy kt t cc ht Ag2CO3 thnh cc ht c kch thc ln. V vy, chng ti tin hn


an u cung cp ion Cu2+ l ng kim loi. C s ca phng php ny nh sau:
Th in cc chun ca ng: 0(Cu2+/Cu) = 0,337V, nn ng khng  tan trong cc axit v c
khi c mt ca cht oxi ha mnh. Nhng khi c mt ca tc nhn phi tr, ng c th  ha
hi , c th to thnh cc phc cht n ca Cu2+ vi cc phi t lm gim th kh ca cp C
cch tnh th chun ca [Cu(NH3)4]2+/ Cu nh sau:
0(Cu(NH3)42+/ Cu) = 0(Cu2+/Cu) + ( 0,0591/ 2)lgKkhng n
= 0,337 + ( 0,0591/ 2)lg ( 9,33. 10-18)
= - 0,166V
Nh c tnh trn, Cu c th tan trong dung dch NH3 khi c mt khng kh.
Chng ti chn cc nguyn liu u l: NH3 nh mt tc nhn phi tr, cht oxi h
l ngun cung cp ion Cu2+, Ag2CO3 v NH4HCO3 cung cp ion Ag+ v OH-. Dung dch phc cht [
3)4]2+ v [Ag(NH3)2]+ c tng hp u tin, sau pha long phc vo nc phc phn ly
lm kt ta Cu2(OH)2CO3 v Ag2CO3 t dung dch. Tch ly hn hp kt ta ng cch li tm, l
Cc phn ng xy ra nh sau:
Cu + 3NH3.H2O + 1/2O2 + NH4HCO3 [Cu(NH3)4]2+ + CO32- + 4H2O.
Ag2CO3 + 4NH3.H2O 2[Ag(NH3)2]+ + CO32- +
4H2O.
[Cu(NH3)4]2+
Cu2+ + 4NH3
[Ag(NH3)2]+
Ag+
+ 2NH3
2Cu2+ + CO32- + 2OH-
Cu2(OH)2CO3
2Ag+
+ CO32- Ag2CO3
Cu2(OH)2CO3
2CuO + CO2 + H2O
2Ag2CO3
4Ag + 2CO2 + O2
y l phng php mi, khng a thm anion vo nn khng cn lm sch sn phm v khng cn
Quy trnh 3: Phng php ng kt ta (I)
Trong qui trnh ny chng ti iu ch kt ta AgCO3 trc, sau  ha tan ng thi
g dch NH4HCO3 bo ha vi s c mt ca dung dch NH3 v oxi khng kh . Qui trnh ny c
Cn 1,5 gam Cu kim loi.
Cn 0,187 gam AgNO3 ha tan trong 5ml H2O (dung dch A).
Cn 0,0528 gam (NH4)2CO3 ha tan trong 5 ml H2O (dung dch B).
Cho dung dch A tc dng vi dung dch B  kt ta Ag2CO3. Lc, ra thu ly kt ta
Sau  cho ng kim loi v kt ta Ag2CO3 vo cc c cha 14 ml dung dch NH4HCO3 b
5 ml dung dch NH3 28%. Khuy trn my khuy t cho n khi Cu v Ag2CO3 tan hon ton to du
h m. Sau  nh t t dung dch mu xanh m ny vo cc ng 100 ml H2O t trn my khuy
yn ph) th dng khuy,  ngui, ly tm ly kt ta, ra kt ta bng nc ct v sy 700
hu c cht rn mu xanh ngc bch gm Cu2(OH)2CO3 v Ag2CO3. Cht rn ny c nung trong l
5000C, 6000C trong 2 gi. Sn phm thu c l bt Ag/CuO c nghin trong ci m no.
Sn phm sau khi nung c: chp XRD, chp nh SEM, TEM, th hot tnh xc tc ph
K hiu mu nung 400OC
M 3.1.4 M 3.2.5 M 3.3.6

Bng 2.4. K hiu dy mu theo qui trnh 3.


K hiu mu nung 500OC
K hiu mu nung 600OC

Qui trnh 3 c th c tm tt theo s  hnh 2.6 di y:

Hnh 2.6. S  qui trnh 3 tng hp v nghin cu xc tc Ag/CuO


Quy trnh 4: Phng php ng kt ta (II)
Khc vi qui trnh 3, trong qui trnh ny chng ti tin hnh ha tan hon ton Cu k
dung dch NH4HCO3 bo ha vi s c mt ca dung dch NH3 v oxi khng kh trc, sau  mi
n.
Qui trnh c thc hin nh sau:
Cn 1,5 gam Cu kim loi.
Cn 0,187 gam AgNO3 ha tan trong 5ml H2O (dung dch A).
Cn 0,0528 gam (NH4)2CO3 ha tan trong 5 ml H2O (dung dch B).
Cho dung dch A tc dng vi dung dch B  ly kt ta Ag2CO3. Ly tm, ra, thu ly k
Cho Cu kim loi vo cc c cha 14 ml dung dch NH4HCO3 bo ha, trong qu trnh ha t
,5 ml dung dch NH3 28%. Khuy trn my khuy t cho n khi Cu tan hon ton to dung dch m
hm kt ta Ag2CO3 trn vo v tip tc khuy cho n khi tan hon ton. Ton b dung dch

t trn my khuy t, un nh cho n khi dung dch tr nn c (dng huyn ph) th dng k
g nc ct v sy 700C trong 10 gi, thu c cht rn mu xanh ngc bch Cu2(OH)2CO3 v Ag
ong l nung cc mc nhit  4000C, 5000C, 6000C trong 2 gi. Sn phm thu c l bt Ag/C
.
Sn phm sau khi nung c: chp XRD, chp nh SEM, TEM, th hot tnh xc tc phn ng phn
Bng 2.5. K hiu dy mu theo qui trnh 4.
K hiu mu nung 400OC
K hiu mu nung 500OC
K hiu mu nung 600OC
M 4.1.4 M 4.2.5 M 4.3.6

Qui trnh 4 c th c tm tt theo s  hnh 2.7 di y:

Hnh 2.7. S  qui trnh 4 tng hp v nghin cu xc tc Ag/CuO.


Quy trnh 5. Phng php tm
Trong qui trnh ny chng ti tin hnh ha tan Cu kim loi trong dung dch NH4HCO3 b
thc hin qu trnh to kt ta Cu2(OH)2CO3. Sau  tm dung dch AgNO3 ln kt ta Cu2(OH)2C
C th qui trnh 5 c thc hin nh sau:
Cn 1,5 gam Cu kim loi.
Cn 0,187 gam AgNO3 ha tan trong 5 ml H2O (dung dch A).
Cho Cu kim loi vo cc c cha 14 ml dung dch NH4HCO3 bo ha ri nh t t vo 
H3 28%. Khuy trn my khuy t cho n khi Cu tan hon ton to dung dch mu xanh m. Sau
nh m ny vo cc ng 100 ml H2O t trn my khuy t, un nh cho n khi dung dch tr n
ly tm, ra bng nc ct thu ly kt ta. Cho kt ta vo chn nung ri trn vi dung dch
hng hn hp 700C trong 10 gi, thu c cht rn mu xanh ngc bch gm Cu2(OH)2CO3 v Ag
ng l nung cc mc nhit  4000C, 5000C, 6000C trong 2 gi. Sn phm thu c l bt Ag/Cu
Sn phm sau khi nung c: chp XRD, chp nh SEM, TEM, th hot tnh xc tc phn
Bng 2.6. Bng k hiu dy mu theo qui trnh 5.
K hiu mu nung 400OC
M 5.1.4 M 5.2.5 M 5.3.6

K hiu mu nung 500OC

K hiu mu nung 600OC

C th tm tt qui trnh 5 theo s  hnh 2.8 di y:

Hnh 2.8. S  qui trnh 5 tng hp v nghin cu xc tc Ag/CuO.


Sau qu trnh thc hin cc qui trnh tng hp, chng ti  tng hp c tt c 8 dy mu
ra  c mu so snh chng ti tng hp 2 mu trng CuO (mt mu tng hp t CuSO4 k hiu l
MT 2). Tng s mu chng ti  tng hp c l 26 mu. Thnh phn, phng php iu ch 
Bng 2.7. Bng tng hp cc mu iu ch c theo cc qui trnh.
STT
K hiu mu
Qui trnh
thc hin
Nhit  nung Khi lng AgNO3 (gam) %Ag trong sn phm Ag/CuO
1
MT 1
T cht u CuSO4
500
0
0 %
2
M 1.1.4 1
400
0,050 5,4%
3
M 1.2.4 1
400
0,056 6,0%
4
M 1.3.4 1
400
0,099 10%
5
M 1.1.5 1
500
0,050 5,4%
6
M 1.2.5 1
500
0,056 6,0%
7
M 1.3.5 1
500
0,099 10%
8
M 1.1.6 1
600
0,050 5,4%
9
M 1.2.6 1
600
0,056 6,0%
10
M 1.3.6 1
600
0,099 10%
11
M 2.1.5 2
500
0,050 5,4%
12
M 2.2.5 2
500
0,056 6,0%
13
M 2.3.5 2
500
0,099 10%
14
M 2.1.6 2
600
0,050 5,4%
15
M 2.2.6 2
600
0,056 6,0%
16
M 2.3.6 2
600
0,099 10%
17
MT 2
T cht u Cu 500
0
0 %
18
M 3.1.4 3
400
0,185 5,9%
19
M 3.2.5 3
500
0,185 5,9%
20
M 3.3.6 3
600
0,185 5,9%
21
M 4.1.4 4
400
0,185 5,9%
22
M 4.2.5 4
500
0,185 5,9%
23
M 4.3.6 4
600
0,185 5,9%
24
M 5.1.4 5
400
0,185 5,9%
25
M 5.2.5 5
500
0,185 5,9%

26
M 5.3.6 5
600
0,185 5,9%
2.5. Th hot tnh xc tc
2.5.1. Th hot tnh xc tc phn ng phn hy H2O2
Sn phm cui cng sau khi nung c em th hot tnh xc tc vi H2O2,[7] tin h
5oC.
Dng pipet ht 2,00 ml H2O2 3% vo mt nhnh ca ng nghim hai nhnh. Cn 0,002 ga
vo nhnh cn li ca ng nghim hai nhnh. Dng c th nghim nh hnh v:

Hnh 2.9. S  thit b th hot tnh xc tc H2O2.


Lp ng nghim vo b sn phm th xc tc, thng bng mc nc hai ng nghim ri cho phn
u  c 30 giy ghi gi tr mt ln ghi n 15 pht th dng, ngm ng nghim trong cc nc
ng ng nghim khng thay i na, b cc nc nng ra  ng nghim ngui v nhit  phng r
T cc kt qu thu c ta v c  th v tnh c hng s vn tc ca phn ng.
Phng trnh phn ng:
H2O2
H2O + O2
Nu gi thit phn ng l bc 1 th hng s tc  ca phn ng c xc nh bng biu thc:
k =
ln =
ln

Trong  : Co: nng  ban u ca H2O2 (mol/l).


x: nng  H2O2  phn hy ti thi im t (mol/l).
V: th tch oxi cc i (ml).
Vt: th tch oxi thi im t (ml).
k: hng s tc  (s-1).
t: thi gian phn ng (s).
2.5.2. Th hot tnh khng khun
Cc mu Ag/CuO v CuO c th hot tnh sinh hc vi chng Escherichia coli ATCC 25922. C
tnh khng khun c thc hin ti phng th nghim b mn Vi sinh v Sinh hc Trng i h
+ Vi khun :
Escherichia coli ATCC 25922
(EC)
+ Mu th: mu trng MT1, mu M 1.3.5, mu M 3.2.5.
+ Dung dch m pht pht: K2HPO4 : 3,6 gam
Na2HPO4 :7,13 gam
Nc ct : 1000 ml
+ Mi trng thch thng: Cao tht : 0,3 gam
Pepton : 0,5 gam
NaCl : 0,5 gam
Nc ct : 100 ml
Cch tin hnh:
Ly 60 ml dung dch m pht pht cho vo bnh nn 500 ml, cho cc bnh vo thanh tr
atm trong 20 pht.
Ly 10 ml nc ct v trng vo ng nghim  nui cy vi khun 24 gi to hn dch
khun cho vo cc bnh dung dch m  dit trng.
* Mu chng: Ly bnh dung dch m  chun b khng cho mu th lm mu chng
* Mu th: Ly 0,1 gam mu th vo bnh dung dch m chun b.
Cho cc bnh ny vo my lc Taitec Bio-Shaker BR 300Lf 3, lc 140 vng/ pht 37oC tr
gi. Sau 24 gi ly cc bnh ra v tin hnh pha long n nng 10-7 .
Mi trng thch thng thanh trng 121oC, 1 atm trong 20 pht c vo cc hp pet
Ly 0,05 ml hn dch pha long cc nng 10-3 ;10-5 ;10-7 cho vo cc hp petri
hp ny vo trong t m 37oC. Sau 24 gi ly ra kim tra s khun lc pht trin trn hp.
* nh gi kt qu da vo s khun lc pht trin trn hp theo cng thc
=
: s khun lc trung bnh
D : s khun lc hp th i.
s : lch thc nghim chun c hiu chnh.
n : s th nghim lm song song.
2.5.3. Th xc tc quang
Trong lun vn ny chng ti tin hnh kho st kh nng xc tc quang ha ca Ag/CuO
ylen. [17]
Cho 0,1 gam mu Ag/CuO vo 250 ml dung dch xanh metylen 2,5.10-3 g/ml.
Khuy trn my khuy t di nh sng ca n si tc 500 W trong 1,5 gi. C 10 pht ly m
ung dch bng my ph quang ti bc sng 594 nm.

chuyn ha ca xanh metylen c xc nh bng cng thc:

Trong : Ao l hp th quang ca dung dch xanh metylen ban u ti bc sng 594


A l hp th quang ca dung dch xanh metylen ti thi im ly mu bc

CHNG 3. KT QU V THO LUN


3.1. kt qu nghin cu vt liu bng phng php nhiu x tia x
Sn phm thu c chng ti tin hnh ghi gin nhiu x tia X (XRD) xc n
thu c trnh by trong cc hnh t 3.1 n hnh 3.27 di y:
Hnh 3.1. Gin nhiu x tia X ca sn phm sau khi sy.
Hnh 3.2. Gin nhiu x tia X ca MT 1.
Hnh 3.3. Gin nhiu x tia X ca M 1.1.4.
Hnh 3.4. Gin nhiu x tia X ca M 1.2.4.
Hnh 3.5. Gin nhiu x tia X ca M 1.3.4.
Hnh 3.6. Gin nhiu x tia X ca mu M 1.1.5.
Hnh 3.7. Gin nhiu x tia X ca mu M 1.2.5.
Hnh 3.8. Gin nhiu x tia X ca mu M 1.3.5.
Hnh 3.9. Gin nhiu x tia X ca mu M 1.1.6.
Hnh 3.10. Gin nhiu x tia X ca mu M
.6.
Hnh 3.11. Gin nhiu x tia X ca mu M 1.3.6.
Hnh 3.12. Gin nhiu x tia X ca mu M 2.1.5.
Hnh 3.13. Gin nhiu x tia X ca mu M 2.2.5.
Hnh 3.14. Gin nhiu x tia X ca mu 2.3.5.
Hnh 3.15. Gin nhiu x tia X ca mu 2.1.6.
Hnh 3.16. Gin nhiu x tia X ca mu M 2.2.6.
Hnh 3.17. Gin nhiu x tia X ca M 2.3.6.
Hnh 3.18. Gin nhiu x tia X ca MT 2.
Hnh 3.19. Gin nhiu x tia X ca M 3.1.4.
Hnh 3.20. Gin nhiu x tia X ca M 3.2.5.
Hnh 3.21. Gin nhiu x tia X ca M 3.3.6.
Hnh 3.22. Gin nhiu x tia X ca M 4.1.4.
Hnh 3.23. Gin nhiu x tia X ca M 4.2.5.
Hnh 3.24. Gin nhiu x tia X ca M 4.3.6.
Hnh 3.25. Gin nhiu x tia X ca M 5.1.4.
Hnh 3.26. Gin nhiu x tia X ca M 5.2.5.

Hnh 3.27. Gin nhiu x tia X ca M 5.3.6.


Trn gin nhiu x tia X ca tt c cc mu u xut hin cc pic c trng c

pic ca cc cht u Cu2(OH)2CO3, Na2SO4, Na2CO3, AgNO3. Nh vy, sn phm thu c l Ag/CuO
tinh th. iu chng t phn ng phn hu nhit cc cht xy ra hon ton.
3.2. Kt qu chp nh SEM
Sau khi ghi gin nhiu x tia X, chng ti tin hnh ghi ph ca mt s mu bng knh hi
g v kch thc tht ca ht. nh chp SEM ca mu MT1, v mt s mu cha bc M 1.3.5, M 1.3
M 3.2.5, M 4.2.5, M 5.2.5, M 5.3.5 c trnh by trn cc hnh t hnh 3.28 n hnh 3.39.

Hnh 3.30. nh SEM mu M 1.3.6

Hnh 3.32. nh SEM mu M 2.3.6


Hnh 3.34. nh SEM mu M 3.2.5
Hnh 3.36. nh SEM mu M 4.2.5

Hnh 3.31. nh SEM mu M 2.3.5

Hnh 3.33. nh SEM mu M 2.3.6


Hnh 3.35. nh SEM mu M 3.2.5
Hnh 3.37. nh SEM mu M 4.2.5

Hnh 3.38. nh SEM mu M 5.2.5


Hnh 3.39. nh SEM mu M 5.3.5
Nhn vo nh SEM ca cc mu c th thy cc ht thu c u dng hnh cu, kch thc t
3.3. Kt qu chp nh TEM
Do nhng iu kin khch quan, chng ti khng th tin hnh chp mu TEM ca tt c cc mu.
O tng hp c chng ti chn mt mu i din chp. Mu i din l mu M 1.3.5, M 2.3.5
Hnh 3.40. nh TEM mu M 1.3.5

Hnh 3.41. nh TEM mu M 2.3.5

Hnh 3.42. nh TEM mu M 3.2.5


Hnh 3.43. nh TEM mu M 3.2.5
Nhn vo nh TEM ta thy cc ht sng ti xen ln nhau, chng t Ag v CuO phn b kh ng
hnh cu, kch thc tng i ng u, kch thc ht trung bnh ca sn phm Ag/CuO trong
3.4. Kt qu chp ph tn x nng lng (EDS)
T gin nhiu x tia X c th bit c sn phm thu c l Ag/CuO tinh khit
u, c dng hnh cu. bit c sn phm thu c c bao nhiu phn trm bc chng ti c
iu bc nht v c nung nhit 500oC. l mu M 1.3.5 v mu M 2.3.5 chp ph EDS.

Hnh 3.44. Ph tn x nng lng EDS ca M 1.3.5


Hnh 3.45. Ph tn x nng lng EDS ca M 2.3.5
Kt qu chp ph tn x nng lng cho thy: trn ph EDS ca mu M 1.3.5 sn p
, O vi phn trm khi lng tng ng l: 6,42%, 68,58%, 25%.
Trn ph EDS ca mu M 2.3.5 ta thy sn phm thu c c cc nguyn t: Ag, Cu,
l: 6,82%; 64,52%; 28,66%. iu ny kh ng nh mt ln na sn phm thu c l Ag/CuO l ti
g mu thu c hi nh hn hm lng bc tnh theo nguyn liu u vo.
3.5. Kho st hot tnh xc tc ca vt liu Ag/CuO
3.5.1. Th hot tnh xc tc phn ng phn hy H2O2
Kt qu th hot tnh xc tc c trnh by c th cc bng s liu phn ph lc. T
nng xc tc phn hy H2O2 ca cc dy mu:

Bng 3.1. Bng tng hp kt qu th phn ng phn hy H2O2.


STT
K hiu mu
Qui trnh
thc hin
Nhit nung %Ag trong sn phm Ag/CuO
Hng s tc phn ng
Ktb
1
MT 1
T cht u CuSO4
500
0 %
1,31.10-4
2
M 1.1.4 1
400
5,4%
1,52.10-3
3
M 1.2.4 1
400
6,0%
1,54.10-3
4
M 1.3.4 1
400
10%
1,62.10-3
5
M 1.1.5 1
500
5,4%
3,95.10-3
6
M 1.2.5 1
500
6,0%
4,12.10-3
7
M 1.3.5 1
500
10%
4,38.10-3
8
M 1.1.6 1
600
5,4%
2,26.10-3
9
M 1.2.6 1
600
6,0%
2,82.10-3
10
M 1.3.6 1
600
10%
2,93.10-3
11
M 2.1.5 2
500
5,4%
1,45.10-3
12
M 2.2.5 2
500
6,0%
2,89.10-3
13
M 2.3.5 2
500
10%
3,36.10-3
14
M 2.1.6 2
600
5,4%
1,28.10-3
15
M 2.2.6 2
600
6,0%
2,45.10-3
16
M 2.3.6 2
600
10%
2,82.10-3
17
MT 2
T cht u Cu 500
0 %
8,21.10-5
18
M 3.1.4 3
400
5,9%
1,30.10-4
19
M 3.2.5 3
500
5,9%
2,60.10-4
20
M 3.3.6 3
600
5,9%
1,76.10-4
21
M 4.1.4 4
400
5,9%
1,57.10-4
22
M 4.2.5 4
500
5,9%
6,25.10-4
23
M 4.3.6 4
600
5,9%
1,24.10-4
24
M 5.1.4 5
400
5,9%
4,77.10-4
25
M 5.2.5 5
500
5,9%
1,67.10-3
26
M 5.3.6 5
600
5,9%
1,54.10-3

H. 3.46. th biu din s ph thuc ca


lnV/(V-Vo) vo thi gian (t) ca mu
MT 1, M 1.1.4, M 1.2.4, M 1.3.4.
H. 3.47. th biu din s ph thuc
Vo) vo thi gian (t) ca
mu MT 1, M 1.1.5, M 1.2.5, M 1.3.5.

H. 3.48. th biu din s ph thuc ca


lnV/(V-Vo) vo thi gian (t) ca mu
MT 1, M 1.1.6, M 1.2.6, M 1.3.6.
H. 3.49. th biu din s ph thuc
ca lnV/(V-Vo) vo thi gian (t) ca
mu MT 1, M 2.1.5, M 2.2.5, M 2.3.5.
H. 3.50. th biu din s ph thuc ca
lnV/(V-Vo) vo thi gian (t) ca mu
MT 1, M 2.1.6, M 2.2.6, M 2.3.6.
ca lnV/(V-Vo)vo thi gian (t) ca
mu MT 2, M 3.1.4, M 3.2.5, M 3.3.6.
H. 3.52. th biu din s ph thuc
ca lnV/(V-Vo) vo thi gian (t) ca
mu MT 2, M 4.1.4, M 4.2.5, M 4.3.6.
lnV/(V-Vo) vo thi gian (t) ca
mu MT 2, M 5.1.4, M 5.2.5, M 5.3.6.

H. 3.51. th biu dins ph thuc

H. 3.53. th s ph thuc ca

ca

.3.6.

Nhn vo cc ng biu din thy rng cc ng biu din u l cc ng tuyn t
T bng 3.1 v cc hnh t 3.46 n 3.53 c th rt ra mt s nhn xt sau:
i vi cc mu xc tc c iu ch t nguyn liu ban u l CuSO4 v AgNO3 (qui t

Tt c cc mu c bc M 1.1.4 M 2.3.6 u c hng s tc  phn ng phn hy H2O2


i c bc kh nng xc tc ca CuO tng ln.
So snh cc dy mu c iu ch theo hai qui trnh (1) v (2) c th thy cc mu
g ln nht. Chng t nhit  500oC l thch hp nht cho qu trnh nung mu.
So snh hng s tc  phn ng ca cc dy mu c iu ch theo qui trnh (1) v
qui trnh (1) c hot tnh tt hn cc mu tng hp theo qui trnh (2).
So snh cc mu trong cng qui trnh, trong cng nhit  nung th cc mu c hm
tc tt nht.
So vi xc tc CuO nguyn cht (MT 1) kh nng xc tc ca mu vt liu c kh nn
ui trnh 1, nung 500oC, 10% Ag)  lm tng hng s tc  phn ng l:
ln.
i vi cc mu xc tc c iu ch t cc nguyn liu u l Cu v AgNO3 (qui t
.
Tt c cc mu c bc M 3.1.4 n M 5.3.6 u c hng s tc  phn ng phn h
khi c thm bc  lm tng kh nng xc tc ca CuO.
Trong s cc mu c bc, cc mu iu ch theo qui trnh 5 c hng s tc  ph
theo qui trnh 5 tt hn qui trnh 3 v qui trnh 4.
Trong qui trnh 5 thy kM 5.1.4 < kM 5..2.5 < kM 5.3.6 chng t khi hm lng b
h nhau th nhit  nung 500oC l tt nht.

Mu M 5.2.5 (qui trnh 5; nung 500oC; 5,9% Ag) c th lm tng tc  phn ng s


2 vi s ln l:
ln.
Tuy s ln tng tc  ca mu ny nh hn so vi mu M 1.3.5 (ca qui trnh 1)
hm lng bc (10%) cao hn hm lng bc c trong M 5.2.5 (5,9%).
* Tm li:
- Xc tc hn hp Ag/CuO c kh nng xc tc cho phn ng phn hy H2O2 tt h
khit.
- Trong khong nng  bc kho st t 5% n 10%, hm lng bc cng ln th
- Nu qui trnh tng hp i t mui CuSO4 v mui AgNO3 th mu iu ch theo
hp ng kt ta) tt hn theo qui trnh 2 (phng php tm). iu ny c th gii thch v b
sn phm. Do vy, c th c kch thc nh hn nn kh nng xc tc tt hn.
- Nu tng hp t Cu kim loi v mui AgNO3 th cc mu iu ch theo qui trn
hn hai phng php ng kt ta (qui trnh 3 v qui trnh 4). iu ny c th gii thch: k
kt ta Cu2(OH)2CO3 v Ag2CO3 l i t cc dung dch phc amoniacat ca hai kim loi. V phc
bc kh bn nn c th mt lng bc cn nm li trong dung dch. iu ny khng xy ra i v
nguyn liu u vo th trong sn phm ca phng php tm c th cha hm lng bc cao hn
3.5.2. Kt qu th hot tnh khng khun
Bng 3.2. Kt qu th tc dng khng khun ca cc mu MT1, M 1.3.5, M 3.2.5
Mu th Kt qu th nghim
10-3
10-5
10-7
s
s
s
M 1.3.5 37,50
M 3.2.5 42,50
MT 1
48,00
Mu chng

9,50
10,50
12,00
Nhiu

25,50
32,00
34,50
_

5,50
6,00
7,50
Nhiu

12,50
12,50
22,00
_

4,50
2,50
6,00
Nhiu

Theo kt qu thu c thy vt liu c kh nng khng khun i vi chng E.coli.


g ngun nc, khng kh v trong c th con ngi. E.coli l tc nhn chnh gy ra cc bnh l
quang, nhim trng mu...

Kt lun:

S lng khun lc trn cc hp c mu th t hn hp mu chng cho thy cc mu th


Mu trng CuO cng c kh nng dit khun, nhng khi c Ag kh nng dit khun tt h
nng dit khun tng.
Mt s hnh nh mu th khng khun:
Hnh 3.54. Mu vi khun
Hnh 3.55. Mu th vi MT1 (10-3)
Hnh 3.57.Mu th vi MT1 (10-5)
Hnh 3.59. Mu th vi MT1(10-7)
Hnh 3.61. Mu th vi M 1.3.5 (10-3)

Hnh 3.56. Mu th vi M 3.2.5 (10-3)


Hnh 3.58. Mu th vi M 3.2.5 (10-5)
Hnh 3.60. Mu th vi M 3.2.5 (10-7)

Hnh 3.62. Mu th vi M 1.3.5 (

Hnh 3.63. Mu th vi M 1.3.5 (10-7)

3.5.3. Kt qu th xc tc quang
Trong phn ny, chng ti ch th hot tnh lm mt mu ca phm nhum xanh metylen
M 3.2.5, M 5.3.6. Kt qu thu c c trnh by bng 3.3 v hnh 3.64.

Bng 3.3. chuyn ha ca xanh metylen khi dng vt liu lm xc tc


Thi gian (pht)
MT 1
M 3.2.5 M 5.3.6
hp th quang
chuyn ho (%)
hp th quang
chuyn ho
chuyn ho (%)
0
0.497
10
0.343 30.99 0.273 49.30 0.265 46.68
20
0.301 39.44 0.246 50.50 0.250 49.70
30
0.300 39.64 0.239 51.91 0.235 52.72
40
0.286 42.45 0.230 53.72 0.232 53.32
50
0.255 48.69 0.219 55.94 0.215 56.74
60
0.231 53.52 0.210 57.75 0.201 59.56
T kt qu kho st xc tc quang, chng ti v th biu din chuyn ha ca xanh met

Hnh 3.64. ng cong biu din s chuyn ha ca dung dch xanh metylen
Nhn vo ng cong biu din s chuyn ha ca dung dch xanh metylen,
ta thy vi mu trng mu xanh metylen c gim nhng tc gim chm.
Vi cc mu c cha Ag, s chuyn ha ca xanh metylen nhiu hn v ti thi im sau t 10
20 pht tc gim mu chm dn.
Nh vy, vt liu Ag/CuO c kh nng lm gim mu ca xanh metylen.
KT LUN
1. tng hp c 26 mu xc tc Ag/CuO c kch thc nano t mui bc
vi ngun cung cp ion ng l CuSO4 v Cu kim loi bng 5 qui trnh khc nhau. Hm lng bc
t 0% 10%.
Tng hp vt liu Ag/CuO t mui CuSO4 v AgNO3 theo cc phng php:
- Phng php ng kt ta (qui trnh1).
- Phng php tm (qui trnh 2).
Tng hp t Cu kim loi v AgNO3 theo 3 phng php:
- Phng php ng kt ta (I) (qui trnh 3).
- Phng php ng kt ta (II) (qui trnh 4).
- Phng php tm (qui trnh 5).
2. kho st nh hng nhit nung n cht lng sn phm v thy rng nhit
h iu ch xc tc Ag/CuO.
3. phn tch cc c trng ca vt liu bng phng php knh hin vi in t
qut (SEM), ph tn x nng lng EDS, nhiu x tia X. Cc kt qu phn tch cho thy ht Ag/

kch thc trung bnh 30 - 60 nm.


4. tin hnh th hot tnh xc tc ca sn phm vi phn ng phn hy H2O2. K
g/CuO c hot tnh xc tc mnh hn vt liu nano CuO. Khi hm lng bc tng kh nng xc t
Nu nguyn liu u l AgNO3 v mui CuSO4 th vt liu c iu ch theo phng ph
h theo phng php tm. Nu nguyn liu u c s dng l ng kim loi v AgNO3 th vt l
2 phng php ng kt ta.
5. th hot tnh khng khun vt liu nano Ag/CuO v thy rng vt liu c tnh
lng Ag trn mu m lng vi khun b dit s khc nhau.
6. th xc tc quang ca vt liu Ag/CuO v kt qu thu c cho thy vt
liu c kh nng lm nht mu xanh metylen, tc nht mu trong khong thi gian 10-20 p
Ti liu tham kho.
Ting Vit
1.
Th Trm Anh (2006), Tng hp v kho st cc hot tnh SERS v khng khun ca b
ica, Lun vn thc s, i hc s phm H ni 2006.
2.
V nh C, Nguyn Xun Chnh (2004), Cng ngh nano iu khin n tng phn t, NXB
3.
V ng (2006), Cc phng php vt l trong ha hc, NXB i hc quc gia H Ni
4.
Nguyn Hong Hi (2007), Ht nano kim loi, http://www.vatlyvietnam.org, tp 1, s 1.
5.
Nguyn c Ngha (2007), Ha hc nano, NXB Khoa hc T nhin v cng ngh, H Ni.
6.
Hong Nhm (2000), Ha hc v v, Tp II, NXB Gio dc H Ni.
7.
Nguyn Vn Ri, T Th Tho (2003), Thc tp ha hc phn tch, NXB i hc quc gia H
8.
Nguyn nh Triu (2000), Cc phng php phn tch vt l v ha l, Tp I, NXB khoa
9.
http:// dantri( suckhoe).
10.
Nguyn c Vn (2006), Ha hc v c, Tp II, Cc kim loi in hnh, NXB khoa hc v
Ting Anh
11.
A. Slisstan Grijalva et al (2005), Assessment of growth of silver nanop
articles synthesized from an ethylene glycolsilvernitrat polivinylpy rrolidone so
lution, Physica E 25, 438-448.
12.
Chan Ho Kwon et al (1999), Temperature dependence and annealing Effecti
n Suface Enhanced Raman Scattering on chemically prepared silver island films, J
. Phys. Chem. B, 103, 9610-9615.
13.
Erol Seker et al (1999), Nitric oxide reduction by propene over silver/a
lumina and silver-gold/alumina catalysts: effect of preparation methods, Applie
d catalysis A: general 183, 121-134.
14.
G.H.Jain, L.A.Patil (2007), CuO- doped BSST thick film resistors for ppb
level H2S gas sensing at room temperature, Sensors and ctuators B 123, 246-253.
15.
Hongxia Zhang, Milin Zhang (2008), Synthesis of CuO nanocrystalline and
their application as electro de materials for capacitors, Material Chemistry and
Physics 108, 184-187.
16.
J.L. Ou, C.P. Chang, Y. Sung, K.L. Ou, C.C. Tseng, H.W.Ling, M.D.Ger (2
007), Uniform polystyrene microspheres decorated with noble Metal nanopartclefor
med without using extra reducing agent, Collioids and surface A: Physicochem. Eng
. Aspects 305, 36-41.
17.
Kaushik Mallik, Mike Witcomb, Mike Scurrell (2006), Silver nanoparticlec
atalysed redox reaction: An electron relay effect,
Meterials Chemistry and
Physics 97, 283-287.
18.
K. Kawahara et al (2000), Antibacterial effect of silver- zeolite onoral
bacterial under anaerobic conditions, Dental Mater. 16, 452- 455.
19.
Kwan Kim et al (2005), Effect of Ag and Au nanoparticle on ther SERS of
4-Aminobenzenthiol assemble on powderer Copper, J. Pyus. Chem. b, 109, 18929 - 1
3934.
20.
Long- Shuo Wang, Jian- cheng Deng, Yang, Ting Chen (2008), Preparation a
nd catalytic properties of Ag/CuO nano composites via a new method, Meterials C
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21.
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22.
Maurizio Muniz-Miranda (2006), The origin of the band at ~ 1025 cm-1 in
the SERS of pyridine adsorbed on silver, Chemical Physics Letters 417, 330-333.
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24.
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25.
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)3+ complex on silver, Electrochimica Acta, Vol. 37, No. 12,
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Ph lc
Cc bng kt qu thc nghim
th phn ng phn hy H2O2

Bng 1. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu MT 1


Thi gian phn ng (s) Mc nc khi thng bng (ml)
Th tch
kh O2 (ml)
ln
Hng s tc (s-1)
0
0.5
600
2.3
1.8
0.076 1,27.10-4
630
2.4
1.9
0.080 1,28.10-4
660
2.5
2.0
0.085 1,29.10-4
690
2.6
2.1
0.093 1,295.10-4
720
2.7
2.2
0.094 1,30.10-4
750
2.8
2.3
0.098 1,31.10-4
780
2.9
2.4
0.103 1,32.10-4
810
3.0
2.5
0.107 1,33.10-4
840
3.1
2.6
0.112 1,34.10-4
870
3.2
2.7
0.116 1,34.10-4
900
3.3
2.8
0.121 1,35.10-4
25.0
V =24.5
Ktb=1.31.10-4
Bng 2. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.1.4
Thi gian phn
kh O2 (ml)
Hng s tc
0
6.10
600
24.95
630
25.00
660
25.05
690
25.10
720
25.15
750
25.20
780
25.25
810
25.30
840
25.35
870
25.40
900
25.40
34.50

ng (s) Mc nc khi thng bng (ml)


ln
(s-1)
18.85 1.090
18.90 1.095
18.95 1.100
19.00 1.106
19.05 1.111
19.10 1.116
19.15 1.121
19.20 1.127
19.25 1.133
19.30 1.138
19.30 1.138
V =28.4

Th tch

1,82.10-3
1,74.10-3
1,67.10-3
1,60.10-3
1,61.10-3
1,49.10-3
1,44.10-3
1,39.10-3
1,35.10-3
1,31.10-3
1,26.10-3
Ktb =1.52.10-3

Bng 3. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.2.4

Thi gian phn


kh O2 (ml)
Hng s tc
0
6.0
600
28.15
630
28.20
660
28.25
690
28.30
720
28.35
750
28.40
780
28.45
810
28.50
840
28.55
870
28.60
900
28.65
39.00

ng (s) Mc nc khi thng bng (ml)


ln
(s-1)
22.15 1.111
22.20 1.116
22.25 1.121
22.30 1.126
22.35 1.132
22.40 1.135
22.45 1.140
22.50 1.145
22.55 1.150
22.60 1.154
22.65 1.159
V =33.00

Th tch

1,85.10-3
1,77.10-3
1,70.10-3
1,63.10-3
1,57.10-3
1,51.10-3
1,46.10-3
1,41.10-3
1,37.10-3
1,33.10-3
1,29.10-3
Ktb=1,54.10-3

Bng 4. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.3.4


Thi gian phn
kh O2 (ml)
Hng s tc
0
3.0
600
26.05
630
26.10
660
26.20
690
26.30
720
26.35
750
26.40
780
26.45
810
26.50
840
26.50
870
26.60
900
26.65
36.50

ng (s) Mc nc khi thng bng (ml)


ln
(s-1)
23.05 1.165
23.10 1.170
23.20 1.179
23.30 1.189
23.35 1.194
23.40 1.199
23.45 1.204
23.50 1.209
23.50 1.209
23.60 1.219
23.65 1.224
V =33.5

Th tch

1,92.10-3
1,86.10-3
1,79.10-3
1,72.10-3
1,66.10-3
1,60.10-3
1,54.10-3
1,49.10-3
1,49.10-3
1,40.10-3
1,36.10-3
Ktb =1,62.10-3

Bng 5. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.1.5


Thi gian phn
kh O2 (ml)
Hng s tc
0
2.1
600
24.8
630
24.9
660
24.95
690
25.0
720
25.05
750
25.1
780
25.15
810
25.2
840
25.25
870
25.3
900
25.35
26.4

ng (s) Mc nc khi thng bng (ml)


ln
(s-1)
22.7
2.7220
22.8
2.785
22.85 2.818
22.9
2.854
22.95 2.890
23.0
2.928
23.05 2.967
23.1
3.008
23.15 3.050
23.2
3.095
23.25 3.141
V =24.3

Th tch

4,53.10-3
4,42.10-3
4,27.10-3
4,13.10-3
4,01.10-3
3,90.10-3
3,80.10-3
3,71.10-3
3,63.10-3
3,55.10-3
3,49.10-3
Ktb =3,95.10-3

Bng 6. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.2.5

Thi gian phn


kh O 2 (ml)
Hng s tc
0
7.7
600
30.6
630
30.65
660
30.7
690
30.75
720
30.8
750
30.85
780
30.9
810
30.95
840
31.0
870
31.05
900
31.1
32

ng (s) Mc nc khi thng bng (ml)


ln
(s-1)
22.9
2.854
22.95 2.890
23
2.928
23.05 2.967
23.1
3.008
23.15 3.050
23.2
3.095
23.25 3.141
23.3
3.190
23.35 3.241
23.4
3.295
V =24.3

Th tch

4,75.10-3
4,58.10-3
4,43.10-3
4,30.10-3
4,17.10-3
4,06.10-3
3,96.10-3
3,87.10-3
3,79.10-3
3,72.10-3
3,66.10-3
Ktb =4,12.10-3

Bng 7. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.3.5


Thi gian phn
kh O2 (ml)
Hng s tc
0
2.0
600
26
630
26.1
660
26.15
690
26.2
720
26.25
750
26.3
780
26.35
810
26.4
840
264.5
870
26.5
900
26.55
27

ng (s) Mc nc khi thng bng (ml)


ln
(s-1)
24
24.1
24.15
24.2
24.25
24.3
24.35
24.4
24.45
24.5
24.55
V = 25

3.218
3.324
3.381
3.342
3.506
3.575
3.649
3.729
3.816
3.912
4.017

Th tch

5,36.10-3
5,27.10-3
5,12.10-3
4,98.10-3
4,87.10-3
4,76.10-3
4,67.10-3
4,6.10-3
4,54.10-3
4,49.10-3
4,46.10-3
Ktb =4,38.10-3

Bng 8. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.1.6


Thi gian phn
kh O 2 (ml)
Hng s tc
0
0.8
600
16.5
630
16.6
660
16.7
690
16.9
720
17.0
750
17.1
780
17.15
810
17.2
840
17.25
870
17.3
900
17.4

ng (s) Mc nc khi thng bng (ml)


ln
(s-1)
15.7
15.8
15.9
16.0
16.2
16.3
16.35
16.4
16.45
16.5
16.6

1.702
1.731
1.760
1.791
1.856
1.890
1.907
1.925
1.943
1.961
1.999

2,83.10-3
2,74.10-3
2,66.10-3
2,59.10-3
2,57.10-3
2,52.10-3
2,44.10-3
2,37.10-3
2,31.10-3
2,25.10-3
2,22.10-3

Th tch

20

V = 19.2

Ktb =2,26.10-3

Bng 9. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.2.6


Thi gian phn
kh O 2 (ml)
Hng s tc
0
2.8
600
20.0
630
20.1
660
20.2
690
20.3
720
20.4
750
20.5
780
20.6
810
20.7
840
20.8
870
20.9
900
21.0
23

ng (s) Mc nc khi thng bng (ml)


ln
(s-1)
17.2
1.907
17.3
1.940
17.4
1.976
17.5
2.012
17.6
2.050
17.7
2.089
17.8
2.130
17.9
2.172
18.0
2.217
18.1
2.263
17.2
2.312
V = 20.2

Th tch

3,17.10-3
3,08.10-3
2,99.10-3
2,91.10-3
2,84.10-3
2,78.10-3
2,73.10-3
2,68.10-3
2,64.10-3
2,60.10-3
2,56.10-3
Ktb =2,82.10-3

Bng 10. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 1.3.6


Thi gian phn
Hng s tc
0
4.8
600
22.0
630
22.1
660
22.2
690
22.3
720
22.4
750
22.5
780
22.6
810
22.7
840
22.8
870
22.9
900
23
24.8

ng (s) Mc nc khi thng bng (ml)


(s-1)
17.2
1.966
17.3
2.002
17.4
2.040
17.5
2.079
17.6
2.120
17.7
2.162
17.8
2.207
17.9
2.253
18.0
2.302
18.1
2.353
18.2
2.407
V = 20.0

Th tch kh O2 (ml)

ln

3,27.10-3
3,17.10-3
3,09.10-3
3,01.10-3
2,94.10-3
2,88.10-3
2,83.10-3
2,78.10-3
2,74.10-3
2,70.10-3
2,67.10-3
Ktb =2,93.10-3

Bng11. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 2.1.5


Thi gian phn
Hng s tc
0
1.0
600
11.6
630
11.8
660
12.0
690
12.2
720
12.4
750
12.6
780
12.8
810
13.0

ng (s) Mc nc khi thng bng (ml)


(s-1)
10.6
10.8
11.0
11.2
11.4
11.6
11.8
12.0

0.092
0.951
0.981
1.012
1.043
1.076
1,110
1,145

1,54.10-3
1,51.10-3
1,49.10-3
1,47.10-3
1,45.10-3
1,44.10-3
1,42.10-3
1,41.10-3

Th tch kh O2 (ml)

ln

840
870
900

13.2
13.4
13.6
18.6

12.2
1.181
12.4
1.219
12.6
1.258
V = 17.6

1,40.10-3
1,39.10-3
1,38.10-3
Ktb =1.45.10-3

Bng 12. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 2.2.5


Thi gian phn
Hng s tc
0
0.6
600
15.2
630
15.4
660
15.6
690
15.8
720
15.9
750
16.0
780
16.1
810
16.2
840
16.3
870
16.4
900
16.5
18.6

ng (s) Mc nc khi thng bng (ml)


(s-1)
14.6
1.827
14.8
1.901
15.0
1.982
15.2
2.068
15.3
2.115
15.4
2.163
15.5
2.215
15.6
2.269
15.7
2.326
15.8
2.386
15.9
2.451
V = 18.0

Th tch kh O2 (ml)

ln

3,05.10-3
3,02.10-3
3,00.10-3
2,99.10-3
2,94.10-3
2,88.10-3
2,83.10-3
2,80.10-3
2,77.10-3
2,74.10-3
2,72.10-3
Ktb =2,89.10-3

Bng 13. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 2.3.5


Thi gian phn
Hng s tc
0
1.0
600
17.0
630
17.1
660
17.2
690
17.3
720
17.4
750
17.5
780
17.6
810
17.7
840
17.8
870
17.9
900
18.0
19.0

ng (s) Mc nc khi thng bng (ml)


(s-1)
16.0
2.197
16.1
2.249
16.2
2.303
16.3
2,359
16.4
2,420
16.5
2.484
16.6
2.554
16.7
2.628
16.8
2.708
16.9
2.795
17.0
2.890
V = 18.0

Th tch kh O2 (ml)

ln

3,66.10-3
3,57.10-3
3,49.10-3
3,42.10-3
3,36.10-3
3,31.10-3
3,27.10-3
3,24.10-3
3,22.10-3
3,21.10-3
3,21.10-3
Ktb =3,36.10-3

Bng 14. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 2.1.6


Thi gian phn
Hng s tc
0
0.5
600
10.4
630
10,6
660
10.8
690
11.0
720
11.2
750
11.4
780
11.6
810
11.8

ng (s) Mc nc khi thng bng (ml)


(s-1)
9.9
10.1
10.3
10.5
10.7
10.9

0.842
0.869
0.896
0.925
0.954
0.985

11.3

1,048

1,04.10-3
1,40.10-3
1,36.10-3
1,34.10-3
1,33.10-3
1,31.10-3
11.1
1,016
1,29.10-3

Th tch kh O2 (ml)

1,30.10-3

ln

840
870
900

11.9
12.0
12.2
17.9

11.4
1.064
11.5
1.082
11.6
1.099
V = 17.4

1,27.10-3
1,24.10-3
1,22.10-3
Ktb =1,28.10-3

Bng 15. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 2.2.6


Thi gian phn
Hng s tc
0
2.2
600
16.2
630
16.4
660
16.6
690
16.8
720
16.9
750
17.0
780
17.1
810
17.2
840
17.3
870
17.4
900
17.5
19.8

ng (s) Mc nc khi thng bng (ml)


(s-1)
14.0
1.587
14.2
1.644
14.4
1.705
14.6
1.769
14.7
1.803
14.8
1.838
14.9
1.875
15.0
1,912
15.1
1.952
15.2
1.992
15.3
2.035
V = 17.6

Th tch kh O2 (ml)

ln

2,65.10-3
2,61.10-3
2,58.10-3
2,56.10-3
2,51.10-3
2,45.10-3
2,40.10-3
2,36.10-3
2,32.10-3
2,29.10-3
2,26.10-3
Ktb =2,45.10-3

Bng 16. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 2.3.6


Thi gian phn
Hng s tc
0
1.6
600
16.60
630
16.65
660
16.70
690
16.75
720
16.80
750
16.85
780
16.90
810
16.95
840
17.00
870
17.05
900
17.10
19.00

ng (s) Mc nc khi thng bng (ml)


(s-1)
15.00 1.98
15.05 2.00
15.10 2.02
15.15 2.05
15.20 2.07
15.25 2.09
15.30 2.11
15.35 2.14
15.40 2.16
15.45 2.19
15.50 2.21
V = 17.4

Th tch kh O2 (ml)

ln

3,30.10-3
3,17.10-3
3,06.10-3
2,97.10-3
2,88.10-3
2,79.10-3
2,71.10-3
2,64.10-3
2,55.10-3
2,52.10-3
2,46.10-3
Ktb =2,82.10-3

Bng 17. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu MT 2


Thi gian phn
Hng s tc
0
12.0
600
12.8
630
12.9
660
13.0
690
13.0
720
13.1
750
13.1
780
13.1

ng (s) Mc nc khi thng bng (ml)


(s-1)
0.8
0.9
1.0
1.0
1.1
1.1
1.1

0.047
0.053
0.059
0.065
0.065
0.065
0.065

7,80.10-5
8,38.10-5
8,91.10-5
8,52.10-5
9,01.10-5
8,65.10-5
8,32.10-5

Th tch kh O2 (ml)

ln

810
840
870
900

13.1
13.1
13.1
13.15
29.5

1.1
0.065
1.1
0.065
1.1
0.065
1.15
0.068
V = 17.5

8,01.10-5
7,73.10-5
7,46.10-5
7,56.10-5
Ktb =8,21.10-5

Bng 18. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 3.1.4


Thi gian phn
Hng s tc
0
12.00
600
13.75
630
13.80
660
13.85
690
13.90
720
13.95
750
14.00
780
14.00
810
14.05
840
14.10
870
14.15
900
14.20
33.50

ng (s) Mc nc khi thng bng (ml)


(s-1)
1.75
0.084
1.80
0.087
1.85
0.089
1.90
0.092
1.95
0.095
2.00
0.097
2.05
0.100
2.10
0.102
2.15
0.105
2.20
0.107
2.25
0.110
V = 21.5

Th tch kh O2 (ml)

ln

1,41.10-4
1,38.10-4
1,35.10-4
1,33.10-4
1,32.10-4
1,29.10-4
1,28.10-4
1,26.10-4
1,25.10-4
1,23.10-4
1,22.10-4
Ktb =1,30.10-4

Bng 19. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 3.2.5


Thi gian phn
Hng s tc
0
15.0
600
19.6
630
17.7
660
19.8
690
19.9
720
20.0
750
20.1
780
20.2
810
20.3
840
20.4
870
20.5
900
20.6
44.0

ng (s) Mc nc khi thng bng (ml)


(s-1)
4.6
0.173
4.7
0.177
4.8
0.181
4.9
0.185
5.0
0.189
5.1
0.193
5.2
0.198
5.3
0.202
5.4
0.206
5.5
0.210
5.6
0.215
V = 29.0

Th tch kh O2 (ml)

ln

2,88.10-4
2,81.10-4
2,74.10-4
2,68.10-4
2,63.10-4
2,58.10-4
2,53.10-4
2,49.10-4
2,45.10-4
2,42.10-4
2,38.10-4
Ktb =2,60.10-4

Bng 20. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 3.3.6


Thi gian phn
Hng s tc
0
12.00
600
14.70
630
14.80
660
14.85
690
14.90
720
14.95
750
15.00

ng (s) Mc nc khi thng bng (ml)


(s-1)
2.70
2.80
2.85
2.90
2.95
3.00

0.117
0.121
0.124
0.126
0.128
0.130

1,95.10-4
1,93.10-4
1,87.10-4
1,83.10-4
1,78.10-4
1,74.10-4

Th tch kh O2 (ml)

ln

780
810
840
870
900

15.10
15.15
15.20
15.25
15.30
29.40

3.10
0.135
3.15
0.138
3.20
0.140
3.25
0.142
3.30
0.145
V = 17.4

1,73.10-4
1,64.10-4
1,67.10-4
1,64.10-4
1,61.10-4
Ktb =1,76.10-4

Bng 21. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 4.1.4


Thi gian phn
Hng s tc
0
12.00
600
13.90
630
14.00
660
14.00
690
14.10
720
14.10
750
14.15
780
14.20
810
14.20
840
14.25
870
14.30
900
14.30
33.00

ng (s) Mc nc khi thng bng (ml)


(s-1)
1.90
2.00
2.00
2.10
2.10
2.15
2.20
2.20
2.25
2.30
2.30
V = 21

0.095
0.100
0.100
0.105
0.105
0.108
0.111
0.111
0.113
0.116
0.116

Th tch kh O2 (ml)

ln

1,58.10-4
1,58.10-4
1,52.10-4
1,53.10-4
1,46.10-4
1,44.10-4
1,42.10-4
1,37.10-4
1,35.10-4
1,33.10-4
1,29.10-4
Ktb =1,57.10-4

Bng 22. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 4.2.5


Thi gian phn
Hng s tc
0
12.00
600
20.65
630
20.90
660
21.10
690
21.35
720
21.60
750
21.70
780
22.00
810
22.20
840
22.45
870
22.45
900
22.80
38.2

ng (s) Mc nc khi thng bng (ml)


Th tch kh O2 (ml)
(s-1)
8.65
8.90
0.401 6,68.10-4
9.10
0.415 6,59.10-4
9.35
0.427 6,46.10-4
9.60
0.441 6,40.10-4
9.70
0.456 6,34.10-4
10.0
0.462 6,17.10-4
10.2
0.481 6,16.10-4
10.45 0.493 6,09.10-4
10.45 0.509 6,06.10-4
10.8
0.509 5,85.10-4
26.2
0.531 5,90.10-4
V = 26.2
Ktb =6.25.10-4

ln

Bng 23. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 4.3.6


Thi gian phn
Hng s tc
0
12.00
600
14.10
630
14.15
660
14.20
690
14.25
720
14.30

ng (s) Mc nc khi thng bng (ml)


(s-1)
2.10
2.15
2.20
2.25
2.30

0.083
0.085
0.087
0.089
0.091

1,38.10-4
1,34.10-4
1,31.10-4
1,29.10-4
1,26.10-4

Th tch kh O2 (ml)

ln

750
780
810
840
870
900

14.35
14.40
14.40
14.45
14.50
14.55
38.50

2.35
0.094
2.40
0.095
2.40
0.095
2.45
0.097
2.50
0.099
2.55
0.101
V = 26.5

1,24.10-4
1,22.10-4
1,17.10-4
1,15.10-4
1,14.10-4
1,12.10-4
Ktb =1,24.10-4

Bng 24. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 5.1.4


Thi gian phn
Hng s tc
0
9.0
600
16.10
630
16.25
660
16.40
690
16.55
720
16.70
750
16.80
780
16,90
810
17.05
840
17.20
870
17.35
900
17.50
35.10

ng (s) Mc nc khi thng bng (ml)


(s-1)
7.10
0.318
7.25
0.325
7.40
0.334
7.55
0.342
7.70
0.350
7.80
0.355
7.90
0.361
8.05
0.369
8.20
0.377
8.35
0.386
8.50
0.394
V = 26.1

Th tch kh O2 (ml)

ln

5,29.10-4
5,17.10-4
5,05.10-4
4,95.10-4
4,86.10-4
4,73.10-4
4,62.10-4
4,55.10-4
4,49.10-4
4,43.10-4
4,38.10-4
Ktb =4,77.10-4

Bng 25. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 5.2.5


Thi gian phn
Hng s tc
0
7.4
600
27.70
630
28.20
660
28.60
690
28.95
720
29.30
750
29.60
780
29.90
810
30.20
840
30.45
870
30.70
900
30.90
38.40

ng (s) Mc nc khi thng bng (ml)


(s-1)
20.30
20.80
21.20
21.55
21,90
22.20
22.50
22.80
23.05
23.30
23.50
V = 31

1.064
1.112
1.152
1.188
1.226
1.259
1.294
1.330
1.361
1.393
1.420

Th tch kh O2 (ml)

ln

1,77.10-3
1,76.10-3
1,74.10-3
1,72.10-3
1,70.10-3
1,68.10-3
1,66.10-3
1,64.10-3
1,56.10-3
1,60.10-3
1,58.10-3
Ktb =1,67.10-3

Bng 26. Kho st hot tnh xc tc phn ng phn hy H2O2 ca mu M 5.3.6


Thi gian phn
Hng s tc
0
6.0
600
27.1
630
27.6

ng (s) Mc nc khi thng bng (ml)


(s-1)
21.10
21.60

0.842
0.869

1,04.10-3
1,40.10-3

Th tch kh O2 (ml)

ln

660
690
720
750
780
810
840
870
900

28.15
28.6
29.1
29.5
29.9
30.3
30.6
31.0
31.3
40.4

22.15 0.896
22.60 0.925
23.10 0.954
23.50 0.985
23.90 1,016
24.30 1,048
24.60 1.064
25.00 1.082
25.30 1.099
V = 34.4

1,36.10-3
1,34.10-3
1,33.10-3
1,31.10-3
1,30.10-3
1,29.10-3
1,27.10-3
1,24.10-3
1,22.10-3
Ktb =1,54.10-3

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