IPC-TM-650 EN 2022 试验方法.pdf - 第330页

5.3.3 Record the temperature, T d (2%), at which the mass of the sample is 2.0% less than its mass measured at 50°C. 5.3.4 Record the temperature, T d (5%), at which the mass of the sample is 5.0% less than its mass meas…

1 Scope This test method establishes a procedure for

determining the thermal decomposition temperature (T

)of

base laminate materials using thermogravimetric analysis

(TGA). Use of this test method for printed wiring boards or

other composites may not yield comparative results.

2 Applicable Documents All terms and definitions in this

document conform to IPC-T-50, Terms and Definitions for

Interconnecting and Packaging Electronic Circuitry.

3 Test Samples

3.1 Sample Construction

The sample may be an unclad

laminate material or laminate material with copper completely

removed and that has been cut (using water cooling/cleaning

only, no oil) approximately square to fit into the TGA sample

pan. Typical sample mass (weight) is 10 mg to 30 mg.

Samples shall be cut to the specified size using appropriate

procedures and equipment to minimize mechanical stress

and/or thermal shock.

Note: Samples of the same mass but with a smaller surface

area may lose mass at a slower rate.

3.2 Surface Preparation All edges of the sample shall be

finished smooth and burr-free by sanding or equivalent (to

allow the sample to rest completely flat on the sample pan).

Use care to minimize the introduction of mechanical stress or

heat to the sample.

3.3 Mass Measurement The accuracy of the mass mea-

surements shall be within ± 0.01 mg.

4 Equipment/Apparatus or Material

4.1 Thermogravimetric Analyzer (TGA)

Thermal gravi-

metric analysis instrument shall comprise the following:

4.1.1 Microbalance, null type, sensitive to 0.001 mg.

4.1.2 Furnace equipped with dry (dew point below -68°C

[-90°F], moisture less than 3.5 ppm) nitrogen (less than

20 ppm oxygen) purge.

4.1.3 Temperature programmer capable of providing con-

trolled 10°C ± 0.1°C [18°F ± 0.18°F] per minute heating rate

from ambient to 800°C [1472°F].

4.2 Mass Measurement Capability The TGA shall be

capable of measuring mass to within 0.01 mg of actual value.

5 Procedure

5.1 Test Sample Preparation

The test samples should be

baked at 110°C ± 2°C [230.0°F ± 3.6°F] for 24 hr and placed

in a desiccator for cooling to room temperature (equilibration)

prior to testing. In standard lab conditions, the TGA test

should be started within 15 minutes of removing test sample

from the dessicator because samples may gain mass due to

moisture absorption.

5.2 Equipment Startup and Calibration (Follow Manu-

facturer’s Recommendations.)

5.2.1 Calibrate the balance to within ± 0.01 mg.

5.2.2 Calibrate the temperature sensor to within ± 1.0°C

[1.8°F].

5.2.3 Set the purge rate of 55 cc/min (0.9 mL/s). Run the

TGA gas purge for 30 minutes before inserting a sample. The

rate of flow of the gas in the cell will have a significant effect

on the calibration, therefore, the instrument must be calibrated

with the same flow rate as is used during the test. The tem-

perature sensor should be positioned so that it does not come

into contact with sample at any time. After the temperature

sensor has been correctly positioned, the instrument can be

calibrated. Neither the sensor position nor the flow rate should

be subsequently changed.

5.3 Heating Sample

5.3.1

Place the sample in the TGA and measure its mass.

5.3.2 Heat the sample at a rate of 10°C/min from ambient

(not to exceed 50°C) to 550°C.

3000 Lakeside Drive, Suite 309S

Bannockburn, IL 60015-1219

IPC-TM-650

TEST METHODS MANUAL

Number

2.4.24.6

Subject

Decomposition Temperature (T

) of Laminate

Material Using TGA

Date

4/06

Revision

Originating Task Group

Laminate/Prepreg Materials Subcommittee (3-11)

Material in this Test Methods Manual was voluntarily established by Technical Committees of 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 IPC.

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ASSOCIATION CONNECTING

ELECTRONICS INDUSTRIES

5.3.3 Record the temperature, T

(2%), at which the mass

of the sample is 2.0% less than its mass measured at 50°C.

5.3.4 Record the temperature, T

(5%), at which the mass

of the sample is 5.0% less than its mass measured at 50°C.

6 Results Report the following information:

a) The initial mass of the sample.

b) The room temperature and relative humidity under which

testing was conducted.

c) The thermal decomposition temperature, T

(2%).

d) The thermal decomposition temperature, T

(5%).

7 References

IPC-TM-650

Method 2.3.40, Thermal Stability

ASTM D-3850 Standard Test Method for Rapid Thermal

Degradation of Solid Electrical Insulating Materials by Thermo-

gravimetric Analysis

IPC-TM-650

Number

2.4.24.6

Subject

Decomposition Temperature (T

) of Laminate Material Using TGA

Date

4/06

Revision

Page2of2

1 Scope This test method is designed to determine the

glass transition temperature of dielectric materials used in

printed boards by differential scanning calorimetry (DSC). It is

suitable for prepreg, metallic clad or unclad laminate, and

printed boards. It also provides a determination of relative

degree of cure, or Cure Factor, for some types of materials.

2 Applicable Documents None

3 Test Specimens

3.1 Size and Configuration

The specimen shall be a

solid piece weighing between 10 to 40 mg. For very thin

materials, multiple pieces may be used to achieve the speci-

fied weight. The specimen shall be of a size and configuration

that fits within the sample pan of the DSC equipment. See 6.1

regarding use of a powdered specimen.

3.2 Quantity and Sampling The sampling shall be ran-

domly taken from the material in question, and, unless other-

wise specified, one specimen shall be tested, to be taken

from the material in question.

4 Equipment/Apparatus

4.1

Differential scanning calorimeter capable of measuring

and recording heat capacity of the applicable material.

4.2 Nitrogen gas supplied at a constant rate, suitable for

purging and calibrating the DSC cell.

4.3 Equipment suitable for specimen preparation in accor-

dance with 3.1, such as a punch press.

4.4 Standard aluminum sample pans and lids and crimping

press.

4.5 Air circulating oven capable of maintaining 105±2°C

[221 ± 3.6 °F].

4.6 Desiccator or drying cabinet capable of maintaining an

atmosphere less than 30% RH at 23 ° C [73.4 °F].

5 Procedure

5.1 Specimen Preparation

5.1.1

Metallic clad laminates and printed boards shall be

tested with metallic cladding left in place whenever possible.

5.1.2 For all laminates and printed boards, the sample shall

be preconditioned by baking for 2 ± 0.25 hours at 105 ± 2 °C

[221 ± 3.6 °F], then cooled to room temperature in a desicca-

tor or drying cabinet for at least 1/2 hour prior to testing.

5.1.3 The specimen shall be prepared from the baked

sample in accordance with 3.1. Edges shall be smoothed

and burrs removed by light sanding, or equivalent, to achieve

proper thermal conduction. Use care to minimize stress or

heating of the specimen.

5.1.4 Place the specimen in a standard aluminum sample

pan with an aluminum lid. Use of a lid and crimping is optional.

For referee purposes, a cover lid crimped onto the sample

pan shall be used. If the specimen is a powder, the pan shall

be covered with a lid and crimped shut.

5.1.5 For referee purposes, a suitable reference shall be

prepared by adding an equivalent weight of aluminum lids to

the reference pan to match the weight of the sample. For

example, if the sample weight is 8 mg, enough lids should be

added to the reference pan to weigh 8 mg.

5.2 Test

5.2.1

Follow start up and operating procedures in accor-

dance with instructions supplied by the test equipment

manufacturer.

5.2.2 Conditioning Pre-Scan:

5.2.2.1 The point of the pre-scan is to erase previous ther-

mal history and the effects on morphology of the sample.

3000 Lakeside Drive, Suite 105N

Bannockburn, IL 60015-1249

IPC-TM-650

TEST METHODS MANUAL

Number

2.4.25

Subject

Glass Transition Temperature and Cure Factor by

DSC

Date

11/17

Revision

Originating Task Group

Laminate/Prepreg Materials Subcommittee (3-11)

Material in this Test Methods Manual was voluntarily established by Technical Committees of 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 IPC.

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