Thermosetting resin and UV curable resin -- Determination of shrinkage by continuous measurement method

This document specifies the continuous measurement method of shrinkage for thermosetting resin and/or UV curable resin.

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Publication Date
21-Apr-2021
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5060 - Close of voting Proof returned by Secretariat
Start Date
25-Mar-2021
Completion Date
25-Mar-2021
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ISO 4216:2021 - Thermosetting resin and UV curable resin -- Determination of shrinkage by continuous measurement method
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INTERNATIONAL ISO
STANDARD 4216
First edition
2021-04
Thermosetting resin and UV curable
resin — Determination of shrinkage
by continuous measurement method
Reference number
ISO 4216:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 4216:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 4216:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Test methods and test conditions ....................................................................................................................................................... 3

5.1 Test methods ............................................................................................................................................................................................. 3

5.2 Test conditions ........................................................................................................................................................................................ 3

6 Number of measurements .......................................................................................................................................................................... 3

7 Apparatus ..................................................................................................................................................................................................................... 4

7.1 Apparatus configuration ................................................................................................................................................................. 4

7.2 Sample container .................................................................................................................................................................................. 5

7.3 Displacement gauge (thickness meter) ............................................................................................................................. 6

7.4 UV irradiation device ......................................................................................................................................................................... 6

7.5 Heating/cooling device .................................................................................................................................................................... 6

7.6 Data processing unit ......... .................................................................................................................................................................. 6

8 Curing method ........................................................................................................................................................................................................ 6

8.1 UV curable resin curing method .............................................................................................................................................. 6

8.2 Thermosetting resin curing method .................................................................................................................................... 6

9 Measurement procedure .............................................................................................................................................................................. 6

10 Expression of results ........................................................................................................................................................................................ 7

10.1 Volumetric shrinkage ........................................................................................................................................................................ 7

10.2 Curing shrinkage ................................................................................................................................................................................... 7

11 Test report ................................................................................................................................................................................................................... 8

Annex A (informative) Influencing factors on measurement ..................................................................................................... 9

Annex B (informative) Examples of measurement result ............................................................................................................10

Annex C (informative) Example of measurement report .............................................................................................................13

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 4216:2021(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12,

Thermosetting materials.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2021 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 4216:2021(E)
Introduction

The use of resin first requires curing it under specific conditions that vary depending on the product

specification. During this curing process, chemical reactions occur and volatiles evaporate, and so the

resin shrinks. This can cause defects, strength reduction, and the deformation of the finished parts or

products, especially in high precision required applications.

The conventional method which measures the shrinkage of resin based on specific gravity requires

long measurement time and an amount of resin about a few cubic centimetres. This sample size is

larger than what is actually used in many applications such as the epoxy encapsulation compounds

for integrated circuits, resin coating or adhesive for electronic devices. In order to improve the quality

control and further promote the technical advancement of high precision production, a convenient and

high accuracy method for determining the shrinkage of resin is essential.

A totally new measurement method has been developed to meet this demand, allowing to measure

curing shrinkage continuously with just a trace amount of resin. Moreover, since measurements are

taken continuously, the curing behaviour of resin such as thermal expansion and thermal contraction

are also observed. This measurement method is described in this document.
© ISO 2021 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 4216:2021(E)
Thermosetting resin and UV curable resin — Determination
of shrinkage by continuous measurement method

SAFETY STATEMENT — Persons using this document should be familiar with normal laboratory

practice, if applicable. This document does not purport to address all of the safety concerns, if

any, associated with its use. It is the responsibility of the user to establish appropriate safety

and health practices.
1 Scope

This document specifies the continuous measurement method of shrinkage for thermosetting resin

and/or UV curable resin.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 472, Plastics — Vocabulary
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 472 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
UV curable resin
resin which is cured by receiving energy from UV rays
3.2
thermosetting resin
resin which is cured by receiving energy from heat
3.3
curing condition
UV irradiation and/or heating condition for curing resin
3.4
curing shrinkage

ratio of the change in resin volume due to curing process to the resin volume before curing

Note 1 to entry: Percentage of shrinkage due to curing of resin.
4 Principle

Cure the resin inside a sample container and continuously measure the changes of sample thickness.

Since the horizontal cross-sectional area of resin sample remains constant due to the sidewalls of

the sample container, the changes in sample volume are proportional to the changes in the sample

© ISO 2021 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO 4216:2021(E)

thickness. Therefore, shrinkage of resin is calculated from the changes in sample thickness, as shown in

Formula (1).
A = ( T – T ) / T × 100 (1)
1 2 1
Where
A is the shrinkage, in %;
T is the initial sample thickness;
T is the sample thickness at an arbitrary time.

In addition to the determination of the curing shrinkage, this continuous measurement technique

also allows to see the volumetric changing behaviour of a resin at the time it is being irradiated by UV,

heated, or cooled during the curing process.

NOTE 1 Typically, upon irradiation by UV rays, UV curable resins expand immediately then contract as curing

proceeds (see Figure 1). However, some types of UV curable resin exhibit fast reactions wherein shrinkage starts

immediately right after irradiation (see Figure B.1).

NOTE 2 When a thermosetting resin undergoes heating, thermal expansion occurs due to the increase in the

resin temperature. This expansion continues as the temperature rises. When the curing temperature is reached,

the curing begins and the resin starts to contract. This shrinkage continues until the resin is fully cured and

returned to room temperature (see Figure 2).
Key
X time (s)
Y volumetric shrinkage (%)
A irradiation start point = curing start point
B shrinkage start point
C curing finish point
D shrinkage finish point
E curing shrinkage
F maximum shrinkage
Figure 1 — Curing behaviour of UV curable resin
2 © ISO 2021 – All rights reserved
---------------------- Page: 7 ----------------------
ISO 4216:2021(E)
Key
X time (min) a, d room temperature
Y volumetric shrinkage (%) b, c curing temperature
temperature(°C)
A start heating point
B start curing point
C curing finish point
D shrinkage finish point
E curing shrinkage
F shrinkage by cooling
G shrinkage by reaction
H maximum shrinkage
Figure 2 — Curing behaviour of thermosetting resin
5 Test methods and test conditions
5.1 Test methods

The test methods are classified according to the curing conditions applied to the resin. There are

three different types of curing condition: UV curing, thermal curing, and a combination of UV and

thermal curing.
5.2 Test conditions

Conduct measurements in the standard laboratory atmosphere of 23 °C ± 2 °C (73,4 °F ± 3,6 °F) and

50 % ± 5 % relative humidity, unless otherwise specified in the experiment conditions.

6 Number of measurements
Three or more samples shall be tested for each curing condition.
© ISO 2021 – All rights reserved 3
---------------------- Page: 8 ----------------------
ISO 4216:2021(E)
7 Apparatus
7.1 Apparatus configuration

An apparatus for measuring the curing shrinkage of resin by this method is a system that consists of

different units. Primarily, it includes a sample container, displacement gauge, UV irradiation device,

heating/cooling device, etc. Figure 3 shows an example of an apparatus configuration compatible with

a UV curable resin, and Figure 4 shows an example of an apparatus configuration corresponding to a

thermosetting resin.
Key
1 displacement gauge
2 sample
3 sample container
4 measuring stage
5 UV irradiation device
6 UV beams
Figure 3 — Example of an apparatus applied for UV curable resin
4 © ISO 2021 – All rights reserved
---------------------- Page: 9 ----------------------
ISO 4216:2021(E)
Key
1 displacement gauge
2 sample
3 sample container
4 measuring stage
5 heating/cooling device
Figure 4 — Example of an apparatus applied for thermosetting resin
7.2 Sample container

A sample container of accurately known volume and dimensions shall be used. To ensure an accurate

measurement, container material should be used which does not cause either the detachment of resin

from the bottom after curing or absorb the sample via the wall surfaces. Moreover, in order to calculate

easily the container capacity/volume, the sample container should have a smooth bottom surface and

cylindrical sh
...

INTERNATIONAL ISO
STANDARD 4216
First edition
Thermosetting resin and UV curable
resin — Determination of shrinkage
by continuous measurement method
PROOF/ÉPREUVE
Reference number
ISO 4216:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 4216:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii PROOF/ÉPREUVE © ISO 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 4216:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Test methods and test conditions ....................................................................................................................................................... 3

5.1 Test methods ............................................................................................................................................................................................. 3

5.2 Test conditions ........................................................................................................................................................................................ 3

6 Number of measurements .......................................................................................................................................................................... 3

7 Apparatus ..................................................................................................................................................................................................................... 4

7.1 Apparatus configuration ................................................................................................................................................................. 4

7.2 Sample container .................................................................................................................................................................................. 5

7.3 Displacement gauge (thickness meter) ............................................................................................................................. 6

7.4 UV irradiation device ......................................................................................................................................................................... 6

7.5 Heating/cooling device .................................................................................................................................................................... 6

7.6 Data processing unit ......... .................................................................................................................................................................. 6

8 Curing method ........................................................................................................................................................................................................ 6

8.1 UV curable resin curing method .............................................................................................................................................. 6

8.2 Thermosetting resin curing method .................................................................................................................................... 6

9 Measurement procedure .............................................................................................................................................................................. 6

10 Expression of results ........................................................................................................................................................................................ 7

10.1 Volumetric shrinkage ........................................................................................................................................................................ 7

10.2 Curing shrinkage ................................................................................................................................................................................... 7

11 Test report ................................................................................................................................................................................................................... 8

Annex A (informative) Influencing factors on measurement ..................................................................................................... 9

Annex B (informative) Examples of measurement result ............................................................................................................10

Annex C (informative) Example of measurement report .............................................................................................................13

© ISO 2021 – All rights reserved PROOF/ÉPREUVE iii
---------------------- Page: 3 ----------------------
ISO 4216:2021(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12,

Thermosetting materials.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv PROOF/ÉPREUVE © ISO 2021 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 4216:2021(E)
Introduction

The use of resin first requires curing it under specific conditions that vary depending on the product

specification. During this curing process, chemical reactions occur and volatiles evaporate, and so the

resin shrinks. This can cause defects, strength reduction, and the deformation of the finished parts or

products, especially in high precision required applications.

The conventional method which measures the shrinkage of resin based on specific gravity requires

long measurement time and an amount of resin about a few cubic centimetres. This sample size is

larger than what is actually used in many applications such as the epoxy encapsulation compounds

for integrated circuits, resin coating or adhesive for electronic devices. In order to improve the quality

control and further promote the technical advancement of high precision production, a convenient and

high accuracy method for determining the shrinkage of resin is essential.

A totally new measurement method has been developed to meet this demand, allowing to measure

curing shrinkage continuously with just a trace amount of resin. Moreover, since measurements are

taken continuously, the curing behaviour of resin such as thermal expansion and thermal contraction

are also observed. This measurement method is described in this document.
© ISO 2021 – All rights reserved PROOF/ÉPREUVE v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 4216:2021(E)
Thermosetting resin and UV curable resin — Determination
of shrinkage by continuous measurement method

SAFETY STATEMENT — Persons using this document should be familiar with normal laboratory

practice, if applicable. This document does not purport to address all of the safety concerns, if

any, associated with its use. It is the responsibility of the user to establish appropriate safety

and health practices.
1 Scope

This document specifies the continuous measurement method of shrinkage for thermosetting resin

and/or UV curable resin.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 472, Plastics — Vocabulary
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 472 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
UV curable resin
resin which is cured by receiving energy from UV rays
3.2
thermosetting resin
resin which is cured by receiving energy from heat
3.3
curing condition
UV irradiation and/or heating condition for curing resin
3.4
curing shrinkage

ratio of the change in resin volume due to curing process to the resin volume before curing

Note 1 to entry: Percentage of shrinkage due to curing of resin.
4 Principle

Cure the resin inside a sample container and continuously measure the changes of sample thickness.

Since the horizontal cross-sectional area of resin sample remains constant due to the sidewalls of

the sample container, the changes in sample volume are proportional to the changes in the sample

© ISO 2021 – All rights reserved PROOF/ÉPREUVE 1
---------------------- Page: 6 ----------------------
ISO 4216:2021(E)

thickness. Therefore, shrinkage of resin is calculated from the changes in sample thickness, as shown in

Formula (1).
A = ( T – T ) / T × 100 (1)
1 2 1
Where
A is the shrinkage, in %;
T is the initial sample thickness;
T is the sample thickness at an arbitrary time.

In addition to the determination of the curing shrinkage, this continuous measurement technique

also allows to see the volumetric changing behaviour of a resin at the time it is being irradiated by UV,

heated, or cooled during the curing process.

NOTE 1 Typically, upon irradiation by UV rays, UV curable resins expand immediately then contract as curing

proceeds (see Figure 1). However, some types of UV curable resin exhibit fast reactions wherein shrinkage starts

immediately right after irradiation (see Figure B.1).

NOTE 2 When a thermosetting resin undergoes heating, thermal expansion occurs due to the increase in the

resin temperature. This expansion continues as the temperature rises. When the curing temperature is reached,

the curing begins and the resin starts to contract. This shrinkage continues until the resin is fully cured and

returned to room temperature (see Figure 2).
Key
X time (s)
Y volumetric shrinkage (%)
A irradiation start point = curing start point
B shrinkage start point
C curing finish point
D shrinkage finish point
E curing shrinkage
F maximum shrinkage
Figure 1 — Curing behaviour of UV curable resin
2 PROOF/ÉPREUVE © ISO 2021 – All rights reserved
---------------------- Page: 7 ----------------------
ISO 4216:2021(E)
Key
X time (min) a, d room temperature
Y volumetric shrinkage (%) b, c curing temperature
temperature(°C)
A start heating point
B start curing point
C curing finish point
D shrinkage finish point
E curing shrinkage
F shrinkage by cooling
G shrinkage by reaction
H maximum shrinkage
Figure 2 — Curing behaviour of thermosetting resin
5 Test methods and test conditions
5.1 Test methods

The test methods are classified according to the curing conditions applied to the resin. There are

three different types of curing condition: UV curing, thermal curing, and a combination of UV and

thermal curing.
5.2 Test conditions

Conduct measurements in the standard laboratory atmosphere of 23 °C ± 2 °C (73,4 °F ± 3,6 °F) and

50 % ± 5 % relative humidity, unless otherwise specified in the experiment conditions.

6 Number of measurements
Three or more samples shall be tested for each curing condition.
© ISO 2021 – All rights reserved PROOF/ÉPREUVE 3
---------------------- Page: 8 ----------------------
ISO 4216:2021(E)
7 Apparatus
7.1 Apparatus configuration

An apparatus for measuring the curing shrinkage of resin by this method is a system that consists of

different units. Primarily, it includes a sample container, displacement gauge, UV irradiation device,

heating/cooling device, etc. Figure 3 shows an example of an apparatus configuration compatible with

a UV curable resin, and Figure 4 shows an example of an apparatus configuration corresponding to a

thermosetting resin.
Key
1 displacement gauge
2 sample
3 sample container
4 measuring stage
5 UV irradiation device
6 UV beams
Figure 3 — Example of an apparatus applied for UV curable resin
4 PROOF/ÉPREUVE © ISO 2021 – All rights reserved
---------------------- Page: 9 ----------------------
ISO 4216:2021(E)
Key
1 displacement gauge
2 sample
3 sample container
4 measuring stage
5 heating/cooling device
Figure 4 — Example of an apparatus applied for thermosetting resin
7.2 Sample container

A sample container of accurately known volume and dimensions shall be used. To ensure an accurate

measurement, container material should be used which does not cause either the detachment of resin

from the bottom after curing or absorb the sample via the wall surfaces. Moreover, in order to calculate

easily the container capacity/volume, the sample container should have a smooth bottom surface and

cylindrical shape.
a) Sectional view
b) Top
...

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