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LI CM N
Em xin gi li cm n chn thnh ti cc anh, ch ang lm vic, cng tc ti Trung
tm Vt liu hu c v Ha phm xy dng Vin Vt liu xy dng ht sc to iu
kin trong qu trnh thc hin cng trnh nghin cu ny. c bit, xin gi li cm n ti
Ths. Trnh Minh t ch bo tn tnh trong phng php tip cn, phng php lm
vic mt cch khoa hc.
Xin gi li cm n ti cc thy gio, c gio ang cng tc ti Trung tm Nghin cu
vt liu Polyme & Compozit Trng i hc Bch khoa H ni c nhng li ng
vin, khuyn khch trong qu trnh thc hin n.
Xin cm n thy gio PGS.TS. Bch Trng Phc ch bo, ng gp nhng kin
qu bu em hon thnh c cng trnh tt nghip ny.
Em xin chn thnh cm n
H ni, ngy 02 thng 06 nm 2011
Sinh vin

Lu Vn Khu

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MC LC

M U..................................................................................................................4
PHN 1. TNG QUAN...........................................................................................5
1.1. Vt liu polyme compozit (PC)................................................................................5
1.1.1. Gii thiu.....................................................................................................................................................5
1.1.2. Vt liu polyme nanocompozit (PNC)..........................................................................................................6

1.2. Nha polyeste khng no...........................................................................................7

1.2.1. Gii thiu.....................................................................................................................................................7
1.2.2. Nguyn liu tng hp nha PEKN...............................................................................................................8
1.2.3. Nha polysete khng no dng octo............................................................................................................10
1.2.4. ng rn PEKN khng no.........................................................................................................................12

1.3. Nano silica..............................................................................................................13

1.3.1. Gii thiu nano silica.................................................................................................................................13
1.3.2. Phng php ch to nanosilica................................................................................................................15
1.3.3. Bin tnh silica ..........................................................................................................................................16
1.3.4. Silica AEROSIL A200................................................................................................................................18
1.3.5. Silica R7200...............................................................................................................................................19

1.4. Cc phng php ch to vt liu polyme nanocompozit.......................................20

1.4.1. Phng php trn hp dung dch .............................................................................................................20
1.4.2. Phng php In-situ..................................................................................................................................22
1.4.3. Phng php sol gel...............................................................................................................................22

1.5. Cu trc v tnh cht ca vt liu PEKN-silica nanocompozit...............................23

1.5.1. Cu trc ca vt liu PEKN-silica nanocompozit.....................................................................................23
1.5.2. Tnh cht....................................................................................................................................................24

PHN 2. THC NGHIM....................................................................................27

2.1. Ha cht v nguyn liu.........................................................................................27
2.2. Kho st thnh phn nguyn liu u v ch to NPC............................................27
2.2.1. Kho st thi gian gel ha.........................................................................................................................27
2.2.2. Kho st hm lng phn gel ha.............................................................................................................28
2.2.3. Quy trnh ch to vt liu nanocompozit...................................................................................................28
2.2.4. o nht.................................................................................................................................................29

2.3. Xc nh cc tnh cht c hc.................................................................................29

2.3.1. bn ko t v gin di khi t.......................................................................................................29
2.3.2. bn va p............................................................................................................................................30
2.3.3. bn un.................................................................................................................................................31
2.3.4. bn nn.................................................................................................................................................31
2.3.5. mi mn................................................................................................................................................31

2.4. Cc phng php xc nh cu trc........................................................................32

2.4.1. TGA............................................................................................................................................................32
2.4.2. SEM v FE SEM.....................................................................................................................................32
2.4.3. Ph hng ngoi IR.....................................................................................................................................32
2.4.4. TEM............................................................................................................................................................32

2.5. S thay i khi lng trong cc mi trng ho cht..........................................33

PHN 3. KT QU NGHIN CU....................................................................33

3.1. Kho st thi gian gel ha v hm lng phn gel.................................................33
3.2. Tnh cht c hc ca vt liu PEKN silica nanocompozit...................................34
3.2.1. nh hng ca hm lng silica n cc tnh cht c hc ca vt liu PC. ...........................................34

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3.2.2. Kho st nh hng ca hp cht ghp ni GF4......................................................................................36

3.2.3. Kt qu kho st tnh cht c hc ca vt liu PC vi nano silica cha bin tnh (AEROSIL A200) v
silica bin tnh (AEROSIL R7200)..................................................................................................................38
3.2.4. Tnh cht c hc ca vt liu PC ch to bng phng php dung mi ph............................................39

3.3. Nghin cu s phn b ca nano silica trong vt liu PEKN-silica compozit........41

3.3.1. SEM v Fe-SEM.........................................................................................................................................41
3.3.2. TEM............................................................................................................................................................47

3.4. S thay i khi lng ca vt liu PC trong mi trng ha cht........................47

PHN 4. KT LUN.............................................................................................49
PHN 5. TI LIU THAM KHO.....................................................................50

TM TT NI DUNG
Ngy nay, vt liu polyme compozit (PC) khng nh c vai tr ca mnh trong
vic thay th cc loi vt liu truyn thng nh rt nhiu cc u im ni tri nh: khi
lng ring thp, bn cao, kh nng cch in c rt nhiu ti v vt liu PC
c tin hnh nghin cu m rng hn na cc ng dng ca loi vt liu ny, c
bit l trong lnh vc polyme nanocompozit. ti: Nghin cu ch to vt liu polyme
compozit t nha polyeste khng no (PEKN) gia cng bng ht nano silica s dng
phng php trn hp trong dung dich c tin hnh nghin cu nh hng ca cht
n dng nano ln cc tnh cht ca nha nn PEKN.
Kt qu nghin cu cc tnh cht c hc, quan st nh SEM, Fe-SEM tm ra iu
kin ti u ch to vt liu PC trn c s nha polyeste khng no v nano silica bng
phng php trn hp dung dch vi hm lng nano silica ti u 1,75 % khi lng
PEKN, hm lng hp cht ghp ni GF4 ti u l 4% khi lng nano silica.
Kt qu nghin cu DSC TGA cng ch ra rng vt liu s c mt ca nano silica
lm tng n nh nhit, lm gim s phn hy do nhit cho vt liu PC.
Cc kt qu nghin cu tinh cht ca vt liu sau thi gian t trong cc dung mi,
ha cht khc nhau nh H2SO4 10%, HNO3 10%, NaOH 10%, NH4OH 10%, NaCl 10%,
toluen, nc ct cho thy loi vt liu ny chu c cc mi trng ha cht.
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Cc kt qu t c bc u cho thy nano silica l cht n l tng cho cc loi

vt liu PC. Sn phm vt liu PC t PEKN v nano silica c th c s dng trong lnh
vc xy dng lm cht kt dnh cho xi mng, x l vt nt cho b tng. Hoc c s
dng lm cht n tng cng tnh cht cho vt liu PC vi cc loi cht gia cng dng
si hoc vi.

M U
Trn th gii vt liu polyme nanocompozit (PNC) c nghin cu pht trin t
hn 40 nm v trc, tuy nhin do khng c ch quan tm, n thp k 1990 mi
c cc nh khoa hc quan tm khi pht hin ra cc tnh cht c ci thin ng k khi
cho ph gia nano silica vo trong b tng. n nay, cc loi vt liu da trn nn tng c
cha cht n nano silica ny c bc pht trin v cng mnh m, c bit trong lnh
vc polyme compozit.
Vit Nam PNC vt liu cng c trin khai nghin cu trong cc vin , trung
tm nghin cu ng dng nh Trung tm nghin cu vt liu Polyme & Compozit i
hc bch khoa H Ni, trung tm nghin cu vt liu Polyme & Compozit i hc
Bch khoa TPHCM, Vin vt liu xy dng B xy dng, Vin k thut nhit i
Vin khoa hc cng ngh Vit Nam c nhiu cng trnh nghin cu v ng dng
ca nano silica trong vic ch to vt liu PNC v thu c mt s thnh tu ng k.
Tuy nhin y vn l mt loi vt liu kh mi m i vi ngnh cng ngh vt liu
polyme compozit ca nc ta.
Vt liu polyme compozit s dng nano silica lm cht n c nhiu tnh nng ni tri
nh tnh cht c hc tt, mc thm thu v bin dng nhit thp, bn cao trong cc
mi trng dung mi, ha cht... Vt liu nn trn c s nha polyme c th s dng
nha nhit rn, nha nhit do hoc cc loi cao su.
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Da trn c s ti Nghin cu ch to vt liu polyme compozit trn c s

nha polyeste khng no (PEKN) v ph gia nano silica (cha bin tnh v bin tnh)
xc nh tnh cht ca vt liu trc v sau khi c gia cng bng cht n dng
nano nghin cu nh hng ca cht n silica dng nano ln tnh cht ca polyeste
khng no.

PHN 1. TNG QUAN

1.1. Vt liu polyme compozit (PC)
1.1.1. Gii thiu
Vt liu PC l mt h thng gm hai hay nhiu pha vi cc pha thng khc bit nhau
v bn cht, khng tan ln vo nhau v c phn cch bi b mt phn chia pha. Trong
pha nn l pha lin tc, pha phn b gin on c bao bc bi pha nn gi l pha gia
cng.
Pha nn (hay vt liu nn) ng vai tr lm cht kt dnh, bao bc bo v pha gia
cng, ngoi ra cn c tc dng chuyn ng sut lc tc dng ln pha gia cng. Cc tnh
cht ca pha nn c nh hng ln n v tnh cht ca vt liu PC. Bn cht ca vt liu
nn s quyt nh phng php gia cng, ch to v nh hng n bn ca sn phm.
Pha nn trong vt liu PC c th l polyme nhit do: PE, PP, PS hoc c th l nha
nhit rn: polyeste khng no, epoxy
Pha gia cng (hay vt liu gia cng) c tc dng l tc nhn chu lc chnh, hp th
ng sut sinh ra do lc bn ngoi tc ng tng cng tnh cht cho vt liu PC nh
mm do, un, ko, nn, co xc, mi mn.
Pha gia cng c th dng si thng c s dng cho cc loi vt liu chu un,
nn: Si tng hp (si thy tnh, si polyamit, si cac bon), si thc vt (xenllulo, ay,
tre, da).
Pha gia cng c th dng ht, vy (si ngn) thng c s dng trong cc loi
vt liu chu nn, chng va p, mi mn, bn nhit.

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1.1.2. Vt liu polyme nanocompozit (PNC)

L loi vt liu compozit vi vt liu gia cng c kch thc c nano mt c gi l
cht n. Trong vt liu nano compozit cc loi cht n (hay gia cng) thng dng
dng hnh cu, dng xp lp, dng si hoc dng ng.
Vt liu compozit gia cng bng cc ht hnh cu c kch thc nano lm tng
module n hi v module un ngoi ra cn gip ci thin bn co xc, va p, mi
mn, n nh nhit, tng nhit phn hy, tng bn trong cc mi trng ha cht,
nh sng ng thi cng lm gim gi thnh ca sn phm.
c im v tnh cht
Thng thng nha nn c kch thc cng knh trong qu trnh ng rn thng sinh
ra cc ng sut ni ca cc mch i phn t to ra cc l trng. Cc l trng ny hnh
thnh nn cc vt nt t vi trong lng vt liu khi chu tc ng lc. Bng cch s dng
cht n dng nano phn b vo trong lng nha nn s gip in y cc l trng to
nn hin tng san bng ng sut khi chu tc ng lc bn ngoi.
Tnh cht ca vt liu PNC ph thuc vo rt nhiu yu t: Bn cht ha hc ca cc
thnh phn, cc pha nha nn, gia cng; cht kt dnh, b mt phn chia; iu kin thi
gian, nhit ; nh hng cu trc mng li; hm lng, kch thc ca cht n;
phng php ch to
Bn cht ca vt liu PNC l s kt hp cc tnh cht tt nht ca pha nn polyme v
pha gia cng l cht n dng nano. Chng hn, polyme c cc tnh cht khi lng
ring thp, bn ring cao, tnh cht cch in, cch nhit, khng ha cht tt.... Cht
n dng nano c cng cao, bn nhit, v gi thnh r
Vi cht n dng nano ch cn mt hm lng rt nh c th (<3%) c th ci thin
c cc tnh cht nh bn un, ko, nn tng bn nhit, n nh nhit cho polyme.
Polyme l loi vt liu khng tan trong nc song c kh nng hp th lng ln hi
m, dung mi hay ha cht. Vi s gia tng ca hm lng cht n kh nng ht m ca
vt liu cng tng ln.

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Tuy nhin c th kt hp c cc tnh cht tt nht ca cc thnh phn trong vt

liu th cn phi c mt lin kt tt gia b mt phn chia, s ng nht ca cc pha gia
cng v pha nn.
Hm lng v kch thc cng nh hng ln n tnh cht ca loi vt liu to thnh.
Thng thng, vi hm lng ln v kch thc b ca cht n s lm tng tnh cht c
l ca vt liu. Nhng vi hm lng qu ln s lm gim lin kt gia cc mch ca
nha nn polyme v xut hin s kt t ca cc ht cht n lm gim bn ko, un
Trong cc nghin cu gn y vt liu PNC trn c s nha polyeste gia cng bng
ht Nano rt c quan tm bi PEKN l loi nha tng i r tin, ph bin v c cc
tnh cht c l cao. Ngoi ra, cn c li th v kh nng d dng ng rn, ng rn
nhanh.
Tuy nhin, to ra loi vt liu c th kt hp mt cch tt nht tnh cht ca PEKN
v nano silica th ngoi bn cht ca cc thnh phn th phng php ch to cng l mt
vn ht sc quan trng. Phng php ch to vt liu compozit s quyt nh n b
mt phn chia pha, tnh ng nht, s phn b ca ht nano trong nha nn PEKN.
ng dng
Vt liu polyme nanoompozit trn c s gia cng bng ht nano c tnh ng dng
rng ri trong cng nghip mng mng, vt liu xy dng, cc loi ng dng cao cp nh
my bay, tu v tr..
1.2. Nha polyeste khng no
1.2.1. Gii thiu
L loi nha nhit rn c s dng rng ri trong lnh vc polyme compozit. Sn
phm thng mi ca PEKN bt u t nhng nm 1940. Sau 60 nm s dng pht
trin v cng mnh m, nht l trong lnh vc polyme compozit (chim n 95% lng
nha nhit rn).
PEKN l sn phm ca phn ng trng ngng gia axit dicacboxylic no v khng no
vi mt ru a chc. Do , trong mch i phn t c cha lin kt khng no.
V d:
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Dung dch PEKN c cha trong monome styren t 25 45% phn khi lng, ng
vai tr pha long v ng rn. Lin kt i trong mch i phn t ca PEKN v styren
tham gia phn ng ng trng hp to ra cu ni khu mch to thnh mng li
khng gian vi h thng xc tin ng rn (VD: octoat coban & peroxit) nhit
thng t 10 40oC hoc ng rn vi ch peroxit (VD: MEKPO, BPO) nhit cao,
trn 80oC.
1.2.2. Nguyn liu tng hp nha PEKN
Tnh cht ca PEKN ph thuc vo bn cht v t l ca cc cht tham gia phn ng
cng nh iu kin tng hp
Axit icacboxylic khng no thng dng nht l anhydric maleic v axit fumaric, l
tc nhn cung cp lin kt khng no trong mch i phn t ca PEKN.
Anhydric maleic r tin v c cha t hn mt mol nc so vi Axit Fumaric thch hp
cho phn ng trng ngng, trong qu trnh phn ng Axit Maleic chuyn sang dng ng
phn ca n Axit Fumaric gip tng cng tnh cht cho sn phm. S sp xp li ny c
th c iu chnh bi xc tc.
Axit fumaric ch c s dng khi s ng phn ha axit maleic (dng Cis) chuyn
sang axit fumaric (dng Trans) l khng p ng cc yu cu v tnh cht c l cho
nha PEKN. Axit fumaric lm tng n nh nhit, v tng c tnh cho sn phm.
Nhc im so vi anhydric maleic l c chi ph cao v hm lng nc cao hn.

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Axit dicacboxylic no.

Axit phtalic (AP) c s dng ph bin di dng anhydic phtalic vi u im: r
tin, s dng cho nhiu mc ch khc nhau, tng thch vi styren AP c s dng
ph bin nht cho cc loi PEKN thng thng.
Axit isophtalic cho PEKN c n nh nhit, tnh cht c hc v bn ha hc cao
hn so vi AP
Axit terephtalic c s dng cho cc loi nha i hi bn va p cao, n nh
nhit v bn thi tit cao.
Axit adipic cho nha c bn, do cao.

Axit hexametylen terephtalic c bn ha hc rt cao, chng chy

Axit tetrabrom phtalic c kh nng chng chy cao hn song d b phn hy di n
sng mt tri gii phng Brom
Diol
Etylen glicol (EG) r tin, song lm gim kh nng tng thch ca PEKN vi Styren.
Thng c dng vi s c mt ca cc iol khc nh dietylen glicol, dipropylen glicol
hoc butylen glicol

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1,2-Propandiol (propylen glicol) c s dng rng ri vi PEKN thng thng. C

kh nng tng thch rt tt vi styren, gy dnh nh sau khi ng rn v c tnh cht c
hc rt tt.
ietylen glicol v ipropylen glicol c tc dng lm mm do nha v tng s hp th
nc, c s dng ch yu vi propylen glicol iu chnh c tnh hoc ch s khc x
ca nha ng rn.
Butandiol (butylen glicol) tng kh nng chu thi tit, nhng t c s dng do gi
thnh cao v him.
Bis phenol A c s dng nhiu cho nha c d n nh nhit cao, v bn ha
cht cc tt. Vi nha PEKN hnh thnh t Bis phenol A
Neopentyl glicol (2,2-dimetyl-1,3 propandiol) tng kh nng n nh nhit, kh nng
khng ha cht, v tia UV cho PEKN. c bit khi s dng vi axit izophtalic s cho sn
phm c tnh cht c l rt cao.
1.2.3. Nha polysete khng no dng octo.
C rt nhiu cch phn loi PEKN song trong gii hn ca nghin cu ta ch xt
cc loi PEKN thng dng theo tnh cht, mc ch s dng ca sn phm cui cng.
Theo ta c cc loi nha PEKN octo, nha izo, nha DCPD
Nha octo hay cn gi l nha PEKN thng thng, c tng hp t anhydric
phtalic, anhydric maleic v propylen glicol. L loi nha c y cc tnh cht cho hu
ht cc ng dng song c nhc im l ht m cao (d b thy phn bi nc).
Nha Izo c tng hp t izophtalic axit, anhydrit maleic, v propylen glicol. L loi
nha c tnh cht c l cao c s dng cho cc mc ch c bit nh chng n mn,
bn ha hc, chng n mn (lm lp ph cho tu bin), bn nhit
Nha DCPD (dicyclopentadien) c tng hp t icylopentadien v anhdydrit
maleic qua phn ng 2 giai on. Nha DCPD c khi lng phn t rt thp nhng c
th ci thin bng cch to blend vi cc loi nha octo, izo hoc vinyl este tng cng
cc tnh cht c l. Nha DCPD c u im r tin. S cng knh ca phn t DCPD
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ngn nga mch i phn t xp b li vi nhau v lm gim s co ngt khi ng rn. Do

c s dng nhiu trong lnh vc chu nc nh tu thuyn, bn tm
Nha octo hay cn gi l nha PEKN thng thng, c tng hp t anhydric
phtalic, anhydric maleic v propylen glicol. L loi nha c y cc tnh cht cho hu
ht cc ng dng song c nhc im l ht m cao (d b thy phn bi nc).
Tnh cht trng thi bnh thng nha PEKN l cht lng c nht thp, trung
bnh hoc cao, ty thuc vo thnh phn ca dung mi pha long styren. Sau khi ng rn
nha PEKN chuyn sang trng thi rn khng nng chy, khng ha tan.
L nha v nh hnh, trong sut (cho nh sng xuyn qua n 92%). Khi tip xc vi
nh sng c bc sng ngn nha b oxi ha chuyn sang mu vng.
Nha PEKN bn vi cc dung dch axit, mui axit v trung tnh, cc dung mi c cc
nhng khng bn trong mi trng baz, xeton, anilin
PEKN c mch i phn t kh cng knh do khi ng rn c co ngt kh ln,
kh nng chu nhit km, bn va p thp.
Mt s c im ca nha PEKN thng thng c nu ra bng di y:
Bng 1.1: Tnh cht nha PEKN dng octo.
Tnh cht
Khi lng ring 20 oC (g/cm3)
nht 25 oC (Pa.s)
Hm lng styren (%)
Ch s axit (mg KOH/g)
Ch s khc x 25 oC
dn nhit (W/mK)

Phng php o
DIN 51757
DIN 53015
DIN 16945
DIN 53402
DIN 53491
DIN 52612

Gi tr o
1.07 1.30
0.2 4.5
25 45
10 30
1.524 1.559
0.16 0.18

ng dng: Nha PEKN khng c mt cht gia cng ch c s dng trong mt s t

cc lnh vc nh keo dnh, vt trang tr, sn hay vt liu cch in. Cc ng dng ch
yu ca nha PEKN c s dng khi c mt ca cht gia cng dng si nh si thy
tinh, si cacbon, kepla trong cc lnh vc phng tin giao thng ( t, tu thuyn), xy
dng (cc tm panel cho h thng thot nc, cc tm che, lt sn, h thng ng,

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xylanh...), trong ngnh in (cc thit b in, cm cch in). Hoc cc cht n
dng ht nh silica, CaCO3 trong lnh vc cng ngh sn
1.2.4. ng rn PEKN khng no
Qu trnh ng rn c th tin hnh nhit cao (>80 oC) vi cht khi u thng
dng nht l benzyl peoxit (BPO) c trn vi dung mi imetyl phtalat gim kh
nng chy n ng thi tng kh nng trn hp. BPO khi dng km theo vi mt amin
thm bc 3, chng hn nh imetyl amin c th tin hnh nhit thng.
S ng rn ca PEKN vi s c mt ca monome styren c th hin trong hnh v
sau:

Hnh 1.1: Hnh nh th hin cu trc nha PEKN trc khi ng rn.

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Hnh 1.2: Hnh nh th hin cu trc nha PEKN sau khi ng rn.
Vi h cht khi u xc tin, VD: MEKPO (hoc xyclohexano peoxit) kt hp vi
hp cht coban nh naphtenat, octoat c th tin hnh nhit thng 10 40 oC.
Peoxit khi c coi nh l mt cht xc tc, cn hp cht coban c coi nh mt
cht xc tin lm gim nhit ng rn ca PEKN.
Monome styren c s dng ph bin nht lm cht khu mch cho PEKN vi cc
u im: gi thnh r, nht thp, tng hp tt, kh nng trng hp cao, nht
thp. Ngoi ra cn c th dng cc monome dng vinyl nh metymeta acrylat, vinyl
toluent, ivinyl benzen, iallyl phtalat
1.3. Nano silica
1.3.1. Gii thiu nano silica
Nano silica l loi silica v nh hnh, trong cu t din TiO 4 kt b li vi nhau
to thnh cc ht nh c kch thc c nm (1-50nm)
B mt ca silica c cha nhiu cc nhm siloxan (SiOSi) vi nguyn t oxi trn
b mt. Silica l hp cht v c nn c kh nng ht m, nn khi trong khng kh silica
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s ht m mnh hnh thnh nn cc nhm silanol (Si OH) trn b mt vi cc dng:

silinol t do, silanol k tip, silanol cp i c th hin trn cc hnh 1.3 v hnh 1.4.

Hnh 1.3: Cu trc nano silica.

Hnh 1.4: Cu trc cc nhm silanol trn b mt silica.

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Silica tan rt t trong nc(100 150ppm 25 oC v pH t 2 8), khng tan trong

ru, axit v c (tr HF). Silica tan trong cc dung mi hu c nh tetrametylamoni
hidroxit, tan nhanh trong dung dch kim nng.
Nano silica vi kch thc nano l cht n in y gip san bng ng sut khi chu
tc ng lc bn ngoi lm tng cc tnh cht ko, nn un ca vt liu compozit. ng
thi, trong cu trc ca silica cha lin kt SiO vi nng lng lin kt rt ln nn ht
silica c cng rt cao. Do kh nng chng mi mn v co xc ca vt liu
polyme khi gia cng bng silica tt hn rt nhiu. Ngoi ra nh lin kt SiO bn vng
lm cho kh nng chu nhit rt cao do cn lm tng kh nng chu nhit, tnh n nh
nhit cho vt liu polyme compozit.
Silica l hp cht tr v mt ha hc do cn lm tng kh nng khng ha cht rt
tt cho cc ng dng lin quan n cc mi trng ha cht nh axit (tr axit HF) hoc
mi trng baz. c bit silica cn c kh nng dn in nn c s dng trong lnh
vc vt liu dn, bn dn.
Silica c din tch b mt ring ln, ty thuc vo kch thc ht, phng php iu
ch, din tch b mt ring ca silica c gi tr trong khong t 50 600 m 2/g, do kh
nng ht m rt ln. c s dng trong cc lnh vc ht m, lm kh, cht hp ph.
Silica c s dng rng ri lm cht n cho cc ng dng trong cc lnh vc: cng
ngh giy, in, cng ngh sn, cao su mt khc, silica l hp cht khng c hi nn
cn c s dng trong cng nghip bao b, thc phm, y t.
1.3.2. Phng php ch to nanosilica
Silica hay dioxit silic l hp cht cc k phong ph trong t nhin. Tuy nhin, n
khng tn ti dng ring bit (SiO 2) m lun tn ti cu trc t din SiO 4 vi tm l
nguyn t Si cc dng qung (khong) nh ct, si, thch anh hoc cc dng hp
cht nh tetraetyloctosilicat (TEOS), SiCl4... do vy nhn c silica tinh khit ta phi
tin hnh iu ch t cc hp cht c cha silic.
C 2 phng php iu ch ht Silica kch thc nano c s dng kh ph bin l
phng php kh (s dng pha kh) v phng php t.
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Phng php kh c tin hnh bng cch nung cc hp cht cha silic nh TEOS,
CH3SiCl3 v SiCl4 nhit 1000 1200 oC trong mi trng O2 v H2 tinh khit,
bng cch iu chnh nhit , thi gian nung ta c th kim sot c kch thc ca sn
phm theo mun.

Si(OC2H5)4 + 12 O2 SiO2 + 10 H2O + 8 CO2

L phng php n gin c s dng nhiu nht trong cng nghip sn xut
nano silica thng cho sn phm khi (smoke) SiO 2 c kch thc ht trong khong
rng t 10nm 2 m bng cch thay i nng cht phn ng hoc khng ch thi
gian, nhit .
Phng php t c tin hnh bng phng php kt ta khi cho hp cht cha
silic tc dng vi H2SO4
Sau khi lc b kt ta nhiu ln ta thu c SiO2 tinh khit, sy kh ta thu c ht c
kch thc t 10 30nm
1.3.3. Bin tnh silica
B mt silica cha cc nhm silinol c cha nhm OH l cc nhm phn cc c kh
nng to ra cc lin kt hidro gia cc nhm OH. Chng thng kt hp vi nhau to ra
dng kt t thnh cc cm, khi silica c kch thc ln lm gim kh nng phn tn ca
silica trong nha nn. Do , lm gim cc tnh cht ca vt liu compozit to thnh.
Mt khc, silica l hp cht v c c a nc, trong khi nha nn polyme l loi k
nc, do tng kh nng trn hp, tng thch ca PEKN vi silica th phi tin
hnh bin tnh silica.
Bin tnh silica l phng php s dng cc hp cht ha hc c kh nng che chn
cc nhm phn cc (OH) trn b mt ca silica. Ngn nga s kt cm ca cc ht silica.
Ngoi ra, cn lm tng kh nng tng thch ca ht silica vi nha nn bi tnh cht
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lng tnh ca hp cht s dng bin tnh. Hp cht ha hc thng dng bin tnh
l cc hp cht hu c khi lng phn t thp c cha 2 loi nhm chc. Mt nhm c
kh nng to lin kt vi cc nhm chc phn cc ca b mt silica, nhm cn li c kh
nng to lin kt vi cc nhm chc ca nha nn.
C 2 phng php thng c s dng bin tnh silica:
Phng php vt l: silica l hp cht mao qun c din tch b mt ring ln nn c
kh nng hp ph phn t cht bin tnh da vo cc lc vt l yu nh lc van dec van,
lc tng tc tnh in to ra lp che chn b mt silica. Tuy nhin phng php bin
tnh ny thng t c s dng.
Phng php ha hc: l phng php bin tnh Silica da trn phn ng ca nhm
silanol trn b mt silica v nhm chc ca cc hp cht hu c c thch hp (thng
dng nht l cc hp cht Silan), hnh thnh nn nhng lin kt ha hc bn vng nh
lin kt ng ha tr, lin kt ion gia nhm chc ca b mt silica v nhm chc ca cht
dng bin tnh. Qu trnh bin tnh ha hc c miu t nh sau:

Hnh 1.5: Bin tnh b mt silica

Ty thuc vo loi vt liu nn ta chn hp cht hu c bin tnh b mt tng
thch vi nha nn
c rt nhiu nghin cu v phng php bin tnh silica nh phng php kh cc
nhm chc phn cc trn b mt (eliminated) hay phng php ghp (grafting) nhng
trong gii hn nghin cu ta ch tm hiu v c s chung nht ca cc phng php s
dng bin tnh b mt silica nh trn.
y, s dng hp cht silan (GF4) bin tnh b mt silica.

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1.3.4. Silica AEROSIL A200

L nano silica sn xut theo phng php kh, tan hon ton trong nc c cung
cp bi DUGUSSA AG c sn xut t SiCl4 theo cc phn ng:

Phn ng tng:
Qu trnh x l bng phng php ny ta c th iu chnh cc thng s nh nng
cht phn ng, nhit ta c th iu chnh c kch thc, din tch b mt ring ca
ht nano to thnh
S d di y biu din qu trnh iu ch silica AEROSIL A200 ca DUGUSSA
AG theo phng php kh.

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Hnh 1.6. S sn xut nano silica AEROSIL A200

Bng 1.2: Mt s tnh cht ca silica AEROSIL A200.

Tnh cht

n v

Gi tr

B mt ring (BET)

m2/g

20025

Kch thc ht trung bnh

nm

12

% khi lng

1,5

% khi lng

1,0

m (sy 2h 105oC)
Tn tht nhit ( 1000oC trong 2 h trn loi vt
liu sy 105oC trong 2h)
PH (dung dch nng 4%)

3,7 4,7

Hm lng SiO2

% khi lng

99,8

ng dng
AEROSIL A200 c s dng trong cng ngh sn ph, lm cht n gim chi ph v
tng cng tnh cht cho PEKN, Cao su silicon HTV v RTV-2K, lm cht kt dnh, cht
in y, lm mc in Silica A200 khng c nn cn c s dng trong cng ngh
thc phm, y t.
1.3.5. Silica R7200
L sn phm bin tnh nano silica bng hp cht silan: 2-propenoic acid, 2-methyl-, 3(trimethoxysilyl)propyl ester (GF4).

Hnh 1.7: 2-propenoic acid, 2-methyl-, 3-(trimethoxysilyl)propyl ester.

Silica R7200 l cht dng bt, mu trng, khng mi, khng tan trong nc. c s
dng c s dng lm cht n cho sn, cao su, cc loi compozit tng cng cc
tnh cht c l, tnh cht nhit v gim gi thnh cho sn phm.
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Bng 1.3: Tnh cht ca silica AEROSIL R7200.

Tnh cht

n v

Gi tr

B mt ring (BET)

m2/g

150 + 25

Kch thc ht trung bnh

nm

12

Khi lng ring ( 20oC)

g/cm3

m (sy 2h 105oC)

% khi lng

1,5

Tn tht nhit ( 1000oC trong 2 h trn loi vt

% khi lng

1,5

46

% khi lng

99,8

liu sy 105oC trong 2h)

PH (dung dch nng 40g/l 20oC)
Hm lng SiO2

Nhit phn hy

>150

1.4. Cc phng php ch to vt liu polyme nanocompozit

1.4.1. Phng php trn hp dung dch
Phng php trn hp thng thng
L qu trnh gia cng trng thi lng, to c s tip xc mc phn t v c
s dng kh rng ri. L qu trnh xy ra khi c nha nn polyme v cc ht nano silica
tan hoc phn tn u vo dung mi. Trn hp dung dch cn bao hm c latex hoc
huyn ph. c s dng gia cng ch yu vi nha nhit rn

Hnh 1.8: S m t phng php dung dch.

Qu trnh ch to cc ht nano c trn vo dung mi lm trng s b. Dung
dch polyme c trn ln vi hn hp nano ha tan trong dung mi, sau cho thm
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cht ng rn v cc ph gia khc qu trnh tng tc xy ra. Sau tin hnh lm bay
hi dung mi khi hn hp.
u im Trnh c hin tng qu nhit lm ng rn khi nha ngay trong qu
trnh trn.
Nhc im Qu trnh tch dung mi khng hon ton nh hng ln n tnh cht
ca sn phm. Vic la chn dung mi ha tan c polyme v nano gp phi kh khn
v gi thnh cao. Qu trnh bay hi dung mi gy c hi, nhim mi trng.
Yu t nh hng Nng dung dch polyme qu ln s lm cn tr qu trnh khuch
tn gia nano silica v nha nn. Do , lm gim tnh cht ca sn phm nh bn v
kh nng chu ha cht. Ngc li, nu nng qu long th nanocompzit thu c s
khng t c cht lng nh mong mun v hm lng dung mi cn li kh ln
Phng php trn hp dung dch c s dng dung mi ph
Do b mt ca silica cha cc nhm chc silanol phn cc (OH) nn thng xy ra
hin tng kt t do hnh thnh lin kt ha hc gia cc ht silica. Mt khc nha
polyeste c nht cao nn vic phn b silica nhn c trng thi phn b ng
u, cc ht silica khng b kt t trong mi trng nha PEKN l mt vn ht sc kh
khn. gii quyt vn ny ta tin hnh ch to bng phng php dung mi ph vi
quy trnh ch to nh sau:
u tin, ta ha tan silica vo mt dung mi dung mi phn cc ph hp c khi
lng phn t, nht thp nh: etanol, metanol(chim khong 10% th tch hn hp).
Ngoi ra dung mi ny c cha nhm chc phn cc c kh nng tng thch vi nhm
chc trn b mt ht silica to thnh mt lp bo v ngn nga s tip xc ca cc nhm
OH trn b mt silica trnh hin tng kt t ca cc ht silica. nht thp ca loi
dung mi ny cn gp phn lm tng s phn b ca cc ht
silica trong nha nn.
Sau qu trnh phn tn trong dung mi ph ta tin hnh
qu trnh chng tch dung mi n mt lng ph hp
khng nh hng n tnh cht ca vt liu sau ny.
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Cho hn hp dung mi ph silica vo nha ri tin hnh ng rn nha thng thng.

L phng php c s dng trong nghin cu ny. Phng php dung mi ph c
u im: n gin, cc thao tc tin hnh khng phc tp. Tuy nhin li c nhc im:
kh tm dung mi ph ph hp, dung mi c hi v vn tch dung mi ph khng
nh hng n tnh cht ca vt liu l mt vn kh khn cn c nghin cu k.
1.4.2. Phng php In-situ.
L phng php c s dng ln u tin tng hp polyme-naonoclaycompozit trn
nha nn polyamid 6. Ngy nay, phng php ny li c s dng ch yu tng hp
nanocompozit nha nhit rn.
Qu trnh trng hp insitu xy ra nh sau: u tin cc ph gia nano c x l bi
cht bin tnh b mt thch hp. Sau c phn tn vo monome ri tin hnh trng
hp trong dung dch hoc trong khi to thnh nanocompzit.
Qu trnh din ra v thay i cu trc c m t nh sau:

Monome

Tc nhn

P/ polyme ha

Hnh 1.9: S m t phng php insitu

u im: d ch to, nhanh v tnh cht sn phm tt.
Nhc im ca phng php l polyme thu c c KLPT thp nn cht lng sn
phm b hn ch.
1.4.3. Phng php sol gel
u im chnh ca phng php ny l khng cn i hi nhit v p sut tng
i cao, phng php sol gel c th tin hnh nhit v p sut tng i thp.
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c ng dng rng ri ch to vt liu trn c s nha nn hu c v cht n v

c
Qu trnh sol gel l qu trnh hai bc. Bc u tin l qu trnh thy phn alkoxit
kim loi v bc th hai l qu trnh a t. im c bit ca phng php ch mng
li oxit c to thnh t alkoxit c kim ngay trong nn hu c.
Phn ng sol gel ca alkoxit silan c m t theo s sau:
Thy phn:

Ngng t:

Nu phn ng sol gel xy ra hon ton, silica c hnh thnh v c th tm tt theo

phng trnh sau:

Rt nhiu yu t nh hng n ng hc ca qu trnh thy phn v ngng t trong

phn ng sol gel: t l nc/silan, xc tc, nhit v bn cht ca dung mi Phng
php sol gel c nhng u im vt tri so vi cc phng php khc bi c th iu
khin c c tnh b mt v hnh thi hc ca pha v c thng qua iu kin phn ng.
1.5. Cu trc v tnh cht ca vt liu PEKN-silica nanocompozit
1.5.1. Cu trc ca vt liu PEKN-silica nanocompozit
Khi cc ht nano silica phn b trong mi trng polyme ty thuc vo nng , thi
gian khuy, tc khuy, nhit , cht lin kt cc ht silica khi phn b trong nha
nn c th xy ra cc trng hp nh hnh v:

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Hnh 1.10: Cu trc polyme/silica nanocompozit

a: Cc ht nano silica kt t trong nha nn polyme
b: Cc ht nano silica ( bin tnh) phn tn trong nha nn polyme
Cc ht kt hp li to thnh tp hp, kt t to thnh cc ht silica c kch thc ln
lm gim kh nng phn b ca silica, cc ht silica s phn b khng ng u s lm
gim cc tnh cht ca vt liu compozit ch to.
Cc ht phn b ng u trong mi trng nha nn. y l trng thi phn b ti u
l t c cc tnh cht u vit nht ca vt liu compozit. Cng lm mc tiu m
nghin cu ny hng ti.
Do nhn c s phn tn tt ca cc ht nanosilica trong vt liu compozit th
phng php ch to vt liu l vn ct li trong cng trnh nghin cu ny.
1.5.2. Tnh cht
Tnh cht ko, un v va p
Php th ko l php th c s dng rng ri nht nh gi tnh cht c hc ca
nanocompozit to thnh. Cc gi tr bn ko, moun n hi v dn di khi t l
ba thng s chnh. Cc thng s ny thay i theo hm lng silica nhng qui lut thay
i khc nhau. Hn na, php th va p cng c s dng rng ri nh gi tnh
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cht c hc. Silica c x l b mt to ra cc dng tp hp ln hn l cc ht silica

cha x l mc d silica x l b mt c tng tc tt hn vi nn nha. M un n hi
ca compozit n silica cha bin tnh tng khi tng hm lng silica trong khi bn
ko v dn di khi t gim. Vi silica bin tnh compozit c dn di tng, mun
n hi gim khi tng hm lng silica bi axt hp ph ln b mt silica to thnh mng
a lp, c tc dng nh cht ha do.
cng
cng dng ch thuc tnh ca vt liu chng li s thay i hnh dng khi c lc
tc dng. cng l nn tng cho nhiu ng dng v l mt thng s c hc quan trng
ca vt liu. cng ca compozit tng dn khi tng hm lng silica kch thc micro
nhng vi silica nano cng gim khi tng n gi tr ti hn.
dai ph hy
dai ph hy l tnh cht th hin kh nng ca vt liu c vt nt chng li s ph
hy. y cng l mt trong nhng tnh cht quan trng nht ca vt liu. Thng s: h s
cng lc c s dng xc nh dai ph hy ca hu ht cc vt liu. Khi h s
ny tin n gi tr ti hn, qu trnh ph hy khng n nh s xy ra. Gi tr ti hn
c gi l dai ph hy ca vt liu. dai ph hy c th c xc nh bng nhiu
phng php nh un mu c kha v dai ph hy m su. Khi thm nanosilica
lm tng ng k do dai ca vt liu.
Tnh cht ma st v mi mn
Ma st l lc ca hai mt phng tip xc hoc lc ca mi trng tc ng v mi
mn l s mt mt vt liu ca b mt rn di tc ng ca vt rn khc. Cc yu t nh
hng n ma st v mi mn ca nanocompozit l kch thc ht, hnh thi hc v hm
lng n. Nanosilica c th nng cao kh nng lm gim ma st ca compozit, c bit
l di ti trng ln.
Tnh cht nhit
Tnh cht nhit c th c xc nh bng DSC, TGA, DTA, TMAPhn tch nhit
khi lng TGA c th xc nh c nhit bt u phn hy nhit v hm lng
silica trong mu. DSC rt hiu qu xc nh cc nhit chuyn ha. Tnh cht c
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nhit c th c xc nh bng DMA nh: mun n hi v mt mt, nhit ha thy

tinh Tg. Khi c thm nanosilica, n nh tng ln v tng theo hm lng silica. Nhit
phn hy v Tg tng khi hm lng nano silica tng. Mt s nghin cu cho thy Tg
ban u tng nhng sau li gim theo hm lng silica v ht nano khng nh hng
ng k n s thay i nhit ha thy tinh.
Tnh cht chng chy
Tc nhn chng chy c s dng lm cho vt liu kh bt chy hn bng cch
lm gim phn hy v tng nhit bt chy. bt chy ca polyme c xc nh da
trn mt s thng s nh tc chy, tc lan truyn v c tnh bt la. c tnh
chng chy ca nanocompozit thng c nghin cu bng cch xc nh ch s oxy.
Nanocompozit lm gim tc ta nhit v tng lng nhit thot ra. Sc bn ca tng
tc gia silica v polyme l yu t quyt nh n vic lm gim tc ta nhit.
Tnh cht quang hc
Tnh cht quang quan trng nht ca mt vt liu l ch s khc x v mc truyn
qua. Mc truyn qua l tnh cht vt l cho php nh sng truyn xuyn qua vt liu.
y l tnh cht quan trng trong nhiu lnh vc ng dng ca nanocompozit. Khi a
silica vo thng lm cho nanocompozit b m c do nh sng b tn x trn cc ht
silica. duy tr c trong sut silica phi c phn tn n cc mn.
Tnh cht thm thu kh
Tnh cht thm thu kh ph thuc rt nhiu vo th tch t do trong nn nha. Khi
a cc cht n tr vo polyme s lm gim tnh thm kh bi lm gim kh nng ha
tan v thm thu ca kh trong nn polyme.

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PHN 2. THC NGHIM

2.1. Ha cht v nguyn liu
Vt liu nanocompozit c ch to t nha PEKN dng octo c tn thng mi 2508
PT-WV (Hn Quc) v silica AEROSIL A200 AEROSIL R7200 c cung cp bi
DEGUSA (c). MEKP (phn khi lng so vi nha) c s dng lm cht khi mo
(hay xc tc) cho phn ng ng rn. Octoat coban c s dng lm cht xc tin cho
phn ng ng rn. Ngoi ra cn s dng dung dch parafin (10% trong xilen), hp cht
ghp ni silan (GF4), metanol tinh khit.
2.2. Kho st thnh phn nguyn liu u v ch to NPC
2.2.1. Kho st thi gian gel ha
L thi gian tnh t thi im cho h thng xc tin ng rn th nha bt u c hin
tng ng rn (th bng cch dng a thy tinh chm nh vo hn hp khi rt ra nha
khng nh git m b ko theo nh si ch mng).

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2.2.2. Kho st hm lng phn gel ha

Hm lng phn gel hay mt ng rn, c xc nh bng cch nghin nh mu
nanocompozit c ch to ri tin hnh ngm trong dung mi thch hp ha tan phn
nha cha c ng rn, khi lng ca mu s gim dn n mt khi lng khng
i. Ti ta coi nha ng rn hon ton.
Hm lng phn gel c tnh theo cng thc:
X=

x 100

go
vi g: khi lng mu sau khi ngm trong dung mi; go: khi lng ban u ca mu.
Qu trnh c kho st bng cch ln lt thay i hm lng MEKP (t 0,4 1%
khi lng nha) v mui coban (t 0,05 0,3% khi lng nha). Sau tin hnh xc
nh hm lng phn gel ca cc mu ch to tm ra t l thch hp nht ca MEKP v
coban.
2.2.3. Quy trnh ch to vt liu nanocompozit
Qu trnh chung ch to vt liu nanocompozit gm 3 bc
Bc 1: Ly PEKN 100 phn khi lng, coban, parafin v silica vi hm lng silica
thay i ln lt t 1,25 2% (phn khi lng). Hn hp c khuy trn my khuy
tc 500 vng/pht trong 30 pht hn hp c phn tn s b. Hn hp c
qua m ~15 ting silica thm nha.
Bc 2: Tin hnh khuy tc cao 5000 vng/pht trong 8 ting silica phn tn
u silica trong nha nn. Qu trnh khuy tc cao c gi nhit t 20 25 oC
gim ti a hin tng bay hi dung mi. Kt thc khuy tc cao, hn hp tip tc
c qua m.
Bc 3: Hn hp trc khi mu c khuy rung siu m 30 pht cc ht kch
thc nano c th phn tn tt hn ng thi loi b bt kh hnh thnh trong qu trnh
khuy tc cao. Tin hnh khun qu trnh ng rn din ra nhit phng. Sau
24 ting th tho khun.
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Khi tin hnh th nghim vi mu vi s c mt ca hp cht gp ni silan (GF4).

GF4 vi hm lng thay i ln lt t 0 6% (phn khi lng ca silica) c cho vo
trong bc 1. Cc bc sau c tin hnh tng t.
Phng php dung mi ph.
Qu trnh ch to vt liu PEKN silica nanocompozit bng phng php dung mi
ph s dng phng php nghin bi c tin hnh theo 3 bc nh phng php ch to
vt liu polymer nanocompozit bng phng php trn hp thng thng. Tuy nhin,
bc th 1, khi pha hn hp ta tin hnh ln lt nh sau: u tin cn chnh xc khi
lng silica. Sau cn chnh xc khi lng metanol cho vo. Cho ln lt coban,
parafin, GF4 (ln lt t 0 6% khi lng silica). Tin hnh nghin bi phn tn silica
vo metanol (4 6 ting). Hn hp sau khi nghin bi c qua m ri tin hnh
chng tch metanol ra khi hn hp. Cn chnh xc lng nha cho vo ri tin hnh
tng t cc bc 2 v 3 ca qu trnh chung ch to nanocompozit.
2.2.4. o nht
nht l mt thng s quan trng c xc nh theo tiu chun DIN 53018 trn
nht k Brookfield RV vi cnh khuy v tc khuy thch hp.
Tin hnh o nht sau khi mu c khuy tc cao (5000 vng/pht) v c
n nh qua m nhit phng (25 oC).
2.3. Xc nh cc tnh cht c hc
2.3.1. bn ko t v gin di khi t
Phng php c thc hin theo tiu chun ISO 527-1993 trn my o INTRON
3382 ca (M), vi tc ko 2 mm/pht, nhit 25oC, m 65%.
Mu o bn ko t c hnh dng mi cho vi kch thc nh sau:

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Hnh 2.1: Hnh dng kch thc mu vt liu PC o bn ko.

Chiu di x chiu rng x chiu dy = 150 x 20 x 4 mm 3. Vi chiu di khong lm
vic l 50mm. ng knh gc ln t 20 25mm. Chiu rng khong lm vic 10mm..
bn ko c tnh theo cng thc :
k =

F
, MPa
A

Trong , F: lc tc dng, N; A: Tit din ngang ca eo mu, mm 2; k : bn ko,

MPa.
2.3.2. bn va p
L phng php xc nh bn ca vt liu khi chu ti trng t ngt
c xc nh theo tiu chun ISO 179-1993 (E) trn my ...: tc 3,5 m/s ; to=
25oC ; m 65%.
Mu hnh dng hnh ch nht v c kch thc nh sau: di x rng x dy = 100 x 10 x
40 mm3
bn va p c xc nh theo cng thc sau:
vd

a =

W , KJ/m

b.h
Trong , W: nng lng ph hy, KJ; h: dy ca mu, mm; b: chiu rng ca
mu, mm.

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2.3.3. bn un
bn un xc nh theo tiu chun ISO178-1993 (E) trn my o INTRON 3382
ca (M). Vi tc ko 2 mm/pht, nhit 25oC, m 65%.
Mu dng hnh ch nht v c kch thc (chiu di x chiu rng x chiu dy) = (100
x 10 x 4 mm)
bn un c tnh theo cng thc sau
u=

3 F l
2 b h2

, MPa

Trong , F: Lc tc dng ln mu, N; l: khong cch gia 2 gi , mm; b: chiu

rng ca mu, mm; h: chiu dy ca mu, mm; u: bn un, MPa.
2.3.4. bn nn
c xc nh theo tiu chun ISO 604-2002 (E) trn my o INTRON 3382 ca
(M), tc o 2 mm/pht.
Mu o bn ko hnh lp phng c kch thc mi chiu 10mm
bn nn c tnh theo cng thc:
n=

Pn
a b

Trong , n : bn gii hn nn, Mpa; P n: Ti trng ph hu mu, N; b: chiu rng

ca mu, mm; a: chiu dy ca mu, mm.
2.3.5. mi mn
Xc nh bn mi mn theo tiu chun ISO 9352: 1995. S dng bnh mi: CS10;
s chu k: 1000 vng quay. Thit b o bn mi mn Taber model 519-1 ca Anh.
Mu o hnh vung c kch thc 100 x 100 x 4mm.
mi mn c tnh theo cng thc: % m = (mt ms)
Trong , mt: Khi lng mu trc khi mi mn (g); ms: Khi lng mu sau khi
mi mn (g)
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2.4. Cc phng php xc nh cu trc.

2.4.1. TGA
TGA l phng php phn tch cho bit mc tn hao khi lng ca vt liu khi
tng nhit t nghin cu s n nh nhit v bn nhit ca polyme khi c thm
cht n nano silica.
Mu c ct thnh mu nh hnh lp phng c kch thc 3x3x3 (mm). Xc nh
trn my TGA model STA 409 PC/PG ca hng NETZSCH.
Mu c gia nhit vi tc 10 oC/pht t nhit phng ti 800 oC
2.4.2. SEM v FE SEM
Phng php chp nh SEM & FE-SEM nghin cu s phn b ca cc ht silica
trong mi trng nha nn.
c thc hin trn my hin vi in t qut JEOL JMS 6360 LV ca Nht Bn. Qu
trnh chp tin hnh b mt ph hy sau khi o bn ko. B mt ca mu c ph
bng mt lp Pt trc khi tin hnh chp. Hiu in th gia tc 15 20 kV v 10 15kV
vi FE SEM. Vi phng i t 250 n 10.000 ln tng ng vi
2.4.3. Ph hng ngoi IR
Ph hng ngoi (infrared ) nghin cu thnh phn ha hc ca vt liu ch to a
ra cc kt lun d on v cc phn ng ha hc din ra trong qu trnh ch to mu vt
liu. Da vo cc tn hiu ph quan st c (em so snh vi cc tn hiu ph chun)
gip nhn bit cc nhm chc c mt trong vt liu nghin cu.
c tin hnh trn my
2.4.4. TEM
L phng php nghin cu cu trc bn trong ca vt liu, nghin cu s phn b
ca silica trong nha nn.
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c tin hnh trn my vi cc thng s

2.5. S thay i khi lng trong cc mi trng ho cht
Mu c sy kh n khi lng khng i, ngui trong bnh ht m v cn chnh
xc n 0,1 mg. Ngm mu trong mi trng ho cht, sau tng khong thi gian xc
nh ly mu ra, dng giy lc thm kh b mt v cn li.
thay i khi lng ca mu PC c tnh theo cng thc:
m2 m1
T=

x 100 , %
m1

Trong :
T : thay i khi lng, %; m1 : Khi lng mu ban u, g; m2: Khi lng
mu sau mt khong thi gian xc nh, g.
Cc ha cht s dng trong nghin cu ny bao gm

PHN 3. KT QU NGHIN CU
3.1. Kho st thi gian gel ha v hm lng phn gel
Hm lng phn gel l thng s quan trng th hin mt ng rn ca vt liu PC
nh hng trc tip n cc tnh cht ca vt liu PC khi hm lng phn gel cng ln
(cng gn n gi tr 100 %) th mc ng rn xy ra cng hon ton.
ti s dng cht xc tc MEKP loi cht xc tc khi mo phn ng trng hp
gc t do nha polyeste khng no vi cc t l thay i t 0,4 n 0,8 % phn khi
lng so vi nh nn. Qu trnh kho st c thc hin ngay ti nhit phng 25

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C. Kt qu nghin cu nh hng ca hm lng xc tc MEKP n thi gian gel ha v

hm lng phn gel ca nha polyeste c trnh by trn bng 3.1.

Bng 3.1: Kt qu kho st thi gian gel v hm lng phn gel ca nha nn PEKN.
Hm lng MEKP

Thi gian gel

Hm lng phn gel

(% PKL)

(pht)

(%)

0.4

80

91.77

0.5

69

95.09

0.6

56

95.15

0.7

45

96.12

0.8

31

94.67

STT

Da vo kt qu kho st thu c qua s liu bng 3.1 cho thy: Nha PEKN
2508PT WV c hm lng phn gel tng i cao v thi gian gel ha ph hp cho qu
trnh gia cng vt liu PC bng phng php trn hp dung dch.
T , ti la chn ra ch ng rn thch hp nht cho loi nha ny nh sau:
Hm lng cht xc tc MEKPO ti u cn dng cho vic ch to vt liu l 0,7 % ng
vi hm lng phn gel t gi tr cao nht (96,12%) v thi gian gel ha l 45 pht.

3.2. Tnh cht c hc ca vt liu PEKN silica nanocompozit

3.2.1. nh hng ca hm lng silica n cc tnh cht c hc ca vt liu PC.
Cc tnh cht c hc nh bn ko, bn un, bn nn bn va p, mi
mn ca vt liu PEKN-silica compozit ph thuc nhiu yu t trong c hm lng
cht n. Vi hm lng cht n khc nhau t 1,25 2 (% khi lng PEKN) kt qu
nghin cu cho ta kt qu sau:
Bng 3.2: Kt qu kho st nh hng ca hm lng A200 n tnh cht ca vt liu PC.

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Module
ko
(MPa)

bn
un
(MPa)

Module
un
(MPa)

bn
nn
(MPa)

bn
va p
(KJ/m2)

mi mn
(mg/100
0v)

37.88

1237

61.22

2109

82.05

2.53

63.47

1.25

38.47

1464

62.01

2284

84.34

3.55

59.56

1.50

39.91

1517

65.09

2362

86.80

4.59

58.10

1.75

42.10

1730

71.25

2421

91.73

6.34

56.45

2.00

35.97

1649

64.93

2292

91.60

6.06

56.40

40

1.25

1.5

1.75

2.53
3.55
4.59
6.34
6.06

60

37.88
38.47
39.91
42.10
35.97

80

20
0
bn ko

bn un

bn nn

Va p

Mi mn

Hnh 3.1: Biu biu din cc tnh cht c hc vi hm lng silica khc nhau.
T th trn ta thy: Ban u, khi tng hm lng nanosilica th gi tr bn ko,
bn un, v bn va p tng vi s gia tng ca hm lng nano silica v t gi tr
ti u (cao nht) ti gi tr ln lt l 42,10 MPa; 71,25 MPa; 91,60 MPa v 6,34 MPa
ng vi hm lng silica l 1,75 (%khi lng PEKN) sau b suy gim nu ta tip tc
tng hm lng silica.
iu ny c th c gii thch l do c ch gia cng ca cht n dng nano. Nh
ta bit PEKN l loi vt liu polyme c kch thc i phn t cng knh, do , trong
qu trnh ng rn s hnh thnh nn nhng l trng t vi trong lng vt liu. Khi chu
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63.47
59.56
58.10
56.45
56.40

100

82.05
84.34
86.80
91.73
91.60

bn
ko
(MPa)

61.22
62.01
65.09
71.25
64.93

Hm
lng
A200
(% PKL)

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tc ng ca lc bn ngoi ti cc l trng ny s hnh thnh nn cc vt nt t vi lm

suy gim kh nng chu tc ng lc ca vt liu. Khi c mt ca cc cht gia cng kch
thc nano s c tc dng in y cc l trng ny to nn hin tng san bng ng
sut khi tc dng lc do lm tng tnh cht ca vt liu.
Tuy nhin, kh nng phn tn ca nano silica vo trong nha nn cn ph thuc vo
nht ca hn hp khi c mt cht n nano silica. nht ca hn hp ny t l thun
vi hm lng nano silica c mt trong . Kt qu o nht ca hn hp silica v nha
vi hm lng khc nhau c th hin bng di y:
Bng 3.3: nht ca mu vt liu PC vi hm lng nano silica khc nhau.
Hm lng silica (%khi lng)

1,25

1,5

1,75

nht 20 oC

780

1729

1920

2050

2417

Khi hm lng nano silica qu cao, kh nng phn tn ca cht n silica s b suy
gim, ng thi lm xy ra hin tng kt t ca cc ht nano silica trong nha nn lm
gim tnh cht ca vt liu.
3.2.2. Kho st nh hng ca hp cht ghp ni GF4.
GF4 l hp cht dng bin tnh silica. c cho vo hn hp nha, silica trong qu
trnh khuy tc cao (5000 vng/pht). C tc dng lm gim kh nng kt t ca cc
ht silica v lm tng kh nng tng hp vi nha PEKN. Kt qu kho st tnh cht c
hc ca cc mu vt liu c cha 1,75% khi lng silica A200 (so vi nha PEKN) v
hm lng khc nhau ca GF4 t 0 6 % khi lng (so vi silica A200) c a ra
trong bng 1.3 di y.
Bng 3.4: Kt qu kho st nh hng ca hp cht ghp ni n cc tnh cht c hc
GF4

bn

Module

bn

Module

bn

bn va

mi mn

(% PKL)

ko

ko

un

un

nn

(mg/1000v)

(MPa)

(MPa)

(MPa)

(MPa)

(MPa)

(KJ/m2)

42.10

1730

71.25

2421

87.68

6.34

56.45

43.67

1781

72.77

2531

91.32

7.54

53.25

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44.11

1816

75.12

2559

95.41

9.65

50.56

42.82

1648

73.13

2343

90.89

7.32

51.38

6.34
7.54
8.65
7.32

56.45
53.25
50.56
51.38

87.68
91.32
95.41
90.89

71.25
72.77
75.12
73.13

120
100
80
60
40
20
0

42.10
43.67
44.11
42.82

Kt qu c biu din qua biu

bn ko

bn un
0

bn nn

2% GF4

4% GF4

bn va p

mi mn

6% GF4

Hnh 3.2: Biu biu din cc tnh cht c hc ca vt liu PC vi cc hm lng khc
nhau ca nano silica.
Ta kt qu thu c ta thy, khi c mt hp cht ghp ni GF4 tnh cht c hc ca
vt liu c ci thin. Cc tnh cht bn ko, bn un, bn va p ca mu vt
liu tng khi tng hm lng GF4 v c kt qu ti u hm lng GF4 l 4% (khi
lng A200) vi gi tr module ko v un ti u ln lt l 1816 MPa v 2559 MPa. Sau
nu tip tc tng hm lng GF4 cc tnh cht c hc ca vt liu c xu hng gim
xung. S tng ln cc tnh cht c hc ca vt liu PC khi c mt hp cht ghp ni
c gii thch l do s c mt ca hp cht ghp ni GF4. Hp cht ny c kh nng
phn ng vi silica trong qu trnh khuy trn gip bin tnh silica ngay trong qu trnh
ch to mu vt liu PC, phn ng bin tnh ca hp cht GF4 vi b mt silica gip kh
cc nhm chc phn cc (-OH) trn b mt cc ht silica do ngn ngha s kt t ca
cc ht vi nhau (s kt t xy ra do cc ht lin kt vi nhau qua cc lin kt yu nh
lin kt hidro gia cc nhm chc phn cc hay lc mao qun trn b mt silica...) lm
cho s phn b ca cc ht nano silica trong nha nn tr nn ng u v hiu qu hn.
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3.2.3. Kt qu kho st tnh cht c hc ca vt liu PC vi nano silica cha bin

tnh (AEROSIL A200) v silica bin tnh (AEROSIL R7200)
Silica AEROSIL A200, AEROSIL R7200 u l sn phm thng mi ca hng
DEGUSSA (c) trong R7200 l sn phm bin tnh ca silica (cha bin tnh) vi
hp cht ghp ni GF4 (3-methacryloxypropyltrimethoxysilanes).
Kt qu nghin cu cc mu vt liu PC vi hm lng nano silica mi loi A200,
R7200 l 1,75% khi lng so vi nha PEKN c trnh by bng di y.
Bng 3.5: Kt qu o cc tnh cht c hc v so snh.
bn

Module

bn

Module

bn

bn

ko

ko

un

un

nn

va p

mi mn

(MPa)

(MPa)

(MPa)

(MPa)

(MPa)

(KJ/m2)

(mg/1000v)

1,75%A200

42.10

1730

72.28

2421

87.68

8.83

56.45

1,75%R7200

47.61

1711

79.13

2410

94.21

12.43

67.30

Loi silica

Kt qu thu c cho ta thy mu vt liu PC t nano silica bin tnh (R7200) c

bn ko v bn un tng mnh so vi vt liu PC t nano silica cha bin tnh
(A200). Song gi tr module ko v module un ca mu vt liu cha nano silica R700
li gim so vi vt liu PC cha nano silica A200. S gim gi tr ca module ko v
module un l do s c mt ca nano silica bin tnh lm tng do ca vt liu PC,
do , ng sut sinh ra khi tc ng lc b gim. mi mn ca vt liu PC cha nano
silica bin tnh cng c gii thch bi s bin tnh ca silica R7200 bao ph b
mt ca cc ht nano silica mt lp hp cht thp phn t do lm mi mn ca vt
liu tng ln.

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67.30

50.56

12.43

20

9.65

8.83

40

56.45

95.21

90.41

87.68

79.13

75.12

47.61

60

44.11

80

42.10

100

Lu Vn Khu

72.28

n tt nghip

0
bn ko

bn un
A200

bn nn
A200+4% GF4

bn va p

mi mn

R7200

Hnh 3.3: Biu biu din cc tnh cht c hc ca vt liu PC vi cht n nano silica
bin tnh v cha bin tnh.
Biu so snh cc tnh cht ca vt liu PC (hnh 3.3) cn th hin c s so snh
gia qu trnh bin tnh nano silica trong khi qu trnh trn hp (c mt hp cht ghp ni
GF4 vi nano silica) v silica bin tnh R7200 cng cho thy tuy tnh cht ca vt
liu PC t A200 vi s c mt ca GF4 lm tng ng k tnh cht ca vt liu song so
vi vt liu PC i t R7200 th cc tnh cht ca n vn cn tng i thp. iu ny
c gii thch bi hm lng ca nano silica A200 l rt thp so vi nha PEKN do
xc sut GF4 tip xc c vi nano silica qu trnh bin tnh nano silica xy ra l
rt b do tnh cht ca vt liu PC t silica A200 v GF4 ch to bng phng php
trn hp thng thng tng ln khng ng k.
3.2.4. Tnh cht c hc ca vt liu PC ch to bng phng php dung mi ph
Tnh cht c hc ca vt liu PC ch to bng phng php dung mi ph c
nghin cu vi hm lng nano silica A200 l 1,75 (% khi lng PEKN) v GF4 vi
hm lng thay i t 0 6 (% khi lng nano silica A200) c phn tn vo metanol
bng phng php nghin bi trc khi cho vo nha PEKN kt qu nghin cu tnh cht
c hc trn my INSTRON 3382 cho kt qu c th hin bng 1.5.
Bng 3.6: Tnh cht c hc ca mu cc vt liu ch to bng phng php dung mi ph.

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Thnh
phn

Hm
lng
(%)

A200
GF4
A200
GF4
A200
GF4
A200
GF4

1,75
0
1,75
2
1,75
4
1,75
6

bn
ko
(MPa)

Module
ko
(MPa)

bn
un
(MPa)

Module
un
(MPa)

bn
nn
(MPa)

bn va
p
(MPa)

41.89

1819

71.88

2530

90.68

4.32

42.12

1834

72.12

2610

92.70

4.80

46.30

1951

75.60

2689

95.09

6.75

41.61

1720

77.70

2406

101.9

5.43

Kt qu cho ta thy c hai phng php trn hp dung dch thng thng v phng
php trn hp s dng dung mi ph vi hm lng silica l 1,75 (% khi lng PEKN)

97.49

95.41

90.68

91.73

77.70

75.12

71.88

46.30

44.11

41.89

42.10

105.00
95.00
85.00
75.00
65.00
55.00
45.00
35.00

71.25

u cho ta kt qu ti u ca hm lng cht ghp ni GF4 l 4% (so vi silica A200).

bn ko

bn un

bn nn

Trn hp thng thng (khng c mt GF4)

Dung mi ph (khng c mt GF4)

Trn hp thng thng (4% GF4)

Dung mi ph (4% GF4)

Hnh 3.4: Biu so snh cc tnh cht c hc ca 2 phng php trn hp thng thng v
trn hp c s dng dung mi ph.
Kt qu so snh gia cc mu vt liu PC ch to bng phng php trn hp thng
thng gm cc mu vt liu PC ca PEKN v: nano silica A200 hm lng 1,75 (%khi
lng PEKN); nano silica A200 1,75 (%khi lng PEKN) v phng php dung mi
ph c th hin biu hnh 3.4 ta thy tnh cht ca vt liu PC ch to bng
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phng php trn hp s dng dung mi ph khi khng c mt GF4 tnh cht vt liu
tng khng ng k so vi vt liu PC ch to bng phng php trn hp thng thng
(khng c mt GF4). iu ny c gii thch mc d metanol lm tng kh nng phn
b ca silica vo mi trng nha nn PEKN. Tuy nhin khi tch metanol ra khi hn
hp th c th cc ht silica li kt t li vi nhau do lm suy gim tnh cht ca vt
liu.
S c mt ca hp cht ghp ni GF4 trong qu trnh phn tn silica trong metanol s
dng phng php nghin bi gii quyt tng i tt vn bin tnh nano silica
A200. Do , cc tnh cht c hc ca vt liu PC ch to bng phng php trn hp s
dng dung mi ph vi s c mt ca GF4 (4%) lm tng mnh cc tnh cht bn
ko, bn nn. Tuy nhin, s c mt ca metanol (do khng tch c trit ) nn
khng t c do cao nh vi vt liu PC i t nano silica R7200.
3.3. Nghin cu s phn b ca nano silica trong vt liu PEKN-silica compozit
3.3.1. SEM v Fe-SEM

Hnh 3.5: nh SEM mu trng.

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Hnh 3.6: nh SEM mu vt liu PC co cha 1,75 % khi lng silica A200.

Hnh 3.7: nh SEM v Fe-SEM ca mu vt liu PC c cha 1,75 % silica A200.

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Hnh 3.8: nh SEM v Fe-SEM ca mu vt liu PC c cha 1,75 % silica A200.

Cc nh t hnh 3.6 n hnh 3.8 cho thy cc ht silica A200 c khuynh hng kt t
li vi nhau v rt kh nhn c s phn b ng u ca cc ht nano silica A200
trong nha nn PEKN.

Hnh 3.9: nh Fe- SEM ca mu vt liu vi s c mt ca 1,75% A200 v 4% GF4.

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Hnh 3.10: nh Fe- SEM ca mu vt liu vi s c mt ca 1,75% A200 v 4% GF4 .

S c mt ca hp cht ghp ni GF4 trong khi trn hp bin tnh nano silica A200
lm tng kh nng phn b ca nano silica A200. Hnh 3.9 v hnh 3.10 cho thy s c
mt ca GF4 cho kt qu kh tt khi phn tn nano silica A200 vo nha PEKN. Cc ht
nano silica phn tn ng u hn v hin tng kt t cc ht nano silica gim kh r rt.

Hnh 3.11: nh Fe-SEM ca mu vt liu cha 1,75% khi lng R7200.

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Hnh 3.12: nh Fe-SEM ca mu vt liu cha 1,75% khi lng R7200.

Quan st nh Fe-SEM ca mu vt liu PC vi cht n nano silica R7200 ta thy
phng php trn hp dung dch gii quyt tt vn phn tn nano silica vo trong
nha nn. Hnh 3.11 v hnh 3.12 cho thy cc ht silica R7200 phn b tch ri v
ng u trong nha PEKN vi kch thc ht vo khong t 10 30 nm. Hin tng kt
t t xy ra do b mt ca nano silica c bin tnh loi b cc nhm chc phn
cc trn b mt. iu ny gii thch ti sao tnh cht ca cc mu vt liu PC vi s gia
cng ca cht n nano silica bin tnh R7200 c cc tnh cht vt tri so vi vt
liu PC t nano silica cha bin tnh A200.
T hnh nh Fe-SEM ca vt liu PC i t nano silica R7200 ta thy phng php
trng hp thng thng s dng trong cng trnh nghin cu gii quyt rt tt vn
phn tn ca silica R7200 trong nha nn.

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Hnh 3.15: nh Fe-SEM ca mu vt liu ch to bng phng php trn hp c s dng

dung mi ph vi hm lng 1,75 % khi lng silica A200 c mt 4% GF4.

Hnh 3.16: nh Fe-SEM ca mu vt liu ch to bng phng php trn hp c s dng

dung mi ph vi hm lng 1,75 % khi lng silica A200 c mt 4% GF4.
Hnh 3.15 v hnh 3.16 th hin cu trc bn trong ca vt liu PC ch to bng
phng php dung mi ph. Kt qu cho thy nano silica phn tn kh tt trong mi
trng nha.

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3.3.2. TEM

Hnh 3.17: Hnh nh TEM ca mu silica phn tn trong metanol sau khi nghin bi.
Hnh nh chp TEM cho ta thy hnh nh phn tn ca silica trong dung mi ph
(metanol). Ta thy silica phn tn ng u trong mi trng dung mi ph vi kch
thc ht ng u t 10 20 nm. iu ny gip cho qu trnh phn tn tip theo ca
silica vo nha nn tr nn d dng hn. Do , gii thch ti sao phng php ch to vt
liu PC bng phng php dung mi ph c cc tnh cht vt tri so vi phng php
ch to bng phng php trn hp thng thng.
3.4. S thay i khi lng ca vt liu PC trong mi trng ha cht
Kt qu nghin cu khi t mu vt liu trong cc dung mi, ha cht bao gm: HNO3
10%, HCl 10%, H2SO4 10%, CH3COOH 10%, NaCl 3%, NaOH 10%, Nc ct, toluen.
Kt qu ca nghin cu c th hin trong bng di y. Vi du + biu din s tng
ln ca khi lng, du biu din s suy gim ca khi lng mu vt liu PC.
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Bng 3.7: S thay i khi lng ca cc mu vt liu PC trong cc mi trng ha cht

Ngy

14

H2SO4

HCl

HNO3 CH3COOH NaCl NaOH

10%

10%

10%

10%

3%

10%

Trng

+0.35

+0.38

+0.35

+0.34

+0.29

A200

+0.40

+0.26

+0.27

+0.27

R7200

+0.34

+0.31

+0.32

Trng

+0.39

+0.40

A200

+0.40

R7200

Nc
ct

Toluen

-1.24

+0.47

+1.56

+0.37

-5.09

+0.43

+2.09

+0.28

+0.46

-3.57

+0.44

+1.82

+0.31

+0.41

+0.36

-1.46

+0.52

+1.65

+0.34

+0.39

+0.40

+0.42

-6.51

+0.62

+1.73

+0.34

+0.38

+0.40

+0.42

+0.59

-4.5 1

+0.54

+1.95

Trng

+0.42

+0.43

+0.33

+0.43

+0.45

-2.41

+0.60

+1.70

A200

+0.41

+0.36

+0.45

+0.45

+0.65 -10.60 +0.70

+1.83

R7200

+0.37

+0.40

+0.46

+0.46

0.67

+2.34

Mu

-7.05

+0.57

Kt qu cho ta thy vt liu PEKN-silica compozit bn vi mi trng axit v trung

tnh. S c mt ca nano silica lm tng nh kh nng hp th cc ha cht c tnh axit v
trung tnh. iu ny c gii thch l do nano silica l hp cht v c c cc mao qun
trn b mt c kh nng hp th cc dung mi ha cht. Nn s c mt ca silica lm gia
tng s hp th dung mi ha cht tuy nhin s gia tng ny l khng ng k, kt qu
nghin cu ln lt sau 3 ngy, 7 ngy v 14 ngy cho thy i vi mi trng axit v
trung tnh khi lng dung mi hp th bi vt liu PEKN-silica compozit sau tng t
gim dn, lng hp th sau 14 ngy tng khng ng k so vi 7 ngy.
i vi mi trng baz do bn thn nha PEKN c cha nhm chc COOH d b
thy phn c bit l trong mi trng kim. S c mt ca nano silica lm tng s phn
hy ca mu vt liu PEKN-silica compozit do silica km bn trong mi trng kim v
s mt mt khi lng tip tc tng u sau 14 ngy ngm.

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PHN 4. KT LUN
Trong cng trnh nghin cu ny, s nh hng ca nano silica (cha bin tnh v
bin tnh) ln cc tnh cht c hc, bn nhit, bn trong cc mi trng ha cht
c nghin cu vi cc kt lun sau:
1.

Kho st nghin cu cc tnh cht c hc vi cc mu vt liu vi hm lng

silica khc nhau t 1,25 2 % tm ra iu kin ti u ch to vt liu
PEKN-silica compozit vi hm lng nano silica ti u l 1,75 (% khi lng
PEKN) v GF4 ti u l 4 % (khi lng nano silica) vi bn ko tng
11,4% bn un tng 16,38%, bn nn tng 6,8%, mi mn tng 11,7%
so vi mu vt liu nha PEKN khng cha cht n.

2.

Quan st nh SEM v Fe-SEM ca mu vt liu ch to cho thy phng

php s dng ch to vt liu PEKN-silica compozit gii quyt tt vn
phn tn ca nano silica trong nha nn PEKN v vn tch dung mi ph ra
khi vt liu.

3.

Kt qu nhn c t cc phng php phn tch nhit DSC v TGA ca vt

liu PEKN-silica compozit cho thy s c mt ca silica lm tng n nh v
lm gim s phn hy do nhit ca vt liu PC.

4.

Kt qu o s thay i khi lng ca mu vt liu khi ngm trong cc mi

trng th hin vt liu PEKN-silica compozit tng i n nh trong cc mi
trng axit v trong mi trng trung tnh, km bn trong mi trng kim.

Cc kt qu nghin cu bc u cho thy nano silica l cht n l tng gip

tng cng tnh cht c l, tng bn, n nh nhit cho vt liu PC. Vt liu i t
nha PEKN v silica c th c s dng trong lnh vc ha phm xy dng nh lm
cht kt dnh cho xy mng, lm cht x l vt nt cho b tng. ng thi cng t nn
mng cho vic s dng nano silica lm cht n tng cng cc tnh cht c l, tnh
cht nhit cho cc loi vt liu PC vi cc cht gia cng khc.

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PHN 5. TI LIU THAM KHO

[1]. ng Vit Hng, Nghin cu ch to vt liu polyme nano compozit trn c s cao
su t nhin v cht n nano . Lun n tin s, i hc Bch khoa H Ni 2009.
[2]. Nguyn Hoi Thu Nghin cu ch to vt liu polyme compozit trn c s nha
polyeste khng no gia cng bng mt na lai to vi si thu tinh. Lun vn thc s.
i hc Bch Khoa- H Ni, 2008.
[3]. Phm Gia Hun, Tnh cht c hc ca vt liu polyme compozit trn c s nha
PEKN gia cng bng si thu tinh v mt tre ch to theo phng php RTM v ht chn
khng. Lun vn thc s. i hc Bch khoa H Ni, 2006.
[4]. P. Singh, A. Kaushik and Kirandeep, Mechanical transport properties of colloidal
Silica Unsaturated polyester composites, Journal of reinforced Plastics and Composites
Vol.25, 119 140, 2006.
[5]. J.F. Watts, P.A. Smith, Processability Studies of Silica-Thermoset Polymer Matrix
Nanocomposites, Polymer Engineering and Science 2008.
[6]. Polyester, Unsaturated; Encyclopedia of Polymer Science and Technology, John
Wiley & Sons; vo.11; 41 65, 2004.
[7]. H. Boenig, Unsaturated Polyesters Structures and Properties, Elsevier Science, Inc,
New York, 1964.
[8]. Hua Zou; Shhan Wu; Jian Shen; Polymer/Silica Nanocomposites: Preparation,
Characterization, Properties, and Applications; Chemnical Reviews; Nanjing Normal
University; August 2007; vol.108, No. 9; 3893 3957.
[9]. Miroslav Jancek; Polymer/Silica Nanocomposite System; TBU in Zln Faculity of
Technology - 2007.
[10]. Martin J.Schich, Athur T.Hubbard, Colloidal silica fundamental and
applications, Taylor and friencis group, (2006).
[11]. Pau F. Bruins. Unsaturated Polyester Technology. Polytechnic Institite of New
York. Gordon and Breach Pulishers 1978.
[12]. P.M. Ajayan, L.S.schadler, P.V.braun, Nanocomposite science and technology,
WILEY-VCH verlag GmbH Co.KGaA, Weinheim ISBN, (2003).
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