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SEMI G15-93 © SEMI 198 2, 1996 2 Figure 1 8.2 Determ ine the onset of melting a n d refer to the manual for the tem perat ure correction m ethod. NOTE 2: There are oth er standard reference materials with higher m elting…

SEMI G15-93 © SEMI 1982, 19961

SEMI G15-93

STANDARD TEST METHOD FOR DIFFERENTIAL SCANNING

CALORIMETRY OF MOLDING COMPOUNDS

1 Preface

1.1 Scope — This document describes procedures for

evaluating epoxy molding compounds by differential

scanning calorimetry (DSC).

1.2 Units — This test method uses SI units.

2 Applicable Documents

2.1 Reference Documents

2.1.1 ASTM Specifications

ASTM E 793 — Test Method for Heats of Fusion and

Crystallization by Differential Scanning Calorimetry

ASTM E 967 — Practice for Temperature Calibration of

Differential Scanning Calorimeters and Differential

Thermal Analyzers

ASTM E 968 — Practice for Heat Flow Calibration of

Differential Scanning Calorimeters

2.2 Related Documents

2.2.1 ASTM Specifications

ASTM E 473 — Standard Definitions of Terms Relating

to Thermal Analyses

ASTM E 1269 — Test Method for Determining Specific

Heat by Differential Scanning Calorimetry

3 Significance

3.1 DSC provides a rapid method at incoming

inspection for evaluating molding compounds for

consistency in subsequent molding processes.

4 Interferences

4.1 Very small quantities of material are used in the

test. Lack of homogeneity may cause variable results.

4.2 Gas Purge — See Section 5.

4.3 Sample Pans — See Section 5.

5 Equipment

5.1 Differential Scanning Calorimeter — Capable of

heating a sample from room temperature to 300°C with

a controlled heating rate.

1 American Society for Testing and Materials, 100 Barr Harbor

Drive, West Conshohoken, PA 19428-2959

NOTE 1: Gas Purge Considerations — A reactive gas purge

affects the material under test. A gas must be chosen that

reflects the molding conditions normally used for that

material (i.e., air or nitrogen).

5.2 Sampling Pans for DSC Cell — (Aluminum with

crimping or hermetically sealed.) The pans must not be

reactive to the sample under test.

5.3 Process Controller — Capable of collecting,

calculating, and plotting the data resulting from the

calorimeter.

5.4 Analytical Balance — Accuracy 0.001 mg.

5.5 Tweezers and Microspatula

6 Sampling

6.1 When the method is used to evaluate incoming

molding materials, the sampling plan shall be agreed

between supplier and customer.

6.2 Powdered or granular molding compounds shall be

thoroughly mixed before sampling. If the compound is

supplied in a preform, a small section may be cut off

the preform with a blade.

7 Preparation of Samples

7.1 Protect samples from moisture absorption while

awaiting test.

8 Equipment Setup and Cal ibration

8.1 Temperature Calibration — (Refer to ASTM E

967.)

8.1.1 Follow the manufacturer's operating manual to

set up and run a calibration curve using indium

(Melting Point 156.6°C) (see Figure 1).

SEMI G15-93 © SEMI 1982, 1996 2

Figure 1

8.2 Determine the onset of melting and refer to the

manual for the temperature correction method.

NOTE 2: There are other standard reference materials with

higher melting points (see Table 1). Choose the standard

which best matches the range of interest for the material under

test.

Table 1

Reference Material Melting Point (°C)

Indium 156.6

Tin 232.0

Zinc 419.6

8.2.1 Indium is also used to calibrate the Heat of

Fusion for the DSC cell. Table 2 also lists the Standard

Heat of Fusion for alternate materials that may be used.

Table 2

Reference Material Heat of Fusion (J/g)

Mercury 11.44

Indium 28.42

Lead 23.16

Tin 59.23

Zinc 112.0

8.2.2 An area calculation of the indium melt provides

the Heat of Fusion for DSC cell (see Figure 1).

8.2.3 Refer to the operating manual to obtain the cell

constant and its correction.

9 Procedure

9.1 Sample Size — 2.000 to 12.000 mg may be used.

8.000 mg is commonly used. A small design of

experiments exercise may be used to obtain the

optimum sample size for the molding compound under

test. Different compound chemistries may have an

effect on the results if the sample size is not carefully

chosen.

Place the sample in the sample pan.

9.2 Use an empty sample pan with its cover as a

reference.

9.3 Carefully place the sample and reference pans onto

their respective thermal sensors in the DSC cell. Seal

the cell according to the manufacturer's instructions.

9.4 Set the heating rate to the optimum conditions

determined for that instrument and the specific material

under test. This rate will normally be between 5°C and

25°C per minute.

9.5 Activate the test sequence, and heat the sample

from room-temperature to 300°C in order to obtain the

DSC curve.

9.6 At the end of the run, remove the sample, and

allow the DSC cell to cool to room-temperature in

preparation for the next sample.

10 Results Report

10.1 The results report shall contain the following

items:

10.1.1 Sample and equipment details

Molding material name/number

Sample weight

Equipment used

Heating rate

Calibration constant

Any pertinent information regarding material or

equipment

10.1.2 Scan Results — The DSC curve shall indicate

the following:

Maximum peak exotherm — units °C

Exotherm onset — units °C

Exotherm — units joules/gram

NOTE 3: The total exotherm is determined by an area

calculation of the exotherm profile using a computer drawn

baseline.

11 Accuracy and Precision (s ee ASTM E 968)

11.1 Repeatability — Single Analyst — The percent

RSD over multiple days was determined to be 4.2%.

11.2 Reproducibility — Multilaboratory — The

percent RSD was determined to be 8.2%.

12 Alternate Procedures

12.1 Thermal Kinetic Modeling

12.2 Isothermal Differential Scanning Calorimetry —

There is a current lack of interlaboratory correlation to

recommend this method.

NOTE 4: Manufacturers’ literature may be used to obtain

information on these methods.

NOTICE: These standards do not purport to address

safety issues, if any, associated with their use. It is the

responsibility of the user of these standards to establish

appropriate safety and health practices and determine

the applicability of regulatory limitations prior to use.

SEMI makes no warranties or representations as to the

suitability of the standards set forth herein for any

particular application. The determination of the

suitability of the standard is solely the responsibility of

the user. Users are cautioned to refer to manufacturer’s

instructions, product labels, product data sheets, and

other relevant literature respecting any materials

mentioned herein. These standards are subject to

change without notice.

The user’s attention is called to the possibility that

compliance with this standard may require use of

copyrighted material or of an invention covered by

patent rights. By publication of this standard, SEMI

takes no position respecting the validity of any patent

rights or copyrights asserted in connection with any

item mentioned in this standard. Users of this standard

are expressly advised that determination of any such

patent rights or copyrights, and the risk of infringement

of such rights, are entirely their own responsibility.

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