IPC-TM-650 EN 2022 试验方法.pdf - 第320页

5.1.2 Specimens shall be cut to the specified size using appropriate procedures and equipment to minimize thermal shock and mechanical stress. Method A specimens shall have their edges smooth and burr-free by means of sa…

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1
Scope
This
test is designed to determine the glass tran-
sition temperature (T
g
)
and room temperature storage modu-
lus (E’) of dielectric materials used in High Density Intercon-
nect (HDI) and Microvias by the use of dynamic mechanical
analysis (DMA).
When testing a stand alone HDI dielectric layer, DMA will pro-
vide modulus as a function of temperature and glass transition
for this layer. When DMA is used on built-up constructions,
the data will be a complex curve representing the composite
moduli and glass transitions.
Two methods are presented:
• Method A for thick specimens
• Method B for thin specimens (recommended for HDIS and
Microvia dielectric layers).
For anisotropic materials (reinforced dielectrics), the x and y
directions will have different modulus vs. temperature behav-
ior. Anisotropic materials shall be tested in both the x and y
directions.
2
Applicable Documents
2.1 ASTM Documents
E 1640
Test
Method for Assignment of the Glass Transition
Temperature by Dynamic Mechanical Analysis
D
4065
Standard
Practice for Determining and Reporting
Dynamic Mechanical Properties for Plastics
D
4092
Standard
Terminology Relating to Dynamic Mechani-
cal Measurements on Plastics
3
Test Specimen
3.1 Size
Method A
Flexural
bending geometry thick specimens
(>0.5 mm): Specimens shall be approximately 8 mm to 12
mm wide, 20 mm to 40 mm long, and 1 mm to 2 mm thick.
The thickness shall be a minimum of 0.5 mm; for thicknesses
<0.50 mm, use Method B. An aspect ratio of length/thickness
= 10/1 or greater should be maintained. Exact specimen
dimensions should be determined by the apparatus used.
Method
B
Thin
film tension geometry thin specimens
(<0.50 mm): Specimens shall be approximately 15 mm to 20
mm long and 2 mm wide. The minimum thickness is deter-
mined by the strength of the material; it should not break dur-
ing testing. Exact specimen dimensions may be determined
by the apparatus used.
3.2
All
specimens should be fully cured according to manu-
facturer’s recommendations. Thick specimens may be made
by use of multiple lamination/cure cycles if required.
3.3
Unless
otherwise specified, one specimen shall be
tested, to be taken from a random location in the material in
question.
4
Apparatus or Material
4.1
A
DMA capable of determination of modulus to +1%
precision and tan δ resolution of 0.01 over the specified tem-
perature range. The DMA will preferably have computer data
acquisition and analysis. The DMA must have an environmen-
tal chamber capable of having inert flush gas and capable of
heating the specimen to at least 310°C.
4.2
Diamond
blade or saw, sanding equipment, or equiva-
lent to provide specimens of the size and edge quality
required for Method A
4.3
Scissors,
razor blades, or equivalent to provide speci-
mens of size and edge quality for Method B
4.4
Air
circulating oven capable of maintaining 105°C ± 2°C
4.5
Dessicator
capable of an atmosphere <30% RH at 23°C
4.6
Etching
system capable of complete removal of metallic
cladding
5
Procedure
5.1.1
Metallic
clad specimens shall be tested without the
cladding. Etch and dry using appropriate procedures and
equipment.
The
Institute for Interconnecting and Packaging Electronic Circuits
2215 Sanders Road Northbrook, IL 60062-6135
IPC-TM-650
TEST
METHODS MANUAL
Number
2.4.24.4
Subject
Glass
Transition and Modulus of Materials Used in
High Density Interconnection (HDI) and Microvias -
DMA Method
Date
11/98
Revision
Originating Task Group
HDI Test Methods Task Group (D-42a)
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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5.1.2
Specimens
shall be cut to the specified size using
appropriate procedures and equipment to minimize thermal
shock and mechanical stress. Method A specimens shall have
their edges smooth and burr-free by means of sanding or
equivalent (to allow the specimen to rest flat on the mounting
stage). Method B specimens shall be rectangular, with their
long edges parallel (to ensure good mounting in the film fix-
ture). Method B specimens shall have smooth edges without
nicks or tears.
5.1.3 Specimens
shall be preconditioned by baking for one
hour ± 15 minutes at 105°C, then cooled to room temperature
in a dessicator.
5.2
Measurement
5.2.1 Apparatus Set-up
5.2.1.1 Install the Required DMA Clamp
Method A
Install
and calibrate the DMA with a bending
geometry fixture/clamp.
Method
B
Install
and calibrate the DMA with a thin film
fixture/clamp.
5.2.1.2
Start the Experiment
Method A
Measure
the length, width, and thickness of the
specimen to within at least +0.01 mm or preferably +0.005
mm. Clamp the specimen in the DMA fixture. Set the sample
strain amplitude to operate within the linear viscoelastic range
of the material. Strains <1% are recommended and are typi-
cally 0.1%. Program the sample temperature range. Enclose
the specimen and fixture in the environmental chamber (fur-
nace).
Method
B
Measure
the length, width, and thickness of the
specimen to within at least +0.01 mm or preferably +0.005
mm. Sample lengths of 10 mm to 20 mm are typical. Mount
the specimen in the clamps of the film fixture according to the
manufacturer’s instructions. Apply tension force between 10 g
and 50 g. A typical base force would be 20 g (see 6.5 for an
explanation of the load criteria). Enclose the specimen and
probe in the environmental chamber.
5.2.1.3
Provide
an inert gas purge (helium or nitrogen) to the
environmental chamber. Temperature calibration of the DMA
must be performed under the same gas conditions.
5.2.2
Running the DMA Temperature Scan
5.2.2.1 Initial Temperature (T
initial
)
a.
For specimens with T
g
below
or near room temperature,
start the scan at least 20°C below the anticipated transi-
tion. This may require a DMA with subambitent cooling
control of the environmental chamber.
b. For specimens with T
g
greater
than room temperature,
start the scan at 30°C.
5.2.2.2
Sample Heating and Deformation Rate
The
specimen
shall be run at 2°C/min and an oscillation frequency
of 1 Hz.
5.2.2.3
Temperature Excursion
Heat
the specimen to at
least 20°C greater than the T
g
.
This test is general in nature
and data may be taken above T
g
if
required. There is no
required upper temperature.
5.3
Evaluation
5.3.1
The
DMA storage modulus should resemble the plot
shown in Figure 1.
5.3.2
An
idealized DMA curve has a linear section below the
transition (glassy region below the temperature of T
g
)
and a
stepwise drop through the glass transition region. These linear
sections are used in calculating T
g
by
onset of the modulus
drop (see Figure 1).
IPC-24244-1
Figure
1 DMA Modulus Plot
IPC-TM-650
Number
2.4.24.4
Subject
Glass
Transition and Modulus of Materials Used in High Density
Interconnection (HDI) and Microvias - DMA Method
Date
11/98
Revision
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5.3.3
Examine
all specimens after the test to look for signs
of excessive loads, distortions, tears, and other defects. If any
defects or sample irregularities are found, discard the sample
and the data, rerun another specimen, or pick a different
method for determining T
g
and
storage modulus.
5.4
Calculations
5.4.1 Glass Transition Temperature (T
g
)
Construct
a
tangent line to the curve below the transition temperature in
the modulus curve. Construct a tangent to the storage modu-
lus curve at or near the inflection point approximately midway
through the step change in the transition. The temperature
where these tangents intersect is the reported T
g
for
the
material. For consistency it is recommended that the DMA
computer analysis software be used for this calculation. See
Figure 1 for an example of this tangent intersection method.
5.4.2
Storage Modulus (E’)
The
sample storage modulus
(E’) shall be calculated at room temperature (22°C) and
reported in units of Pa (N/m
2
).
For consistency it is recom-
mended that the DMA computer analysis software be used for
this geometry specific calculation.
5.4.3
Alternative
thermal transitions may be reported as the
transition peak temperature in the sample loss modulus (T
I
)o
r
tan δ plots (T
t
)
(see Figure 2 and Figure 3).
5.5
Report
5.5.1
Report
the glass transition temperature 22°C (room
temperature) for each specimen, rounding to the nearest
whole number.
5.5.2
Report
the modulus in units of Pa (N/m
2
)
at 22°C.
5.5.3
For
anisotropic (reinforced) samples report the both
the x and y direction modulus.
5.6
Plot
5.6.1
Plot
the storage modulus vs. temperature (°C) for the
specimen. If using computer-based analysis, include the T
g
IPC-24244-2
Figure
2 DMA Tan Delta Plot
Note: T
t
is
the transition peak temperature.
IPC-24244-3
Figure
3 DMA Loss Modulus Plot
Note: T
I
is
the transition peak temperature.
IPC-TM-650
Number
2.4.24.4
Subject
Glass
Transition and Modulus of Materials Used in High Density
Interconnection (HDI) and Microvias - DMA Method
Date
11/98
Revision
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