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7/30/2019 TONG HOP BSCF
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TNG HP BSCF-5582 BNG PP SOL-GEL GVHD: L MINH VIN
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I. Tng quan:1. Pin nhin liuFuel cell
Pin nhin liu c bit nh l thit b chuyn ha nng thnh in nng nh
qu trnh oxi ha nhin liu (thng l H2, O2, khng kh).
Khi dng hidrocabon thay cho kh hidro, sn phm to ra ca qu trnh phn
ng l H2O v CO2. Vi nhin liu c cu trc vi Hidro nhiu hn carbon th nc
to ra nhiu hn, kh CO2 gim. Hin cc nghin cu lun hng n 100% hidro
trong tng lai.[1]
Hnh 1.1:Xu hng sdng nhin liu.[1]
a. Phn loi:Hin nay c nhiu loi pin nhin liu khc nhau ang c hon thin thnh
sn phm thng mi. Cn c theo thnh phn cu to ca cc b phn trong pin:electrolyte, in cc, cc cht xc tc m ngi ta phn loi pin nhin liu. Mt s
loi pin nhin liu dng ph bin hin nay l:
Dung dch KOH (Alkaline) Dung dchmui cabonat nng chy: Molten Carbonate Axit Phosphoric H3PO4: Phosphoric axit fuel cell Mng trao i Proton: PEMFC
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Oxide rn: Solid oxide fuel cell (SOFC)Mi pin nhin liu c ch hot ng v nguyn l dn in khc nhau. Hnh
1.2 l s hot ng ca mt s pin nhin liu hin nay. T y ta thy pin nhin
liu oxit rn (SOFCs) nhit hot ng ln 900-1000oC, cao hn hnso vi cc loi
cn li.
Hnh 1.2: C ch hot ng, ch hot ng mt s pin nhin liu.(s liu
c ly t website university of Cambridge)
b. u im, nhc im ca pin nhin liu:i. u im:
Hiu sut cao : nu ch sn xut in th t 40% (bng nhit in), nu
l cm nhit in th c tht ti 90%
Hiu sut ny t thay i theo cng sut pht
Cng sut ca PAC c th t vi kW ti hng MW m khng lm thay
i hiu sut
t gy n (ngoi trmy nn kh v bm)
t phi bo qun v gi thnh bo dng r.
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Gn nh khng gy nhim mi trng : khng chy, khng thi kh
c SOx, cn COx th thp hn 2 ln v NOx th thp hn 50 ln so vi my pht
nhit in
ii. Nhc imD c rt nhiu im mnh song c th cnh tranh thng mi th pin nhin
liu cn t c cc yu cu sau:
tin cy ca h thng: cn t c 40 nghn givn hnh vi cc ng
dng tnh(pht in ln li in).
Gi thnh sn xut gim: phi t c5000F/kW cng sut t. Ring vi
t th gi ny cn gim 10 ln.Gim lng platine cn dng.
Hn th na l phi m bo n nh c ngun nhin liu v ho c
vo li in.
2. Pin nhin liu oxit rn (SOFCs)SOFC c bt u nghin cu t Haber 1905, Schottky 1935, Baur 1937 v
Wagner 1943 [2] trong n s dng mt hp cht oxit kim loi rn (nh calcium
hay ziconium) lm cht in phn.Hnh 1.3l s vn hnh ca mt pin nhin liu
SOFC.
Hiu sut t c khong 60% v vn hnh nhit t 600C n 1000C.
y l dng pin nhin liu vn hnh nhit cao nht hin nay.
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Hnh 1.3: S ca pin nhin liu SOFC
Phn ng xy ra trong pin:
Anode: 2H2 + 2O2 2H2O + 4e-
Cathode: O2 + 4e- 2O2-
Tng qut: 2H2 + O2 2H2O + nng lng in
Loi pin ny vn hnh nhit kh cao, do dng pin nhin liu SOFC
thng ng dng gii hn trong cc h thng tnh kh ln v nhit tha c th ti tn
dng to thm ngun in b sung.
n nm 1962, Weissbart v Ruka [3] pht trin pin nhin liu SOFC hon
thin hn s dng 85% ZrO2 v 15% CaO lm cht in phn . Hnh 1.4 th hin ca
pin nhin liu SOFCs do Weissbart v Ruka ch to vo nhng nm nm 1962.
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Hnh 1.4: Pin nhin liu nm 1962 ( hon thin hn)[3]
Cc pin nhin liu oxit rn (SOFCs) c coi l mt th h cng ngh bi mi
v nhin liu linh hot v hiu sut cao. Tuy nhin, nhng nghin cu c gii thiu
phn trn u thc hin vi dng SOFCs truyn thng. Cc dng truyn thng Dual
Chamber solid oxide fuel cells (DCSOFCs) hin ang c nghin cu v ci tin.
Nhit hot ng p sut cao t ra s thch thc v tin cy v n nh lu di
ca pin nhin liu DC - SOFCs. C th, thoi ha vt liu, khng th gi kn kh v
cc lc c hc do h s gin nnhit khc nhau gia cc thnh phn pin dn n hiu
sut thp v mt n nh. Nhit cao gii hn vic s dng cc SOFCs ng
dng quy m nh. Do , gim nhit vn hnh l mt trong nhng thch thc
chnh trong nghin cu SOFC.
khc phc nhng trngi nh nu trn, pin nhin liu single-chamber
solid oxide fuel cells (SC-SOFCs) c nghin cu v pht trin. Thut ng "single-
chamber" c gii thiu vo nm 1999 bi Hibino v ng nghip [4, 5, 6] mt
trong nhng ngi tin phong ca cng ngh SC-SOFC. SC-SOFCs hot ng trong
cc hn hp nhin liu v cht oxy ha, do hon ton loi b cc yu cu v vic
kn kh.
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Thng thng vi dual-chamber SOFCs, kh c ngn cch bi mt lp
electrolyte c kt khi tt phn tch kh cung cp vo anode v cathode thnh
hai ngn ring bit. Cht Oxy ha c cung cp vo cc m v nhin liu c a
vo cc dng thng qua cc ngun cung cp kh ring bit m khng c bt k strn ln ca hai kh dng kh ny. S khc bit trong p lc oxy gia hai ngn in
cc ring bit dn n vic thnh lp mt in p mch m(OCV).
Trong SC-SOFCs, pin c t trong mt bung kh v hn hp nhin liu v
cht oxy ha tin vo t bo ca pin nhin liu. Nguyn tc lm vic ca SC-SOFCs
da trn cc phn ng phn bit in cc, ngha l, cc dng phi hot ng vi
nhin liu v trvi cht oxy ha, trong khi cc m phi hot ng vi cht oxiha v tr vi nhin liu. Nh vy, c s hot ng ca xc tc in ho v s phn
ng ring bit ca cc in cc dn n s hnh thnh OCV v dng in.
Mt trong nhng thch thc chnh ca SC-SOFC l vic tm kim cc vt liu
c chn lc cao cho cc th h tip theo ca SC-SOFCs vi hiu sut ci tin
vn hnh thc t. Mt nhc im ca SC-SOFCs l nguy cchy n cao do s dng
hn hp nhin liu v khng kh nhit cao.
Tm li, cc u im v nhc im ca SC-SOFC c tm tt nh sau:
u im:
- Khng cn phi lm kn ngn s trn ln ca hai dng kh.
- H thng cung cp kh n gin.
- Tng bn c-nhit
- T bo pin nhin liu rn chc v thit kn gin.
- Kt ni cc t bo pin nhin liu n gin.
- Electrolyte khng cn t kt khi cao.
- Phn ng ta nhit duy tr nhit hot ng ca pin.
- D ch to.
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Nhc im:
- Vt liu xc tc cn phi c chn lc v hot tnh cao.
- Hiu sut thp.
- Hiu sut s dng nhin liu thp hn so vi SOFC truyn thng.
- C th gy chy n hn hp kh nhit cao.
Tuy nhin, bt chp nhng kh khn, SC-SOFCs c nhng u im hn
SOFCs thng thng. Do vic s dng cc hn hp kh t, l mt trong nhng li
th quan trng ca SC-SOFCs bao gm vic khng cn phi kn kh. Cc cu trc pin
SC- SOFCs n gin, nh gn, khng cn kn kh, c d kin s tng cng kh
nng chu nhit v c. Thm vo , lp electrolyte c kt khi thp (hnh thnh
cc l trng nh) vn c chp nhn. V th, SC-SOFC c ch to n gin, v chi
ph ch to gim.
3. BSCF 5582 (Ba0.5Sr0.5Co0.8Fe0.2O3):BSCF -5582 l mt loi Perovskite, c bit c nhiu tim nng trong vic ng
dng lm vt liu cathode trong in cc IT SOFCs. Cu trc BSCF cha ion O2- v
l trng VO2-. T nhng nghin cu u tin c cng b bi Shao v ng nghip
[9, 15, 20], BSCF tr thnh vt liu y tim nng trong vic ng dng mng
ceramic dn ion O2-, bi v khnng dn O2-, cu trc cao, v khnng bn ha hc,
cng vi hot tnh xc tc hp dn cho khnng oxi ha chn lc nhit cao (mt
s nghin cu c cng b: Shao v ng nghip - 2000; Van Veen v ng nghip
- 2003; Liu v Gavalas2005, Chen v ng nghip - 2007; Zeng v ng nghip -2007). Gn y, mt s nghin cu cho thy khnng ng dng ca vt liu ny y
ha hn lm cathode ca pin nhin liu ITSOFCs.
4. Phng php tng hp BSCF:C nhiu phng php c ng dng tng hp BSCF nh: phng php
sol gel, ng kt ta (co-precipitation), phn ng trng thi rn (solid-state
reaction) Trong cc thp k gn y, c nhiu nghin cu v cho thy rng phng
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php tng hp nh hng n kch thc tinh th, cu trc, hnh thi, v cu trc b
mt ca vt liu. Nhng c tnh c thnh hng n tnh dn in ca cathode
SOFCs. Do , nghin cu tng hp BSCF da vo t tnh cathode l ht sc cn
thit.
H. Patra v ng nghip [10] kt hp hai tc cht EDTA citric acid (EC)
trong qu trnh tng hp BSCF. H chng minh c cc yu t tng hp nh: pH,
t l EDTA: acid citric: metal, thi gian nung, nhit nung nh hng rt ln n
qu trnh tng hp nano BSCF. Wei Zhou v ng nghip [9] cng nghin cu nh
hng ca pH ln qu trnh tng hp BSCF bng phng php EC. Trong phn
nghin cu ny hcng ch ra nh hng ca pH ln phc cht ca EDTA v cc ionkim loi: Fe3+, Co2+, Ba2+, Sr2+, c th hin hnh 1.5.
Hnh 1.5:nh hng ca pH i vi cc phc cht EDTA-Ba, EDTA-Sr,
EDTA-Co, v EDTA-Fe
Hnh 1.5 th hin rng pH tt nht cho phc ca EDTAFe3+/Co2+ tn ti l
3-12. Trong khi vi phc ca EDTA- Sr2+/Ba2+, pH tt phn ng l 7-13. y
l c s l thuyt cho tng hp BSCF 5582 bng phng php sol gel, v da vo
y chng ti chn pH cho cc th nghim kho st l: 6, 8, 10, 12.
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Phng php sol- gel c bit n nh l phng php tng hp n gin, thu
c nano BSCF c kch thc t 10-40nm. Rt nhiu nghin cu [7, 13, 17] thc
hin bng phng php sol-gel s dng: ethylene glycol, polyacrylicaced (PAA)
nh l cht phn tn nhm to ra BSCF c cu trc perovskite, dn in cao.
Bn cnh phng php tng hp sol-gel, Zeljkovi v ng nghip [8] c mt
s nghin cu tng hp BSCF c h trvi sng. BSCF -5582 c tng hp t nhng
hn hp mui nitrate, cacbonate, hay oxit ca nhng ion kim loi tng ng, h trvi
sng trn 2.45GHz. y l hng mi chophng php tng hiu qunng lng v
tit kim thi gian cho tng hp BSCFs.
Trong thp k gn y, Muhammet v ng nghip [18, 19] tp trung nghin
cu tng hp BSCF bng phng php ng kt ta. Trong axit oxalate c s
dng nh l tc cht cho phn ng ng kt ta. Kt qu cho thy rng BSCF c
to ra cu trc perovskite c tnh ng nht cao. C chphng php ng kt ta:
Phn ng phn hy oxit trong axit:MOn(s)+ 2n H
+M
2n++ n H2O
Phn ng kt ta vi oxalateM
2n++ n C2O4
2-M(C2O4)n(s)
Phn hy hp cht oxalate to BSCF nhit 950oCM(C2O4)n(s) + 0.5 n O2 (g) MOn(s)+ 2n CO2(g)
II. Mc tiu ti:Mc tiu ca ti l nghin cu tng hp BSCF 5582 c tinh khit cao v
c kch thc nano bng phng php tng hp sol-gel. Cc yu tnh hng nh:
pH, nhit nung, t l tc cht c nghin cu nhm tm hiu iu kin tng hp.
im khc bit ca lun vn ny l nghin cu nh hng ca cht phn tn PEG ln
tinh khit v kch thc ca cc kt qu tng hp.
III. Ni dung v phng php nghin cu:1. iu ch BSCF5582
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a. Ha cht& thit bHa cht dng tng hp BSCF theo phng php Sol Gel:
Ba(NO3)2 Sr(NO3)2 Co(NO3)26H2O Fe(NO3)39H2O Citric Acid Dung dch ammonia Ethylenediaminetetraacetic acid (EDTA) Polyethylene glycol (PEG) Acohol 99%
Cc thit b dng trong qu trnh tng hp BSCF-5582.
Dng c th nghim thng thng My khuy t c gia nhit + c t: 70-80mm. L nung 1000oCchn nung alumina My nghin + bi nghin zirconia kch thc 5mm.
Phng php phn tch kt qu tng hp:
Thit bo SEM XRD TGA/DTA BET
b. Tng hpChun bdung dch
Mui nitrat:
o Ba(NO3)2 : 0.01 molo Sr(NO3)2 : 0.01 mol
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o Co(NO3)26H2O : 0.004 molo Fe(NO3)39H2O : 0.016mol
Qui trnh tng hp:
BSCF 5582 c tng hp theo qui trnh nh c trnh bi s 1.
T l EDTA: NH4OH = 1:1 Nhit phn ng (to solgel): 80oC Cht phn tn PEG c thm vo sau khi hn hp EDTA v
mui nitrate hon ton ng nht.
Nhit lm kh gel: 200
o
C. Thi gian sy kh gel: 5h pH phn ng: 6-12 Thi gian nung: 4h, nhit nung: 55011000C Tc gia nhit: 5oC/ pht. Sau khi nung, mu c nghin mn bng bi zirconia kch thc
5mm trong dung mi C2H5OH, trong 2 h nhm ph vnhng kt t hnh thnh
trong qu trnh sol-gel v nung mu
Mu sau khi nghin c sy kh trong 12h nhit 100oC.
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S 1: Tng hp BSCF5582 bng phng php sol-gel
2. Kho st cc yu tnh hng n kch thc ht v tinh khit ca snphm:
Cc iu kin tng hp lun nh hng ln n qu trnh phn ng, to mm
tinh th hay kt khi. Cc iu kin tng hp sc kho st v ghi nhn li t
cu trc ti u.
iu kin cn kho st:
1. Kho st pH dung dch sol-gel2. T l EDTA : metal3. Nhit nung kt sn phm 550, 800, 950, 1100oC (da theo
TGA tham kho ta c lng, khi tng hp mu o TGA chnh xc => nhit
nung chnh xc)
EDTA NH4OH Ba(NO3)2 Sr(NO3)2 Co(NO3)26H2O
Fe(NO3)39H2O
Dd EDTANH4OH Dd ng nht
Dd ng nht Cht phn tn (PEG)
Hn hp gel
iu chnh pH bngNH4OH
Sy kh 200oC
Bt gel kh en
Khuy t v gia nhit
Nung 550-1100oC
Bt BSCF
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4. nh hng ca cht phn tn: cht phn tn polyethylene glycol(PEG). Kho st t l EDTA: PEG.
3. Cc th nghim dkinCc th nghim d kin thc hin gm 2 phn:
Phn 1: Thc hin phn ng tng hp khng s dng cht phn tn
Kho st cc yu tnh hng ti qu trnh tng hp, tm iu kin ti uthu c BSCF tinh khit, kch thc nano.
Phn tch kt qu BSCF c tng hp.Phn 2: Thc hin tng hp vi s kt hp ca cht phn tn Polyethylene
glycol (PEG)
Da vo cc iu kin ti u trong th nghim phn 1, tm t l cht phntn thch hp thu c BSCF tinh khit v c kch thc nano.
So snh kt qu tng hp vi trng hp tng hp phn 1.Phn 1: Thc hin phnng tng hp khng sdng cht phn tn
Kho st nhit nung:
Mu sol gel sau khi sy nhit 200oC, c phn tch TGA nhm tm hiu s
bin i cu trc vt liu theo nhit . T sa ra cc ch nhit nung v
nhit kt khi ph hp.
iu kin phn tch TGA/DTA:
Mi trng: khng kh, hoc oxi Nhit : t nhit phng n 900oC. Tc gia nhit: 5oC/min.
Kt quphn tch TGA l c s kho st nh hng ca nhit nung n s hnh
thnh cu trc ca BSCF. Nhit nung kho st l: 550, 800, 1000, 1100oC. Bng
3.1 l iu kin kho st ch nung.
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Bng 3.1:iu kin kho stnh hng ca nhit nung.
Cht to gel T l EDTA :
nM+
pH Nhit nung ToC Thi gian
nung, h
EDTA 1:1 8
550
800
1000
1100
4
Phn tch cu trc BSCF ti nhng ch phn hy khc nhau, tm hiu cutrc Perovskite BSCF.
Chn nhit nung thch hp T
*o
CKho st pH:
Hnh 1.5 th hin nh hng ca pH i vi cc phc cht kim loi trong qu trnh to
solgel. y cng l cn c thc hin cc th nghim kho st nh hng ca pH
n qu trnh tng hp BSCF. Bng 3.2 l iu kin kho st trong trng hp ny.
Bng 3.2:iu kin kho st ch pH
Cht to gel T l EDTA :
nM+
pH Nhit nung ToC Thi gian
nung, h
EDTA 1:1
6
8
10
12
T* 4
pH dung dch c iu chnh bi dung dch ammoniac. Chn pH ph hp c BSCF tinh kit c kch thc nano=> pH*
Kho st cu trc BSCF, kch thc ht nhng ch pH khc nhau.Kho st t l EDTA : metal
Bng 3.3 l iu kin kho st t lEDTA: nM+.
Bng 3.3:iu kin kho st tl EDTA : metal
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Cht to gel T l EDTA :
nM+
pH Nhit nung ToC Thi gian
nung, h
EDTA
0.5 : 1
1 : 11.5 : 1
2 : 1
pH* T* 4
Chn t l EDTA: M+ ph hp: R* Kho st cu trc nano BSCF c tng hp theo t l tc cht khc nhau.
Kt lun s b phn 1:
T nhng kt quc kho st trong cc iu kin trn, cc thng s ti u c lachn nhm tng hp BSCF tinh khit, c kch thc nano:
Nhit nung: T* pH dung dch: pH* T lEDTA : nM+: R*
Vi mu BSCF thu c tiu kin ti u ny, chng ti kho st cc tnh cht vt
liu nh:
Kch thc nano BSCF phn bkch thc. Kho st din tch b mt (BET) kt khi.
Phn 2: Kho stnh hng PEG.
iu kin tng hp:
pH dung dch sol-gel: pH* T lEDTA : nM+ = R* Nhit nung: T*oC
Cht phn tn c thm vo trong qu trnh to sol gel nhm thu c BSCF c
kch thc nano, nhhn so vi trng hp khng s dng cht phn tn. Mt s cht
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phn tn c th s dng: ethylene glycol (EG), polyethylene glycol (PEG), propanol
Th nghim ny s nghin cu nh hng ca cht phn tn polyethylene glycol
(PEG) i vi kt qu tng hp BSCF.
Bng 3.4: iu kin kho stnh hng cht phn tn PEG n tng hp BSCF
Cht to gel T l EDTA :
nM+
Cht phn tn,
PEG
T l
EDTA: nM+:PEG
Thi gian
nung, h
EDTA R* PEG
R*:PEG = 1:0.5
R*:PEG = 1:1
R*:PEG = 1:1.5
R*:PEG = 1:2
4
Nghin cu cu trc nano BSCF khi c b sung cht phn tn PEG so vi cctrng hp trn.
Tm t lEDTA: nM+: PEGthu c BSCF tinh khit, kch thc nm.4. Kho st tnh cht ca sn phm c tinh khit cao nht:
Cc mu c tng hp v mu gel c mang i phn tch cc chtiu sau
y:
4.1 Phn tch SEM:
Dng phng php Scanning electron microscopy (SEM):
Kho st cu trc hnh hc v vi cu trc ca vt liu c chto nhng iu kin nghin cu khc nhau.
phn gii khc nhau c th kim tra ng u ca snphm
4.2 Phn tch XRD:
Dng phng php XRD xc nh cu trc ca cht tng hp v kho st
tinh khit ca vt liu tng hp. Nhiu x X- ray dng bc x CuK35kV v 20mA,
phn tch vi gc 2 = 10 80, xc nh kch thc ht t XRD s dng hm Debye
Scherrer Equation:
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T = 0,9 / B cos
Vi: t: kch thc trung bnh, nm
: chiu di bc sng (0.15418nm) K ca Cu.
B: chiu rng trung bnh ca peak.
: gc nhiu x Bragg
Kt hp phn mm Unitcell phn tch cu trc vt liu
nh gi kt qu vt liu tng hp:
Xc nh cu trc tinh th. Tnh ton kch thc tinh th.
4.3 Phn tch TGA:
Kho st s phn hy ca mu BSCF gel, dng 4mg cho vo chn Alumina
(oxit nhm) v phn tch trong my TGA. Kho st s thay i cu trc vt liu t
nhit phng n 900
o
C, tc gia nhit 5
o
C/pht.
IV. K hoch thc hinD tnh thc hin lun vn tng hp BSCF 5582 trong 10 thng, tnh t
10/2012 n 07/2013.
STT NI DUNG THC HIN THI GIAN GHI CH
1 Kho st nh hng ca pH i vi qu
trnh tng hp
27/10/2012 -
08/11/2012
2 Kho st nh hng ca t l EDTA : M+ 09/11/2012
09/01/2013
3 Kho st nh hng ca nhit nung
n cu trc BSCF
10/01/2013
09/02/2013
4 Kho st nh hng ca cht phn tn
PEG n qu trnh solgel v kch thc
10/02/2013
09/03/2013
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ht nano BSCF
5 Tng hp, phn tch s liu th nghim.
Vit lun vn
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06/2013
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TI LIU THAM KHO
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