Plastics — Instrumented micro-indentation test for hardness measurement

This document specifies a hardness test method for plastics using instrumented indentation in the micro scale with one clearly defined test condition to ensure reproducibility and comparability of test results. The test method is selectively suitable for use with the following materials: — moulding, extrusion and cast thermoplastic materials; rigid and semi-rigid thermoplastics sheets; — rigid and semi-rigid thermosetting moulding materials; thermosetting sheets. This test method could also be utilized for nanometric filled system, considering the fillers are distributed uniformly in the polymer matrix. This test method allows dumbbell type specimen, strip type specimen, platens and specimen cut from any finished parts or products. This test method is useful for quality control, material selection, and screening of new formulations. NOTE This document does not aim to describe all scientific or technical aspects of microhardness testing on plastics in general.

Plastiques — Essai instrumenté de micro-indentation pour le mesurage de la dureté

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Status
Published
Publication Date
31-Mar-2019
Current Stage
9060 - Close of review
Due Date
02-Sep-2022
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ISO/TS 19278:2019 - Plastics -- Instrumented micro-indentation test for hardness measurement
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TECHNICAL ISO/TS
SPECIFICATION 19278
First edition
2019-04
Plastics — Instrumented micro-
indentation test for hardness
measurement
Plastiques — Essai instrumenté de micro-indentation pour le
mesurage de la dureté
Reference number
ISO/TS 19278:2019(E)
ISO 2019
---------------------- Page: 1 ----------------------
ISO/TS 19278:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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ii © ISO 2019 – All rights reserved
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ISO/TS 19278:2019(E)
Contents Page

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

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

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

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

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

4 Principle ........................................................................................................................................................................................................................ 2

5 Apparatus ..................................................................................................................................................................................................................... 2

5.1 General ........................................................................................................................................................................................................... 2

5.2 Indenter ......... ................................................................................................................................................................................................ 2

5.3 Displacement measurement device ...................................................................................................................................... 3

5.4 Loading unit and force measuring device ........................................................................................................................ 3

5.5 Periodic checks of test apparatus ........................................................................................................................................... 3

6 Test specimen .......................................................................................................................................................................................................... 3

7 Conditioning .............................................................................................................................................................................................................. 3

8 Procedure..................................................................................................................................................................................................................... 4

9 Number of test specimens .......................................................................................................................................................................... 5

10 Expression of results ........................................................................................................................................................................................ 5

11 Test report ................................................................................................................................................................................................................... 6

Annex A (informative) Precision statement .................................................................................................................................................. 8

Bibliography ................................................................................................................................................................................................................................ 9

© ISO 2019 – All rights reserved iii
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ISO/TS 19278:2019(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 2,

Mechanical behaviour.

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 2019 – All rights reserved
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ISO/TS 19278:2019(E)
Introduction

This document was developed in response to a demand to define an instrumented indentation hardness

test method in the micro scale for quality control of plastics materials and material selection. The test

conditions are defined to ensure reproducibility and comparability of test results.

The Rockwell hardness method (ISO 2039-2) and the ball indentation method (ISO 2039-1) have been

formulated for determining the indentation hardness of plastics. These test methods use different

scales depending on the hardness of the material and it is difficult to compare hardness values of

materials when they are measured on different scales.

The Vickers hardness test method (ISO 6507-1), used for metallic materials, is a method that does not

use different scales. The Vickers hardness is calculated as the ratio of indentation load and the residual

area of contact of the indenter. However, when this method is applied to plastics materials, it is difficult

to measure the residual area of contact of the indenter because the edge of the indentation cannot be

specified.

The instrumented indentation hardness test method (ISO 14577-1) is intended for hardness

measurement in the range from nano-indentation to macro-indentation. In this method, since the

contact area of the indenter is directly determined from the indentation depth, the above-mentioned

problem is solved. It is therefore possible to determine the indentation hardness of the plastic materials.

In this document, in order to avoid errors due to detection of initial contact, a test force that can result in

sufficient indentation depth within the range of micro-indentation is specified. For example, the range

of indentation depth under this condition, which is from 10 μm to 50 μm in the case of the four types of

materials described in this document, also corresponds to the dimension (scale) of the diagonal length

range of 0,020 mm to 1,400 mm specified by the Vickers hardness test method (ISO 6507-1). In this

document, the measurement time of a single condition is specified similarly to the Rockwell hardness

method (ISO 2039-2).
© ISO 2019 – All rights reserved v
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TECHNICAL SPECIFICATION ISO/TS 19278:2019(E)
Plastics — Instrumented micro-indentation test for
hardness measurement
1 Scope

This document specifies a hardness test method for plastics using instrumented indentation in the

micro scale with one clearly defined test condition to ensure reproducibility and comparability of test

results.
The test method is selectively suitable for use with the following materials:

— moulding, extrusion and cast thermoplastic materials; rigid and semi-rigid thermoplastics sheets;

— rigid and semi-rigid thermosetting moulding materials; thermosetting sheets.

This test method could also be utilized for nanometric filled system, considering the fillers are

distributed uniformly in the polymer matrix.

This test method allows dumbbell type specimen, strip type specimen, platens and specimen cut from

any finished parts or products.

This test method is useful for quality control, material selection, and screening of new formulations.

NOTE This document does not aim to describe all scientific or technical aspects of microhardness testing on

plastics in general.
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 291, Plastics — Standard atmospheres for conditioning and testing

ISO 2602, Statistical interpretation of test results — Estimation of the mean — Confidence interval

ISO 4287, Geometrical Product Specifications (GPS) — Surface texture: Profile method — Terms, definitions

and surface texture parameters

ISO 14577-1, Metallic materials — Instrumented indentation test for hardness and materials parameters —

Part 1: Test method
3 Terms and definitions
No terms and definitions are listed in this document.

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/
© ISO 2019 – All rights reserved 1
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ISO/TS 19278:2019(E)
4 Principle

The original Berkovich indenter is forced under a specified load into the surface of the test specimen.

The depth of indentation is measured under load. Indentation hardness H is calculated from F and

IT max
A (see 10.1).
5 Apparatus
5.1 General

The testing apparatus comprises of a rigid frame, a stage, a test specimen holder, an indenter, a loading

unit, and a displacement measuring device. The apparatus is required to measure and record the applied

force, the indentation depth, and the time throughout the testing cycle. The apparatus shall have the

capability of compensating for the machine compliance and of utilizing the appropriate indenter area

function in accordance with ISO 14577-1. The general design is as shown in Figure 1.

Key
1 machine frame 5 stage
2 indenter 6 test specimen holder
3 loading unit 7 test specimen
4 displacement measuring device
F test force
Figure 1 — Example of testing apparatus
5.2 Indenter

The testing apparatus shall be equipped with an original Berkovich indenter in accordance with

ISO 14577-1. The indenter should be calibrated according to ISO 14577-2.
2 © ISO 2019 – All rights reserved
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ISO/TS 19278
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