Báo cáo " Nghiên cứu phản ứng khâu mạch quang hóa của một số hệ khâu mạch quang trên cơ sở glyxydylete của nhựa o- crezolfomandehyt " ppt

Tgp chi Hoa hoc, T. 47 (6), Tr. 685 - 690, 2009
NGHIEN
CQU
PHAN
LTNG
KHAU MACH QUANG HOA CUA
MOT SO HE KHAU MACH QUANG TREN CO
s6
GLYXYDYL ETE
CUA
NHl/A
0-CREZOLFOMANDEHYT
I - ANH
HLfdNG
CUA TY LE CHAT
KHOl
MAO QUANG CATION TAS DEN PHAN
L/NG
KHAU MACH QUANG HOA QUA HE
CG-BGDE-TAS
Den Tda soan 5-5-2008
LE XUAN HIEN,
D6
THI NGOC
MJNU,
NGUYEN THI VIET TRIEU
Vien Ky thuat nhiet ddi, Vien Khoa hgc vd Cong nghe Viet Nam
ABSTRACT
The influence of the content of cationic photoinitiator-triarylsulfonium salt (TAS) on the
photocrosslinking of the systems containing glyxydyl ete of
o-crezolformaldehyde

resine (CO),
hiscycloaliphatic diepoxy monome (BCDE) with the mass ratio CGIBCDE
= 111
has been
studied.
The study of
the
photopolymerization of
the epo.vy
group in the 20
jjin
thickness
film
of
the
system
hy IR - Spectroscopy in the presence of TAS in the
range
from 1% to 7% of the total mass of the
CO and BCDE showed the fastest convertion rate of
the
TAS and epoxy groups at the content of
TAS
5%. leading to the final convertion
of
TAS,
epo.xy
groups of BCDE and the total epoxy groups
ofCG
and BCDE 99%.

98%
and 82% respectively after
exposure
under 250 mW/cnr intensity
UV - lamp.
I - MO DAU
Do cd nhieu uu dilm ndi bat, viee che tao
cac idp phu bao ve, trang tri bing phuang phap
quang hda dang ed tdc do phat trien nhanh va
iirng
dung trong nhilu
ITnh
vuc ky thuat, ddi
sdng
[1,2].
Trong dd, khau mach quang hda cae
hgp cha't chiia nhdm epoxy cd hieu qui cao, tao
mang ddng rin chit lugfng tdt dang thu
hiit
su
quan tam
chii
y
ciia
nhilu nha nghien
cii*u
[3, 4].
Nhua epoxy novolac sau khi ddng ran cd
nhilu tinh nang quy, cd do
bin

hda chit,
bin
nhiet cao [5]. Tuy nhien, cac
kit
qui nghien
ciiu
khau mach quang hda nhua epoxy novolac vi
tfnh chat
ciia
sin phim cdn it dugc cdng bd.
Phan irng khau mach quang hda
ciia
he khau
mach quang tren ca sd nhua va monome chiia
nhdm epoxy, chat khai mao quang cation chiu
anh hudng
ciia
nhilu yeu td nhu bin cha't va ty
le cac hgp phin,
chilu
day mang, cudng do
biic
xa [1 - 4, 6 -
11].
Bai bao nay trinh bay
kit
qua nghien
ciiu
anh hudng
ciia

ham lugng chat
khai mao quang cation TAS de'n qua trinh khau
mach
ciia
he khau mach quang tren ca sd
glyxydyl ete
ciia
nhua
o-crezolfomandehyt,
bisxycloaliphatic diepoxy monome va chit khai
mao quang cation - mudi triarylsunfoni.
II - THUC NGHIEM
1.
Nguyen lieu va hda chat
- Glyxydyl ete cua nhua o-crezolfomandehyt
(CG)
ciia
hang
Sigma-Aldrich,
Dire, ham lugng
nhdm epoxy 2,7
mol/kg.
- Monome bisxycloaliphatic diepoxy (BCDE
- loai Cyracure 6105
ciia
hang UCB, cd ham
685
lugng nhdm epoxy = 7,9 mol/kg.
- Chit khai mao quang cation: mudi
triarylsunfoni (TAS) - loai Cyracure

UVI
- 6974
ciia
hang Ciba.
- Clorofom - loai P cua Ba Lan.
2.
Tao he khau mach quang
He khau mach quang dugc tao bing each
trdn
diu
cac td hgp nhua CG vdi monome
BCDE va chit khai mio quang cation TAS theo
ty le trgng lugng CG/BCDE = 50/50, chiia tir 1 -
7%
TAS so
vdd
tdng trgng lugng
eiia
CG va
BCDE.
3.
Khau mach quang
Miu khau mach quang dugc tao mang ed do
day 20
jam
tren vien KBr, dugc chilu dudi den
tir ngoai cudng do 250
mW/em'
tren miy
FUSION UV model F 300S (My) tai Vien Ky

thuat nhiet ddi (Vien KTND), Vien Khoa hoe vi
Cdng nghe Viet Nam (Vien
KHc&'CNVN).
4.
Phan tich hong ngoai
Phan tich hdng ngoai dugc thuc hien tren
may FT-IR NEXUS 670 NICOLET (My) tai
Vien KTND, Vien KH&CNVN. Biln ddi cac
nhdm dinh chdc
ciia
he khau mach quang trong
thdi gian chieu tia tir ngoai dugc xac dinh dua
vao
sir
thay ddi cudng do hip thu dac trung cua
chiing tren phd hdng ngoai. Cic bien ddi nay
cdn dugc xac djnh dinh
lugng
theo phucmg phap
ngi chuin dua vao hip thu dae trung
eiia
dao
dgng hda tri
eiia
lien ket doi trong vdng tham tai
1506 cm"', khdng thay ddi trong qua trinh chilu
tia tir ngoai.
Ill
- KET QUA VA THAO LUAN
Nghien

ciiu
phd hdng ngoai cua ming trong
qua trinh chieu tia tir ngoai cho thiy eae hip thu
dac trung cho lien
kit
C-H no trong dai 2847 -
2935 cm', 1470 - 1434 cm', 1393 - 1300 cm'
va hip thu dac trung eho dao dgng hda tri cua
lien
kit
ddi trong vdng tham tai 1506 cm' cung
nhu cudng do cua chiing khdng thay ddi. Cudng
dd cac hip thu cd sd sdng 3475 em"' va 1084
em' dac trung cho nhdm hydroxyl vi nhdm ete
tang len. Cae hip thu cd sd sdng 914, 790, 1798
cm' dac trung cho tdng lugng nhdm epoxy
ciia
686
CG va BCDE, nhdm epoxy cua BCDE va TAS
giam rat manh. Vi vay,
sir
thay ddi cudng do cua
eae hip thu niy da dugc khao sat bing phuang
phap ngi chuan theo cudng do hip thu dac trung
eho dao dgng hda tri
ciia
lien ket ddi trong vdng
tham tai 1506 em"'.
Bie'n ddi ham lugng TAS trong cac he cd ty le
chit khai mao khic nhau khi chieu tia tir ngoai

mang diy 20
)im
dugc trinh bay tren hinh
1.
Tir hinh 1 ed thd thay khi ham lugng TAS
trong he cd gia tri 1%, 3%, 4%, 5%, 7% lugng
TAS cdn lai sau 18 giay chieu tir ngoai tucmg
ling 22%, 8%, 6%, 1%, 15% gia tri ban diu.
Bie'n ddi tdng lugng nhdm epoxy
ciia
nhua
CG va monome BCDE cung nhu bien ddi ham
lugng nhdm epoxy
ciia
monome BCDE trong
cac he ed ty le chit khai mao khac nhau khi
chieu tia tir ngoai mang day 20
)j.m
dugc trinh
biy
tren
hinh 2 va 3.
Tir hinh 2 cd the thay khi ham lugng TAS
thay ddi tir 1% de'n 7%, tdng lugng nhdm epoxy
cua nhua CG vi monome BCDE giam nhanh
trong khoang tir 0,3 - 1,2 giay dau
ciia
phan
ung, dat eae do chuyin hoa 22%, 38%, 42%,
54%,

30% tuong irng vdi ham lugng TAS trong
he 1%, 3%, 4%, 5%, 7%. Sau dd,
chuydn
hoa
nhdm epoxy cham dan va hau nhu
biSn
ddi
khdng dang ke, dat cic gia tri 28%, 64%, 72%,
82%,
46%
sau 18 giay.
Chuyen hoa nhdm epoxy
ciia
BCDE trong
qua trinh chieu tia tir ngoai cung cd quy luat
tuang tu nhu chuyen hda tdng lugng nhdm
epoxy cua nhua CG vi monome BCDE (hinh 3),
giam manh trong khoang
1,2
giay diu
ciia
phan
iing vdi
miic
chuyen hoi 64%, 76%, 82%, 86%,
66%
khi ham lugng TAS tucmg dng 1%, 3%,
4%,
5%, 7%, bie'n ddi cham din va hiu nhu
khdng thay ddi, dat cac gia tri chuyen hoa 73%,

92.%,
94%, 98%, 82% sau 3,6; 6; 12; 18 giay
chieu.
Ciing vdi bie'n ddi ham lugng nhdm epoxy,
mat do quang tai 1084 em"' dae trung cho hip
thu
ciia
lien ket ete C-O-C (hinh 4) va tai 3475
cm ' dae trung cho hap thu
eiia
lien
kit
O-H
(hinh 5) tang len ro ret trong qui trinh chiiu tia
tir ngoai.
<;
CO
5-
_5
E
X
100
80
60
40
20
Ham lugng TAS (%): • 1;
-3;
A
4;

x
5; * 7
20
Thai gian chieu, sec
Hinh
1:
Bie'n ddi ham lugfng TAS trong qua trinh chieu tia tu ngoai he khau mach quang
CG-BCDE-TAS
g
o.
a
.a
c
S
/rt
0
-
0
5 10 15 20
Thai gian chieu, sec
Ham lugng TAS (%):
•I;
•3;
A
4; x 5;
*
7
Hinh 2: Bien ddi tdng lugng nhdm epoxy
eiia
CG vi BCDE trong qua trinh chieu tia tir ngoai he

khau mach quang CG-BCDE-TAS
687
^
100
f
X
o
n.
E
^o
J2
C
60
g.
S
E
.•rt
80
60
40
20
0
0
10 15
20
Thdi gian chieu, see
Ham lugng TAS (%): • 1; • 3;
A
4;
x

5;
* 7
Hinh 3: Biln ddi ham lugng nhdm epoxy
ciia
BCDE trong qua trinh chieu tia tir ngoai he khau
mach quang CG-BCDE-TAS
D1084cm"'/D1506cm"'
0.8
n
0.6
0.4
0.2
5 10
Thdi gian chieu (giay)
15
20
Ham lugng TAS (%):
•I;
.3; A 4;
x
5; *7
Hinh 4: Bien ddi ti sd D1084 cm"'/D1506 cm"' tren phd hdng ngoai
ciia
he khau mach quang
CG-BCDE-TAS trong qua trinh chieu tia tir ngoai
688
D3475cm"'/D1506cm"'
0.8
0.6
0.4

0.2
5 10 15
Thdi gian chieu, sec
Ham lugng TAS (%):
•I;
•3;
A
4;
20
x5;
*7
Hinh 5: Bien ddi ti so D3475
cm"'/D1506
cm"' tren phd hdng ngoai cua he khau mach quang
CG-BCDE-TAS trong qua trinh chie'u tia tir ngoai
Nhiing
kit
qua trinh bay tren cac hinh 1 - 5
cho thiy he vdi ham lugng TAS 5% cd chuyen
hda nhdm epoxy cao, tao
nen
nhilu lien
kit
ete
va lugng TAS du sau khi chieu tia tir ngoai
khdng nhilu.
Kit
qua nay dugc giai thich bing
hieu ling chin anh sang
ciia

cac phin tir trong
chat khai mao quang. Ham lugng chit khai mao
tang thiic day phan
iing
triing hgp quang do tang
kha nang tao thanh proton de khai mao phan
iimg
nhung ddng thdi ciing tang
sir
che chin anh
sang tir ngoai
lim
giim tdc do phan quang
ciia
chat khai mao. Su canh tranh
eiia
hai xu the nay
la nguyen nhan lam he chiia lam lugng TAS ban
dau 5% ed chuyen hoa TAS, cac nhdm epoxy
nhanh va nhilu nhat trong qua
trinh
chilu tia tir
ngoai.
IV - KET LUAN
Da khio sat qua trinh khau mach quang cua
mang tren ca sd nhua epoxy novolac CG,
monome epoxy Cyracure BCDE, chit khai mao
quang cation - mudi triarylsunfoni TAS vdi ty le
chat khai mao khac nhau.
Da lua chgn dugc he khau mach quang vdi

ty le cac hgp phin CG/BCDE/TAS = 50/50/5 cd
tdc do chuyen hoa TAS, cac nhdm epoxy cao va
cd gia tri chuyen hoa TAS cao nhit, cd chuyin
hoa nhdm epoxy
ciia
BCDE va tdng lugng nhdm
epoxy tucmg
iing
99%, 98% va 82% khi chilu
tia tir ngoai.
Ldi cam
ofn:
Tap the tdc gid chdn thdnh cdm an
chuong trinh nghien
cihi
co bdn trong
ITnh vifc
Khoa hoc
Tii
nhien dd ho trg kinh phi de hodn
thdnh cong trinh ndy.
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2.
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James V. Crivello. Nuclear Instruments and
Methods in physics research B,
151,
8 - 21
(1999).
689
5.
6.
Anthony Kelly, Carl Zweben, Comprehensive
composite
materials.
Vol.
U,
3 - 18,
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