IPC-TM-650 EN 2022 试验方法.pdf - 第318页

6.1 Calibration of the instrument must be carried out according to the manufacturer’s recommendations. Two cali- brations are required, one to establish the baseline and the other to calibrate the TMA relative to a stand…

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

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

)

and tangent B (T

)

(i.e., the

transition range), e.g., transition range: 160-205°C.

6.0

Notes

2.4.24.3-01

Figure

emperature

Tangent A

Tangent 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.

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6.1

Calibration

of the instrument must be carried out

according to the manufacturer’s recommendations. Two cali-

brations are required, one to establish the baseline and the

other to calibrate the TMA relative to a standard.

6.2

quartz specimen of 11-13 mm in length (between the

grips) is run at 5°C/min under inert gas purge (He) from −20

to 400°C to establish a baseline. The baseline is used to elimi-

nate the effects of grip expansion on extension measure-

ments. The coefficient of linear thermal expansion of quartz is

0.57 x 10

-6

/°C

(16-500°C)

6.3 After

the baseline is established, the TMA must be cali-

brated with at least one standard being 99.9999% pure alu-

minum which has a linear CTE of 24.9 x 10

-6

/°C

from

0-250°C. An aluminum specimen is run between -10 and

200°C and the coefficient of linear thermal expansion is calcu-

lated. If the measured value differs from the literature value,

the specimen size is adjusted to correspond to the measured

value, and the specimen is rerun. Once the measured and lit-

erature values are in agreement, this constant factor is used

on subsequent specimen sizes.

6.4

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-10 Hz) or 141°C (DSC-5°C/min).

6.5

general, DMA is more sensitive that DSC or TMA. This

is especially important for high temperature polymers with

weak transitions.

Lange’s Handbook of Chemistry, 12th edition, J. A. Dean, ed., McGraw-Hill, New York (1979).

IPC-TM-650

Number

2.4.24.3

Subject

Glass

Transition Temperature of Organic Films − TMA Method

Date

7/95

Revision

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Scope

This

test is designed to determine the glass tran-

sition temperature (T

)

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.

Applicable Documents

2.1 ASTM Documents

E 1640

Test

Method for Assignment of the Glass Transition

Temperature by Dynamic Mechanical Analysis

4065

Standard

Practice for Determining and Reporting

Dynamic Mechanical Properties for Plastics

4092

Standard

Terminology Relating to Dynamic Mechani-

cal Measurements on Plastics

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

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.

Apparatus or Material

4.1

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

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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