IPC-TM-650 EN 2022 试验方法--.pdf - 第316页

IPC-TM-650 Number Subject Date Revision Page 2 of 2 2.4.24.2 Glass Transition Temperature of Organic Films - DMA Method 7/95 6.3 In general, DMA is more sensitive that DSC or TMA. This is especially important for high te…

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Figure 1 Cutaway view of vitreous silica tube dilatometer
IPC-TM-650
Number
Subject Date
Revision
Page 2 of 3
5.2.2
Condition
E-1/1
10.
5.3.4
Recommended
standard
reference
materials:
5.2.3
Condition
-40/23/50.
5.3
Calibration
5.3.2
The
temperature
sensor
shall
be
calibrated
according
to
an
appropriate
ASTM
method
(E-220)
or
procedure
recom¬
mended
by
the
National
Bureau
of
Standards.
•
OFHC
Copper;
GTE
1
7.3
PPM/℃
(for
use
with
“high
expansion"
materials)
5.3.3
The
dilatometer,
as
a
total
system,
shall
be
calibrated
by
measuring
two
reference
materials
of
known
thermal
expansion.
One
of
the
materials
should
have
an
expansion
close
to
the
sample
specimen,
and
the
other
close
to
that
of
the
dilatometer.
5.3.1
The
transducer
shall
be
calibrated
by
imposing
a
series
of
known
displacements
with
a
precision
screw
micrometer
or
set
of
end
gage
blocks.
•
NBS
Fused
Silica
-
SRM
739;
CTE
.55
PPM/℃
(for
cali¬
bration
of
dilatometer)
5.3.5
The
expansion
of
the
dilatometer
system,
(AL/LO)S,
and
the
calibration
constant,
for
corrections
of
lead
lag,
tem¬
peratures,
etc.,
are
determined
at
20℃
intervals
using
the
fol¬
lowing
equations:
(A^LO)S
=
(AULJ
-
(AULJm
•
NBS
Single
Crystal
Sapphire
-
SRM
732;
CTE
~
5.5
PPM/℃
(for
use
with
l1ow
expansion"
materials)
尚
「代）
s
A
=
2.4.41.1
A
Coefficient
of
Thermal
Expansion
by
the
Vitreous
Silica
(Quartz)
Dilatometer
Method
8/97
给
m
IPC-TM-650
Number
Subject Date
Revision
Page 2 of 2
2.4.24.2
Glass
Transition
Temperature
of
Organic
Films
-
DMA
Method
7/95
6.3
In
general,
DMA
is
more
sensitive
that
DSC
or
TMA.
This
is
especially
important
for
high
temperature
polymers
with
weak
transitions.
6.4
If
the
polymer
decomposes
before
the
glass
transition
is
reached,
report
the
decomposition
temperature
and
indicate
that
it
is
a
decomposition
temperature
and
not
a
glass
transi¬
tion
temperature.
ASTM D 618
Figure 1
Temperature
Tangent A
Tangent B
T
A
T
B
Extension
The Institute for Interconnecting and Packaging Electronic Circuits
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Page 1 of 2
IPC-TM-650
TEST
METHODS
MANUAL
1
.0
Scope
This
test
method
establishes
a
procedure
for
determining
the
glass
transition
temperature
of
organic
films
using
thermal
mechanical
analysis
(TMA).
2
.0
Applicable
Documents
Standard
Practice
for
Conditioning
Plastics
and
Electrical
Insulating
Materials
for
Testing
3
.0
Test
Specimen
The
test
specimen
shall
consist
of
a
strip
15-20
mm
long
and
2
mm
wide
with
a
minimum
thick¬
ness
of
10
gm.
4
.0
Apparatus
or
Material
Perkin-Elmer
TMA-7
with
a
film
fixture
in
extension
mode
or
equivalent
equipment
capable
of
handling
films
less
than
25
|im
thick.
5
.0
Procedure
5.1
The
test
specimens
should
be
conditioned
at
23
±
2
℃
and
50
±
5%
relative
humidity
for
not
less
than
24
hours
prior
to
testing.
Refer
to
ASTM
D
618.
5.2
Follow
the
manufacturer's
recommendations
for
equip¬
ment
startup
and
calibration.
5.2
Mount
the
test
specimen
in
the
film
holder.
The
sample
length
(between
the
grips)
should
be
between
11-13
mm.
5.3
Set
the
force
at
30
mN.
5.4
Perform
a
prescan
by
heating
at
a
rate
of
20℃/min
under
inert
atmosphere
from
ambient
to
50℃
beyond
the
apparent
completion
of
the
thermal
activity
to
erase
previous
thermal
history.
5.5
Hold
the
temperature
for
10
min.
5.6
Cool
to
50℃
below
the
transition
temperature
observed
in
the
prescan.
Number
2.4.24.3
Subject
Glass
Transition
Temperature
of
Organic
Films
一
TMA
Method
Date
Revision
7/95
Originating
Task
Group
Deposited
Dielectric
Task
Group
(C-13a)
5.8
Reheat
the
specimen
at
a
rate
of
5
℃/min
until
all
desired
transitions
have
been
completed.
5.9
The
glass
transition
is
determined
by
a
construction
pro¬
cedure
on
the
transition
region
of
the
extension
versus
tem¬
perature
curve
(Figure
1).
5.10
Construct
a
tangent
line
to
the
curve
above
and
below
the
transition.
5.1
1
The
temperature
at
which
the
tangents
intersect
is
the
glass
transition
temperature.
5.12
Report
both
the
glass
transition
(intersection
of
tan¬
gents),
e.g.,
200℃
(TMA-5℃/min),
and
the
temperatures
at
the
beginning
of
tangent
A
(TJ
and
tangent
B
(TB)
(i.e.,
the
transition
range),
e.g.,
transition
range:
1
60-205℃.
6
.0
Notes
5
.7
Hold
the
temperature
for
10
min.