ISO/DIS 4216
(Main)Thermosetting resin and UV curable resin -- Determination of shrinkage by continuous measurement method
Thermosetting resin and UV curable resin -- Determination of shrinkage by continuous measurement method
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DRAFT INTERNATIONAL STANDARD
ISO/DIS 4216
ISO/TC 61/SC 12 Secretariat: JISC
Voting begins on: Voting terminates on:
2020-10-28 2021-01-20
Thermosetting resin and UV curable resin — Determination
of shrinkage by continuous measurement method
ICS: 83.080.10
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ISO/DIS 4216:2020(E)
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PROVIDE SUPPORTING DOCUMENTATION. ISO 2020
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ISO/DIS 4216:2020(E)
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ii © ISO 2020 – All rights reserved
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ISO/DIS 4216:2020(E)
Contents Page
Foreword ........................................................................................................................................................................................................................................iv
Introduction ..................................................................................................................................................................................................................................v
1 Scope ................................................................................................................................................................................................................................. 1
2 Normative references ...................................................................................................................................................................................... 1
3 Terms and definitions ..................................................................................................................................................................................... 1
4 Principle ........................................................................................................................................................................................................................ 2
5 Test methods and test conditions ....................................................................................................................................................... 3
5.1 Test methods ............................................................................................................................................................................................. 3
5.2 Test conditions ........................................................................................................................................................................................ 3
6 Number of measurements .......................................................................................................................................................................... 3
7 Apparatus ..................................................................................................................................................................................................................... 3
7.1 Apparatus configuration ................................................................................................................................................................. 3
7.2 Sample container .................................................................................................................................................................................. 4
7.3 Displacement gauge (thickness meter) ............................................................................................................................. 5
7.4 UV irradiation device ......................................................................................................................................................................... 5
7.5 Heating/cooling device .................................................................................................................................................................... 5
7.6 Data processing unit ......... .................................................................................................................................................................. 5
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 ........................................................................................................................................................................................ 6
11 Test report ................................................................................................................................................................................................................... 8
Annex A (informative) Influencing factors on measurement ..................................................................................................... 9
Annex B (informative) Examples of measurement result ............................................................................................................10
Annex C (informative) Description of measurement report .....................................................................................................12
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ISO/DIS 4216:2020(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
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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
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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 [or Project 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 2020 – All rights reserved
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ISO/DIS 4216:2020(E)
Introduction
The use of a 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 may 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 2020 – All rights reserved v
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DRAFT INTERNATIONAL STANDARD ISO/DIS 4216:2020(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 and to ensure compliance with any regulatory requirements.1 Scope
This document specifies the continuous measurement method of shrinkage for thermosetting resin
and/or UV curable resin.2 Normative references
The following referenced documents, in whole or in part, are normatively referenced in this document
and are indispensable for the application 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
ISO 291, Plastics — Standard atmospheres for conditioning and testing
3 Terms and definitions
For the purposes of this document, the following terms and definitions 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
the UV irradiation and/or heating condition for curing resin
3.4
curing shrinkage
the ratio of the change in resin volume due to curing process to the resin volume before curing
(percentage of shrinkage due to curing of resin)© ISO 2020 – All rights reserved 1
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ISO/DIS 4216:2020(E)
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
thickness. Therefore, shrinkage of resin is calculated from the changes in sample thickness.
initialsamplethickness−samplethicknessatanabittrarytimeShrinkage% = ×100
initialsamplethickness
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 (Figure 1). However, some types of UV curable resin exhibit fast reactions wherein shrinkage starts
immediately right after irradiation (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,
curing begins and the resin then starts to contract. This shrinkage continues until the resin is fully cured and
returned to room temperature (Figure 2).Key
A irradiation start point = Curing start point
B shrinkage start point
C curing finish point
D shrinkage finish point
Figure 1 — Curing behaviour of UV curable resin
2 © ISO 2020 – All rights reserved
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ISO/DIS 4216:2020(E)
Key
A start heating point Room temperature: a, d
B start curing point Curing temperature: b, c
C curing finish point
D shrinkage finish point
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 ± 2 °C (73.4 ± 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.
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.© ISO 2020 – All rights reserved 3
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ISO/DIS 4216:2020(E)
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
...
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