Professional Documents
Culture Documents
MC LC
Chng I..........................................................................................................................................3
PHNG PHP HP PH A LP BET...................................................................................3
I. Khi nim v hp ph...............................................................................................................3
II. Phng php hp ph a lp BET..........................................................................................3
II.1.C s ca phng php.....................................................................................................3
II.2. Cu to, nguyn tc hot ng, cc c im ca thit b hp ph a lp BET..............6
III. Kt qu o din tch b mt BET ca h xc tc ba cu t Bi-Mo-V...................................9
Chng II ......................................................................................................................................10
PHNG PHP NHIU X TIA X .......................................................................10
I. Nhiu x tia X (XRD):............................................................................................................10
I.1. Gii thiu v tia X...........................................................................................................10
I.2. C s ca phng php nhiu x tia X............................................................................12
II. Cu to, nguyn tc hot ng, thc nghim phn tch v cc phng php tnh ton ca
phng php nhiu x tia X.......................................................................................................13
II.1. Cu to............................................................................................................................13
II.2. Nguyn tc hot ng:....................................................................................................16
II.3. Thc nghim phn tch nhiu x tia X trn my D8 Advance ca Bruker....................17
II.4. Cc phng php tnh ton. ..........................................................................................18
III. ng dng ca phng php XRD ......................................................................................18
IV. u nhc im ca phng php XRD..............................................................................19
V. nh gi kt qu ph XRD vi mu xc tc Bi0,85V0,55Mo0,45O4 theo cc phng php
tng hp khc nhau....................................................................................................................19
TI LIU THAM KHO.............................................................................................................22
LI M U
Mc ch ca mn hc nghin cu cu trc vt liu trong cng ngh ha
hc:
-Nghin cu thnh phn ca vt liu v xc nh cc tnh cht ca vt liu
- Lin h gia thnh phn, tnh cht vt liu vi kh nng ng dng vo xc
tc v hp ph.
- Ch to xc tc v vt liu mi.
xc nh cu trc ca vt liu, ngi ta s dng ch yu l cc phng
php ha l. C nhiu phng php nh ph hng ngoi, X-ray, ph khi, cng
hng t ht nhn, phn tch nhit, Cc phng php ny va mang tnh c
lp, va mang tnh h tr. Vi mt cht phc tp phi s dng nhiu phng php,
da trn nhiu kha cnh nh gi chnh xc v cu trc vt liu.
Trong gii hn bi tiu lun ny, em xin bo co mt phng php phn tch
cu trc thng dng ang c s dng ti phng th nghim Ha du thuc i
hc Bch khoa H Ni l phng php:
-
o
Vm c P o
V ( P P ) Vm c
(m2/g)
Trong :
S : din tch b mt (m2/g).
nm : dung lng hp ph (mol/g).
Am : din tch b chim bi mt phn t (m2/phn t).
N : s Avogadro ( s phn t/mol)[6].
Trng hp hay gp nht l hp ph vt l ca Nit (N 2) 77K c tit din
ngang ca N2 bng 0,162 nm2. Nu Vm c biu din qua n v cm3/g v SBET l
m2/g th ta c biu thc:
SBET = 4,35Vm.
Vic xc nh tit din ngang ca phn t N2 c thc hin vi cc cht
rn khc nhau khng c cu trc mao qun v c ht kh ng u. Bng
phng php knh hin vi in t ngi ta xc nh c din tch b mt, bit Vm
th suy ra tit din ngang. i vi cc cht b hp ph khc, ngi ta xc nh
sn v lp bng.
Cc gi tr tit din ngang khng phi l i lng tuyt i. chng c th
ph thuc vo nhit hp ph v cc tnh cht vt l ca b mt. Chng hn nh,
HV: Trn Th M Thm - Lp: 11BKTHH
BET
II.2.1.Cu to v nguyn tc hot ng
V1
P
ng h o
p sut
V2
adsorbate
N2 (77.3 K) hoc
Ar, He, CH4, CO2, Kr
adsorbent
Halenda) t ng hp ph v nh hp ph.
Bo co dng file pdf rt thun tin khi chuyn sang word hoc ppt.
cp c th t 10-12torr.
Bnh Dewar c dung tch 3 lit cho php thc hin php o lin tc
trong sut 72 h.
bt khng cn p vin.
III. Kt qu o din tch b mt BET ca h xc tc ba cu t Bi-Mo-V
Cc mu xc tc Bitmut-Molypden-Vanadi bng phng php solgel v
ng kt ta c o din tch b mt ring trn h Micromeritics ASAP 2010,
PTN Lc Ho Du, HBK H Ni. Bi v h xc tc Bismuth-Molipden-Vanadi l
h vt liu khng c mao qun nn b mt ring ca cc mu thng rt thp (14m2g-1). Do , khi tin hnh o trnh sai s chng ti a lng mu ln
vo trong cell o (>1g xc tc). Do din tch b mt ca cc mu tng hp c
u rt nh nn chng ti khng quan st thy s ph thuc ca hot tnh xc tc
vo b mt ring. Do chng ti mi ch dng li kho st hot tnh xc tc ca
cc mu theo thnh phn pha. y cng chnh l nhc im ca h xc tc
Bismuth Molipdat cho nn cng c BET cha ng vai tr l cng c mnh trong
nghin cu h xc tc ny.
Mu xc tc Bi0,85V0,55Mo0,45O4 iu ch theo phng php ng kt ta c
din tch b mt SBET = 2,103m2/g, nh hn so vi mu xc tc Bi0,85V0,55Mo0,45O4
iu ch theo phng php solgel c SBET = 2,96m2/g. iu ny c gii thch l
vi mu xc tc iu ch theo phng php solgel, v c Citric nn khi nung, citric
b chy ht, li phn b mt c gii phng ca xc tc. Cng do citric b chy
nh vy, cng lm cho cc ht trn b mt xc tc mt phn b thiu kt.
Chng II
10
11
: bc sng tia X .
d: l khong cc gia 2 mt phng tinh th k tip
trong h cc mt phng tinh th (hkl) (m).
: l gc gia tia ti (hoc tia phn x) v mt phn x ().
n : bc phn x v l s nguyn dng.
12
2
d
d
13
14
C TRNG C
Kim
loi
Em
(k
K
()
Cr
24
2,291
5,9
S nguyn
Fe
26
1,937
7,1
8,9
15
B lc tia t
Anod
K ()
Lc
Cr
2.291
Fe
1.937
Mn
16
17
18
Tn km chi ph.
19
C ng
peak, a.u
320
300
280
260
240
220
200
180
160
140
120
100
80
60
40
20
0
0
,8
5
V 0,55 M
o
0
,4
5
O4
n
gk
tt
a
B
i
0
,8
5
V 0,55 M
o
0
,4
5
O4
S
o
lg
e
l
20
30
40
50
60
2th
e
ta
,
C ng
peak, a.u
20
Bi
0,85
V 0,55 Mo
0,45
O4
Trcph
nng
Bi
0,85
V 0,55 Mo
0,45
O4
S
a
up
h
nng
30
40
50
60
2the
ta
,
20
21
22