IPC-TM-650 EN 2022 试验方法.pdf - 第316页

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 de…

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1.0
Scope
This
test method establishes a procedure for
determining the glass transition temperature of organic films
using dynamic mechanical analysis (DMA).
2.0
Applicable Documents
ASTM D 618
Standard
Practice for Conditioning Plastics and
Electrical Insulating Materials for Testing
3.0
Test Specimen
The
test specimen shall consist of a
strip 22.5 mm long and 6.25 mm wide with a minimum thick-
ness of 5 µm. The analysis is based on the assumption of a
constant specimen geometry, therefore the test specimens
must be stiff enough not to plastically deform during the
experiment.
4.0
Apparatus or Material
Rheometrics
Solids Analyzer
Model RSA-II with a film/fiber fixture or equivalent.
5.0
Procedure
5.1
The
test specimens should be conditioned at 23 ± 2°C
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.
5.3 Mount
the specimen in the film/fiber fixture. Make certain
that the specimen is mounted perpendicular to the clamps.
Hand tighten the clamps as much as possible to prevent
specimen slippage during a run.
5.4
Operate
at a frequency of 1 Hz (6.28 radians/sec). Heat
the specimen in dry nitrogen at a rate of no faster than 2°C/
min., or in steps of 5°C increments, in dry air.
5.5
When
the transition has been observed, heat at least
50°C beyond the apparent completion of the thermal activity
before returning to initial conditions.
5.6
The
glass transition temperature is defined as the tem-
perature corresponding to the maximum in the tan δ vs. tem-
perature curves at a frequency of 1 Hz. Tan δ is calculated
from
tan δ= E’’/E’
where E’’ is the loss modulus and E’ is the storage modulus.
A typical plot is shown in Figure 1.
5.7
Report
both the glass transition (maximum in tan δ), e.g.,
200°C (DMA-1 Hz), and the temperature range over which the
storage modulus (E’) changes (i.e., the transition range), e.g.,
transition range: 160-205°C.
6.0
Notes
6.1
Calibration
of the instrument must be carried out
according to the manufacturer’s recommendations with at
least one standard being indium.
6.2
The
glass transition temperature for a given material will
be significantly different depending on the method of analysis
(i.e, DMA, DSC, or TMA). The glass transition determined by
DMA is frequency dependent and increases with increasing
frequency. The glass transition determined by DSC or TMA
will depend on the heating rate. The test method used along
with the frequency (DMA) or heating rate (DSC or TMA) should
be noted beside the glass transition value, e.g., 135°C
(DMA-1 Hz) or 141°C (DSC-5°C/min).
2.4.24.2-01
Figure
1
Temperature (°C)
E
1
(dynes/cm
2
)
10
11
10
10
10
9
10
8
0
50 100 150 200 250 300 350 400
0.0
0.2
0.4
0.6
0.8
1.0
TAN δ
E
1
TAN δ
200°C
The
Institute for Interconnecting and Packaging Electronic Circuits
2215 Sanders Road • Northbrook, IL 60062-6135
IPC-TM-650
TEST
METHODS MANUAL
Number
2.4.24.2
Subject
Glass
Transition Temperature of Organic Films −
DMA Method
Date
7/95
Revision
Originating Task Group
Deposited Dielectric Task Group (C-13a)
Material
in this Test Methods Manual was voluntarily established by Technical Committees of the IPC. This material is advisory only
and its use or adaptation is entirely voluntary. IPC disclaims all liability of any kind as to the use, application, or adaptation of this
material. Users are also wholly responsible for protecting themselves against all claims or liabilities for patent infringement.
Equipment referenced is for the convenience of the user and does not imply endorsement by the IPC.
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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.
IPC-TM-650
Number
2.4.24.2
Subject
Glass
Transition Temperature of Organic Films − DMA Method
Date
7/95
Revision
P
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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
ASTM D 618
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 µm.
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 µm thick.
5.0
Procedure
5.1
The
test specimens should be conditioned at 23 ± 2°C
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°C/min
under inert atmosphere from ambient to 50°C 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°C below the transition temperature observed
in the prescan.
5.7
Hold
the temperature for 10 min.
5.8
Reheat
the specimen at a rate of 5°C/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.
5.11
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°C (TMA-5°C/min), and the temperatures at
the beginning of tangent A (T
A
)
and tangent B (T
B
)
(i.e., the
transition range), e.g., transition range: 160-205°C.
6.0
Notes
2.4.24.3-01
Figure
1
T
emperature
Tangent A
Tangent B
T
A
T
B
Extension
The
Institute for Interconnecting and Packaging Electronic Circuits
2215 Sanders Road • Northbrook, IL 60062-6135
IPC-TM-650
TEST
METHODS MANUAL
Number
2.4.24.3
Subject
Glass
Transition Temperature of Organic Films −
TMA Method
Date
7/95
Revision
Originating Task Group
Deposited Dielectric Task Group (C-13a)
Material
in this Test Methods Manual was voluntarily established by Technical Committees of the IPC. This material is advisory only
and its use or adaptation is entirely voluntary. IPC disclaims all liability of any kind as to the use, application, or adaptation of this
material. Users are also wholly responsible for protecting themselves against all claims or liabilities for patent infringement.
Equipment referenced is for the convenience of the user and does not imply endorsement by the IPC.
P
age1of2
电子技术应用　　　　　　　ｗｗｗ．ＣｈｉｎａＡＥＴ．ｃｏｍ