SIST EN ISO 19628:2021
(Main)Fine ceramics (advanced ceramics, advanced technical ceramics) - Thermophysical properties of ceramic composites - Determination of specific heat capacity (ISO 19628:2017)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Thermophysical properties of ceramic composites - Determination of specific heat capacity (ISO 19628:2017)
ISO 19628:2017 describes two methods for the determination of the specific heat capacity of ceramic matrix composites with continuous reinforcements (1D, 2D, 3D).
Unidirectional (1D), bi-directional (2D) and tridirectional (XD, with 2 < x ≤ 3).
The two methods are:
- method A: drop calorimetry;
- method B: differential scanning calorimetry.
They are applicable from ambient temperature up to a maximum temperature, depending on the method: method A can be used up to 2 250 K, while method B is limited to 1 900 K.
NOTE Method A is limited to the determination of an average value of the specific heat capacity over a given temperature range and can give a larger spread of results.
Hochleistungskeramik - Thermophysikalische Eigenschaften von keramischen Verbundwerkstoffen - Bestimmung der spezifischen Wärmekapazität (ISO 19628:2017)
Dieses Dokument legt zwei Verfahren zur Bestimmung der spezifischen Wärmekapazität von keramischen Verbundwerkstoffen mit Endlos-Faserverstärkung (1D, 2D, 3D) fest.
Unidirektional (1D), bidirektional (2D) und tridirektional (XD, mit 2 < x <- 3).
Die beiden Verfahren sind:
- Verfahren A: Fallkalorimetrie;
- Verfahren B: dynamische Differenz-Kalorimetrie.
Die Verfahren sind von Umgebungstemperatur bis zu einer verfahrensabhängigen Höchsttemperatur anwendbar: Verfahren A kann bis 2 250 K angewendet werden, während Verfahren B auf Temperaturen bis 1 900 K beschränkt ist.
ANMERKUNG Verfahren A ist auf die Bestimmung einer mittleren spezifischen Wärmekapazität für einen vorgegebenen Temperaturbereich beschränkt und kann daher zu größeren Messwertstreuungen führen.
Céramiques techniques - Propriétés thermophysiques des composites céramiques - Détermination de la capacité thermique specifique (ISO 19628:2017)
L'ISO 19628:2017 décrit deux méthodes pour la détermination de la capacité thermique spécifique des composites à matrice céramique à renforts continus (1D, 2D, 3D).
Les matrices sont à renforts unidirectionnels (1D), bidirectionnels (2D) et tridirectionnels (XD, avec 2 < x ≤ 3).
Les deux méthodes sont:
- méthode A: calorimétrie à chute;
- méthode B: calorimétrie différentielle à balayage.
Elles sont applicables depuis la température ambiante jusqu'à une température maximale qui dépend de la méthode: la méthode A peut être utilisée jusqu'à 2 250 K, tandis que la méthode B est limitée à 1 900 K.
NOTE La méthode A se limite à la détermination d'une valeur moyenne de la capacité thermique spécifique dans un intervalle de température donné et peut conduire à une dispersion importante des résultats.
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Termofizikalne lastnosti keramičnih kompozitov - Ugotavljanje specifične toplotne kapacitete (ISO 19628:2017)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 19628:2021
01-maj-2021
Nadomešča:
SIST EN 1159-3:2004
SIST EN 1159-3:2004/AC:2007
SIST EN 1159-3:2004/AC:2008
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Termofizikalne
lastnosti keramičnih kompozitov - Ugotavljanje specifične toplotne kapacitete (ISO
19628:2017)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Thermophysical
properties of ceramic composites - Determination of specific heat capacity (ISO
19628:2017)
Hochleistungskeramik - Thermophysikalische Eigenschaften von keramischen
Verbundwerkstoffen - Bestimmung der spezifischen Wärmekapazität (ISO 19628:2017)
Céramiques techniques - Propriétés thermophysiques des composites céramiques -
Détermination de la capacité thermique specifique (ISO 19628:2017)
Ta slovenski standard je istoveten z: EN ISO 19628:2021
ICS:
81.060.30 Sodobna keramika Advanced ceramics
SIST EN ISO 19628:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 19628:2021
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SIST EN ISO 19628:2021
EN ISO 19628
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2021
EUROPÄISCHE NORM
ICS 81.060.30 Supersedes EN 1159-3:2003
English Version
Fine ceramics (advanced ceramics, advanced technical
ceramics) - Thermophysical properties of ceramic
composites - Determination of specific heat capacity (ISO
19628:2017)
Céramiques techniques - Propriétés thermophysiques Hochleistungskeramik - Thermophysikalische
des composites céramiques - Détermination de la Eigenschaften von keramischen Verbundwerkstoffen -
capacité thermique specifique (ISO 19628:2017) Bestimmung der spezifischen Wärmekapazität (ISO
19628:2017)
This European Standard was approved by CEN on 22 February 2021.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 19628:2021 E
worldwide for CEN national Members.
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SIST EN ISO 19628:2021
EN ISO 19628:2021 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 19628:2021
EN ISO 19628:2021 (E)
European foreword
The text of ISO 19628:2017 has been prepared by Technical Committee ISO/TC 206 "Fine ceramics” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 19628:2021
by Technical Committee CEN/TC 184 “Advanced technical ceramics” the secretariat of which is held by
DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by September 2021, and conflicting national standards
shall be withdrawn at the latest by September 2021.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 1159-3:2003.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO 19628:2017 has been approved by CEN as EN ISO 19628:2021 without any modification.
3
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SIST EN ISO 19628:2021
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SIST EN ISO 19628:2021
INTERNATIONAL ISO
STANDARD 19628
First edition
2017-04
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Thermophysical properties of ceramic
composites — Determination of
specific heat capacity
Céramiques techniques — Propriétés thermophysiques des composites
céramiques — Détermination de la capacité thermique specifique
Reference number
ISO 19628:2017(E)
©
ISO 2017
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SIST EN ISO 19628:2021
ISO 19628:2017(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2017, Published in Switzerland
All rights reserved. Unless otherwise specified, 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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2017 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 19628:2021
ISO 19628:2017(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Method A – drop calorimetry. 2
4.1 Principle . 2
4.2 Apparatus . 2
4.3 Standard reference materials . 2
4.4 Test specimens . 2
4.5 Calibration of calorimeter . 3
4.5.1 General. 3
4.5.2 Electrical calibration . 3
4.5.3 Calibration using standard reference material . 3
4.6 Test procedures . 3
4.6.1 Test without a crucible . 3
4.6.2 Test with a crucible . 4
4.6.3 Description of test. 4
4.7 Calculations . 5
4.7.1 General. 5
4.7.2 Determination of the calorimetric calibration factor . 5
4.7.3 Determination of mean specific heat capacity C .
p
5
5 Method B – differential scanning calorimetry . 6
5.1 Principle . 6
5.1.1 General. 6
5.1.2 Stepwise heating method . 6
5.1.3 Continuous heating method . 7
5.2 Apparatus . 8
5.3 Standard reference materials, SRM . 8
5.4 Test specimens . 8
5.5 Temperature calibration . 8
5.6 Test procedure for the determination of C .
p 8
5.6.1 General. 8
5.6.2 Method 1: Measurements requiring the knowledge of the K factor . 9
5.6.3 Method 2: measurements requiring the use of a reference standard
material (SRM) .11
5.7 Calculation of results .14
5.7.1 Method requiring the knowledge of the K factor .14
5.7.2 Method using an SRM .16
6 Test report .17
Annex A (normative) Drop calorimetry – determination of the calibration factor using
standard reference material .18
Annex B (informative) Standard reference material .20
Annex C (informative) Materials for calorimeter calibrations .25
Bibliography .26
© ISO 2017 – All rights reserved iii
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SIST EN ISO 19628:2021
ISO 19628:2017(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 on 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 the following
URL: w w w . i s o .org/ iso/ foreword .html
This document was prepared by Technical Committee ISO/TC 206, Fine ceramics.
iv © ISO 2017 – All rights reserved
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SIST EN ISO 19628:2021
INTERNATIONAL STANDARD ISO 19628:2017(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Thermophysical properties of ceramic
composites — Determination of specific heat capacity
1 Scope
This document describes two methods for the determination of the specific heat capacity of ceramic
matrix composites with continuous reinforcements (1D, 2D, 3D).
Unidirectional (1D), bi-directional (2D) and tridirectional (XD, with 2 < x ≤ 3).
The two methods are:
— method A: drop calorimetry;
— method B: differential scanning calorimetry.
They are applicable from ambient temperature up to a maximum temperature, depending on the
method: method A can be used up to 2 250 K, while method B is limited to 1 900 K.
NOTE Method A is limited to the determination of an average value of the specific heat capacity over a given
temperature range and can give a larger spread of results.
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 19634, Fine ceramics (advanced ceramics, advanced technical ceramics) — Ceramic composites —
Notations and symbols
IEC 60584-1, Thermocouples — Part 1: Reference tables
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 19634 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http:// www .electropedia .org/
— ISO Online browsing platform: available at http:// www .iso .org/ obp
3.1
specific heat capacity
C
p
amount of heat required to raise the temperature of a mass unit of material by 1 K at constant
temperature and pressure
1 dQ
C =
p
mdT
where Q is the heat required for a test-piece of mass m.
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SIST EN ISO 19628:2021
ISO 19628:2017(E)
3.2
mean specific heat capacity
C
p
amount of heat required to raise the temperature of a mass unit of a material from temperature T to
1
temperature T at a constant pressure, divided by the temperature increase (T – T ) expressed in K
2 2 1
3.3
representative volume element
RVE
minimum volume which is representative of the material considered
4 Method A – drop calorimetry
4.1 Principle
A test piece is dropped from a conditioning chamber at a constant temperature T to another chamber
1
at a constant temperature T .
2
The mean specific heat capacity is determined from the measured amount of heat required to maintain
the temperature constant in the second chamber. Transfer of the test piece shall be done under
conditions as close as possible to adiabatic conditions.
4.2 Apparatus
4.2.1 Drop calorimeter, there are several types of drop calorimeters. They include one (or more)
conditioning chambers and measuring chambers, which can be operated under controlled atmosphere
and which are all equipped with a temperature control system that allows a temperature stability of less
than 1 K.
The conditioning chamber shall have a homogeneous temperature zone size greater than the test
specimen size. The measuring chamber shall have a homogeneous temperature zone of a sufficient
length to accept several specimens and a sufficient thermal inertia to limit the temperature disturbance,
due to the drop.
Heat transfer by radiation during the drop shall be avoided as far as possible.
4.2.2 Balance, with an accuracy of 0,1 mg for test pieces over 10 mg and an accuracy of 0,01 mg for
test pieces below 10 mg.
4.2.3 Temperature detectors, thermocouples in accordance with IEC 60584-1 shall be used for the
measurement of temperature up to 1 920 K.
For higher temperatures, infrared detectors or any other suitable device may be used.
4.2.4 Data acquisition system, the sampling period during the test shall be less than 0,5 s.
4.3 Standard reference materials
Standard reference materials which can be used for calibration purposes are listed in Annex B.
4.4 Test specimens
The test specimens shall be representative of the material.
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SIST EN ISO 19628:2021
ISO 19628:2017(E)
This criterion is generally met by test specimens containing the maximum number of representative
volume elements compatible with the volume of the crucible. If this number is less than five, several
solutions are possible:
a) the test specimens should have an exact number of representative volume elements;
b) the material should be cut into specimens; a number of similar test specimens should be tested and
an average value determined.
4.5 Calibration of calorimeter
4.5.1 General
Calibration of calorimeters may be done according to two different methods. The first consists of
dissipating a known amount of thermal power using a calibrated resistor introduced in the second
chamber of the calorimeter. In the second method a reference specimen with known specific heat
capacity is dropped according to the procedure described in 4.6.
4.5.2 Electrical calibration
The calibration factor is the ratio of a known amount of thermal power dissipated in the resistor to the
steady-state calorimetric output signal, and is measured at temperature T .
2
NOTE 1 The method using power dissipation in a resistor is limited to 1 350 K.
NOTE 2 This method can only be used if the sensitivity of the calorimeter is not affected by the filling of the
measuring chamber.
4.5.3 Calibration using standard reference material
This calibration is called “drop calibration”. A specimen made of a standard reference material with a
known specific heat capacity is dropped according to the test procedures described in 4.6. (See Annex B
for standard reference material.) The calibration factor is determined according to Annex A.
4.6 Test procedures
4.6.1 Test without a crucible
4.6.1.1 Test with drop calibration
The test without a crucible and with drop calibration is done in the following order:
R, T, R, T, R, T, R
where
R is the test of standard reference material;
T is the test of test specimen.
Carry out each test as described in 4.6.3.
4.6.1.2 Test with electrical calibration
The test without a crucible and with calibration using power dissipation in a resistor is done in the
following order:
— calibration of calorimeter;
© ISO 2017 – All rights reserved 3
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SIST EN ISO 19628:2021
ISO 19628:2017(E)
— test on three test specimens.
Carry out each test as described in 4.6.3.
NOTE The avoidance of interaction between the test specimen and the calorimetric conditioning and
measuring chambers can require the use of a sealed crucible.
4.6.2 Test with a crucible
4.6.2.1 General
The mass of all empty crucibles used for the test shall not differ by more than 5 %.
4.6.2.2 Test with drop calibration
The test with a crucible and with drop calibration is carried out in the following order:
C, C + R, C + T, C, C + R, C + T, C, C + R, C + T, C
where
C is the test with the empty crucible;
C + R is the test of crucible plus standard reference material;
C + T is the test of crucible plus test specimen.
Carry out each test as described in 4.6.3.
4.6.2.3 Test with electrical calibration
The test with a crucible and with calibration using power dissipation in a resistor is done in the
following order:
— calibration of calorimeter;
— carry out the following sequence:
C, C + T, C, C + T, C, C + T, C
where
C is the test with the empty crucible;
C + T is the test with crucible plus test specimen.
Carry out each test as described in 4.6.3.
4.6.3 Description of test
The test piece (test specimen, standard material or empty crucible) and reference material shall be
dried at (110 ± 5) °C until the difference in weight of two successive weighings is lower than 0,2 mg:
— measure the mass when a crucible is not used with an accuracy of ± 0,1 mg or ± 0,1 %, whichever is
the smaller;
— when a crucible is used, measure the mass of each assembly dropped (empty crucible, crucible and
standard reference material, crucible and test specimen);
4 © ISO 2017 – All rights reserved
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SIST EN ISO 19628:2021
ISO 19628:2017(E)
— place the test piece (test specimen, standard material or empty crucible) in the conditioning chamber
at temperature T and wait for a sufficient period (around 15 min) to reach thermal equilibrium of
1
the test piece with its environment;
— measure T and T ;
1 2
— start recording the calorimetric signal before the test piece is dropped;
— drop the test piece;
— stop the recording when the steady-state output signal is reached.
4.7 Calculations
4.7.1 General
The change in heat Q corresponding to the drop of the test piece is related to the area A under the
calorimetric output signal by the following equation.
QK=⋅A
where K is the calorimeter calibration factor.
4.7.2 Determination of the calorimetric calibration factor
4.7.2.1 Electrical calibration
See Annex A.
heat dissipated H
K = ==
area under the calorimetric output signal A
4.7.2.2 With standard reference material
See Annex B.
4.7.3 Determination of mean specific heat capacity C
p
The mean specific heat capacity is determined using the following formula:
QT( ,)T
1
i1 2
CT(=,)T
p1 2
m (TT− )
i 21
where
T is the initial temperature at which test pieces are conditioned;
1
T is the calorimeter temperature;
2
Q (T ,T ) is the heat variation between T and T ;
i 1 2 1 2
m is the mass of the test piece, determined by weighing;
i
is the mean specific heat capacity between T and T .
1 2
CT(,T )
p1 2
© ISO 2017 – All rights reserved 5
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SIST EN ISO 19628:2021
ISO 19628:2017(E)
The subscript i has a different meaning depending on the type of test piece:
— i = c for an empty crucible;
— i = t for a test piece;
— i = t + c for a test piece and crucible.
without crucible
KA⋅
t
C =
pt
mT −T
()
t 21
with crucible
KA( −A )
c + tc
C =
pt
mT( −T )
t2 1
where
A is the value of integration of calorimetric output signal of test specimen;
t
A is the value of integration of calorimetric output signal of crucible;
c
A is the value of integration of calorimetric output signal of test specimen plus crucible.
c+t
5 Method B – differential scanning calorimetry
5.1 Principle
5.1.1 General
The method consists in measuring the difference in power needed to raise the temperature of the test
specimen in its crucible and of an empty identical crucible using the same heating programme, which
may be stepwise heating or continuous heating.
Stepwise heating allows only the determination of the mean specific heat capacity CT ,T over a
()
p1 2
temperature range (T ,T ), whereas continuous heating allows determination of the specific heat
1 2
capacity C at a given temperature.
p
5.1.2 Stepwise heating method
The mean specific heat capacity CT ,T is measured in a temperature interval defined by two
()
p1 2
isothermal levels, T and T . The heat, Q , which is necessary to change the temperature from T to T is
1 2 E 1 2
determined by integrating the thermal power, P , with respect to time. The corresponding heat, Q , is:
E E
6 © ISO 2017 – All rights reserved
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SIST EN ISO 19628:2021
ISO 19628:2017(E)
t
QP==dt ((mC TT,+))CC+ (TT− )
EE tp 12 co 21
∫
o
where
m is the mass of the test specimen;
t
is the mean specific heat capacity of the test specimen;
CT ,T
()
p1 2
C is the heat capacity of the calorimeter;
o
C is the heat capacity of the crucible.
c
Another experiment for the determination of the baseline is performed using an identical imposed
heating sequence with the empty crucible. The corresponding heat, Q , is given by:
B
t
QP==dt CC+( TT− )
BB co 21
∫
o
From the above equations, the mean specific heat capacity can be calculated as:
QQ−
EB
CT(=−T )
p1 2
mT( −T )
t2 1
5.1.3 Continuous heating method
Temperature is increased linearly versus time at a constant heating rate ß. Using the same notation as
in 5.1.2, the thermal power P supplied to the system at every moment is:
E
KS⋅= mC ++CC β
()
c+tt pc o
Another experiment for the determination of the baseline is performed with the empty crucible. The
corresponding thermal power is given by
KS⋅ =(CC+)β
cc o
The specific heat capacity can be calculated from:
KS( −)S
c+tc
C =
p
m β
t
where
K is the calibration factor;
S , S are the output signals;
c c+t
K ⋅ S and K ⋅ S are the thermal powers supplied to the system.
c c+t
© ISO 2017 – All rights reserved 7
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SIST EN ISO 19628:2021
ISO 19628:2017(E)
5.2 Apparatus
5.2.1 Differential scanning calorimeter.
5.2.1.1 There are two types of differential scanning calorimeters operating on power compensation
and heat flux principles, both designed to operate und
...
SLOVENSKI STANDARD
oSIST prEN ISO 19628:2021
01-januar-2021
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Termofizikalne
lastnosti keramičnih kompozitov - Ugotavljanje specifične toplotne kapacitete (ISO
19628:2017)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Thermophysical
properties of ceramic composites - Determination of specific heat capacity (ISO
19628:2017)
Hochleistungskeramik - Thermophysikalische Eigenschaften von keramischen
Verbundwerkstoffen - Bestimmung der spezifischen Wärmekapazität (ISO 19628:2017)
Céramiques techniques - Propriétés thermophysiques des composites céramiques -
Détermination de la capacité thermique specifique (ISO 19628:2017)
Ta slovenski standard je istoveten z: prEN ISO 19628
ICS:
81.060.30 Sodobna keramika Advanced ceramics
oSIST prEN ISO 19628:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN ISO 19628:2021
---------------------- Page: 2 ----------------------
oSIST prEN ISO 19628:2021
INTERNATIONAL ISO
STANDARD 19628
First edition
2017-04
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Thermophysical properties of ceramic
composites — Determination of
specific heat capacity
Céramiques techniques — Propriétés thermophysiques des composites
céramiques — Détermination de la capacité thermique specifique
Reference number
ISO 19628:2017(E)
©
ISO 2017
---------------------- Page: 3 ----------------------
oSIST prEN ISO 19628:2021
ISO 19628:2017(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2017, Published in Switzerland
All rights reserved. Unless otherwise specified, 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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2017 – All rights reserved
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Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Method A – drop calorimetry. 2
4.1 Principle . 2
4.2 Apparatus . 2
4.3 Standard reference materials . 2
4.4 Test specimens . 2
4.5 Calibration of calorimeter . 3
4.5.1 General. 3
4.5.2 Electrical calibration . 3
4.5.3 Calibration using standard reference material . 3
4.6 Test procedures . 3
4.6.1 Test without a crucible . 3
4.6.2 Test with a crucible . 4
4.6.3 Description of test. 4
4.7 Calculations . 5
4.7.1 General. 5
4.7.2 Determination of the calorimetric calibration factor . 5
4.7.3 Determination of mean specific heat capacity C .
p
5
5 Method B – differential scanning calorimetry . 6
5.1 Principle . 6
5.1.1 General. 6
5.1.2 Stepwise heating method . 6
5.1.3 Continuous heating method . 7
5.2 Apparatus . 8
5.3 Standard reference materials, SRM . 8
5.4 Test specimens . 8
5.5 Temperature calibration . 8
5.6 Test procedure for the determination of C .
p 8
5.6.1 General. 8
5.6.2 Method 1: Measurements requiring the knowledge of the K factor . 9
5.6.3 Method 2: measurements requiring the use of a reference standard
material (SRM) .11
5.7 Calculation of results .14
5.7.1 Method requiring the knowledge of the K factor .14
5.7.2 Method using an SRM .16
6 Test report .17
Annex A (normative) Drop calorimetry – determination of the calibration factor using
standard reference material .18
Annex B (informative) Standard reference material .20
Annex C (informative) Materials for calorimeter calibrations .25
Bibliography .26
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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 on 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 the following
URL: w w w . i s o .org/ iso/ foreword .html
This document was prepared by Technical Committee ISO/TC 206, Fine ceramics.
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oSIST prEN ISO 19628:2021
INTERNATIONAL STANDARD ISO 19628:2017(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Thermophysical properties of ceramic
composites — Determination of specific heat capacity
1 Scope
This document describes two methods for the determination of the specific heat capacity of ceramic
matrix composites with continuous reinforcements (1D, 2D, 3D).
Unidirectional (1D), bi-directional (2D) and tridirectional (XD, with 2 < x ≤ 3).
The two methods are:
— method A: drop calorimetry;
— method B: differential scanning calorimetry.
They are applicable from ambient temperature up to a maximum temperature, depending on the
method: method A can be used up to 2 250 K, while method B is limited to 1 900 K.
NOTE Method A is limited to the determination of an average value of the specific heat capacity over a given
temperature range and can give a larger spread of results.
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 19634, Fine ceramics (advanced ceramics, advanced technical ceramics) — Ceramic composites —
Notations and symbols
IEC 60584-1, Thermocouples — Part 1: Reference tables
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 19634 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http:// www .electropedia .org/
— ISO Online browsing platform: available at http:// www .iso .org/ obp
3.1
specific heat capacity
C
p
amount of heat required to raise the temperature of a mass unit of material by 1 K at constant
temperature and pressure
1 dQ
C =
p
mdT
where Q is the heat required for a test-piece of mass m.
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3.2
mean specific heat capacity
C
p
amount of heat required to raise the temperature of a mass unit of a material from temperature T to
1
temperature T at a constant pressure, divided by the temperature increase (T – T ) expressed in K
2 2 1
3.3
representative volume element
RVE
minimum volume which is representative of the material considered
4 Method A – drop calorimetry
4.1 Principle
A test piece is dropped from a conditioning chamber at a constant temperature T to another chamber
1
at a constant temperature T .
2
The mean specific heat capacity is determined from the measured amount of heat required to maintain
the temperature constant in the second chamber. Transfer of the test piece shall be done under
conditions as close as possible to adiabatic conditions.
4.2 Apparatus
4.2.1 Drop calorimeter, there are several types of drop calorimeters. They include one (or more)
conditioning chambers and measuring chambers, which can be operated under controlled atmosphere
and which are all equipped with a temperature control system that allows a temperature stability of less
than 1 K.
The conditioning chamber shall have a homogeneous temperature zone size greater than the test
specimen size. The measuring chamber shall have a homogeneous temperature zone of a sufficient
length to accept several specimens and a sufficient thermal inertia to limit the temperature disturbance,
due to the drop.
Heat transfer by radiation during the drop shall be avoided as far as possible.
4.2.2 Balance, with an accuracy of 0,1 mg for test pieces over 10 mg and an accuracy of 0,01 mg for
test pieces below 10 mg.
4.2.3 Temperature detectors, thermocouples in accordance with IEC 60584-1 shall be used for the
measurement of temperature up to 1 920 K.
For higher temperatures, infrared detectors or any other suitable device may be used.
4.2.4 Data acquisition system, the sampling period during the test shall be less than 0,5 s.
4.3 Standard reference materials
Standard reference materials which can be used for calibration purposes are listed in Annex B.
4.4 Test specimens
The test specimens shall be representative of the material.
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This criterion is generally met by test specimens containing the maximum number of representative
volume elements compatible with the volume of the crucible. If this number is less than five, several
solutions are possible:
a) the test specimens should have an exact number of representative volume elements;
b) the material should be cut into specimens; a number of similar test specimens should be tested and
an average value determined.
4.5 Calibration of calorimeter
4.5.1 General
Calibration of calorimeters may be done according to two different methods. The first consists of
dissipating a known amount of thermal power using a calibrated resistor introduced in the second
chamber of the calorimeter. In the second method a reference specimen with known specific heat
capacity is dropped according to the procedure described in 4.6.
4.5.2 Electrical calibration
The calibration factor is the ratio of a known amount of thermal power dissipated in the resistor to the
steady-state calorimetric output signal, and is measured at temperature T .
2
NOTE 1 The method using power dissipation in a resistor is limited to 1 350 K.
NOTE 2 This method can only be used if the sensitivity of the calorimeter is not affected by the filling of the
measuring chamber.
4.5.3 Calibration using standard reference material
This calibration is called “drop calibration”. A specimen made of a standard reference material with a
known specific heat capacity is dropped according to the test procedures described in 4.6. (See Annex B
for standard reference material.) The calibration factor is determined according to Annex A.
4.6 Test procedures
4.6.1 Test without a crucible
4.6.1.1 Test with drop calibration
The test without a crucible and with drop calibration is done in the following order:
R, T, R, T, R, T, R
where
R is the test of standard reference material;
T is the test of test specimen.
Carry out each test as described in 4.6.3.
4.6.1.2 Test with electrical calibration
The test without a crucible and with calibration using power dissipation in a resistor is done in the
following order:
— calibration of calorimeter;
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— test on three test specimens.
Carry out each test as described in 4.6.3.
NOTE The avoidance of interaction between the test specimen and the calorimetric conditioning and
measuring chambers can require the use of a sealed crucible.
4.6.2 Test with a crucible
4.6.2.1 General
The mass of all empty crucibles used for the test shall not differ by more than 5 %.
4.6.2.2 Test with drop calibration
The test with a crucible and with drop calibration is carried out in the following order:
C, C + R, C + T, C, C + R, C + T, C, C + R, C + T, C
where
C is the test with the empty crucible;
C + R is the test of crucible plus standard reference material;
C + T is the test of crucible plus test specimen.
Carry out each test as described in 4.6.3.
4.6.2.3 Test with electrical calibration
The test with a crucible and with calibration using power dissipation in a resistor is done in the
following order:
— calibration of calorimeter;
— carry out the following sequence:
C, C + T, C, C + T, C, C + T, C
where
C is the test with the empty crucible;
C + T is the test with crucible plus test specimen.
Carry out each test as described in 4.6.3.
4.6.3 Description of test
The test piece (test specimen, standard material or empty crucible) and reference material shall be
dried at (110 ± 5) °C until the difference in weight of two successive weighings is lower than 0,2 mg:
— measure the mass when a crucible is not used with an accuracy of ± 0,1 mg or ± 0,1 %, whichever is
the smaller;
— when a crucible is used, measure the mass of each assembly dropped (empty crucible, crucible and
standard reference material, crucible and test specimen);
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— place the test piece (test specimen, standard material or empty crucible) in the conditioning chamber
at temperature T and wait for a sufficient period (around 15 min) to reach thermal equilibrium of
1
the test piece with its environment;
— measure T and T ;
1 2
— start recording the calorimetric signal before the test piece is dropped;
— drop the test piece;
— stop the recording when the steady-state output signal is reached.
4.7 Calculations
4.7.1 General
The change in heat Q corresponding to the drop of the test piece is related to the area A under the
calorimetric output signal by the following equation.
QK=⋅A
where K is the calorimeter calibration factor.
4.7.2 Determination of the calorimetric calibration factor
4.7.2.1 Electrical calibration
See Annex A.
heat dissipated H
K = ==
area under the calorimetric output signal A
4.7.2.2 With standard reference material
See Annex B.
4.7.3 Determination of mean specific heat capacity C
p
The mean specific heat capacity is determined using the following formula:
QT( ,)T
1
i1 2
CT(=,)T
p1 2
m (TT− )
i 21
where
T is the initial temperature at which test pieces are conditioned;
1
T is the calorimeter temperature;
2
Q (T ,T ) is the heat variation between T and T ;
i 1 2 1 2
m is the mass of the test piece, determined by weighing;
i
is the mean specific heat capacity between T and T .
1 2
CT(,T )
p1 2
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The subscript i has a different meaning depending on the type of test piece:
— i = c for an empty crucible;
— i = t for a test piece;
— i = t + c for a test piece and crucible.
without crucible
KA⋅
t
C =
pt
mT −T
()
t 21
with crucible
KA( −A )
c + tc
C =
pt
mT( −T )
t2 1
where
A is the value of integration of calorimetric output signal of test specimen;
t
A is the value of integration of calorimetric output signal of crucible;
c
A is the value of integration of calorimetric output signal of test specimen plus crucible.
c+t
5 Method B – differential scanning calorimetry
5.1 Principle
5.1.1 General
The method consists in measuring the difference in power needed to raise the temperature of the test
specimen in its crucible and of an empty identical crucible using the same heating programme, which
may be stepwise heating or continuous heating.
Stepwise heating allows only the determination of the mean specific heat capacity CT ,T over a
()
p1 2
temperature range (T ,T ), whereas continuous heating allows determination of the specific heat
1 2
capacity C at a given temperature.
p
5.1.2 Stepwise heating method
The mean specific heat capacity CT ,T is measured in a temperature interval defined by two
()
p1 2
isothermal levels, T and T . The heat, Q , which is necessary to change the temperature from T to T is
1 2 E 1 2
determined by integrating the thermal power, P , with respect to time. The corresponding heat, Q , is:
E E
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t
QP==dt ((mC TT,+))CC+ (TT− )
EE tp 12 co 21
∫
o
where
m is the mass of the test specimen;
t
is the mean specific heat capacity of the test specimen;
CT ,T
()
p1 2
C is the heat capacity of the calorimeter;
o
C is the heat capacity of the crucible.
c
Another experiment for the determination of the baseline is performed using an identical imposed
heating sequence with the empty crucible. The corresponding heat, Q , is given by:
B
t
QP==dt CC+( TT− )
BB co 21
∫
o
From the above equations, the mean specific heat capacity can be calculated as:
QQ−
EB
CT(=−T )
p1 2
mT( −T )
t2 1
5.1.3 Continuous heating method
Temperature is increased linearly versus time at a constant heating rate ß. Using the same notation as
in 5.1.2, the thermal power P supplied to the system at every moment is:
E
KS⋅= mC ++CC β
()
c+tt pc o
Another experiment for the determination of the baseline is performed with the empty crucible. The
corresponding thermal power is given by
KS⋅ =(CC+)β
cc o
The specific heat capacity can be calculated from:
KS( −)S
c+tc
C =
p
m β
t
where
K is the calibration factor;
S , S are the output signals;
c c+t
K ⋅ S and K ⋅ S are the thermal powers supplied to the system.
c c+t
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5.2 Apparatus
5.2.1 Differential scanning calorimeter.
5.2.1.1 There are two types of differential scanning calorimeters operating on power compensation
and heat flux principles, both designed to operate under adiabatic conditions.
Both comprise two measuring cells housed in a furnace which provides overall system heating. One cell
contains the test specimen and its crucible, the other contains an empty crucible only.
5.2.1.2 Power compensation type: each cell has an additional heater to compensate for the temperature
variations from the overall heating programme. The power which is supplied to either cell heater to
maintain equal temperatures during heating is measured.
5.2.1.3 Heat flux type: power is exchanged between each cell and its respective surrounding during the
heating programme. The difference in power exchange between the two cells is measured.
5.2.2 Balance, with an accuracy better than 0,1 mg.
5.2.3 Temperature detectors, thermocouples in accordance with IEC 60584-1 shall be used for the
measurement of temperature.
5.2.4 Data acquisition system, the time duration between two successive measurements shall be less
than 0,5 s.
5.3 Standard reference materials, SRM
Standard reference materials shall be used for calibration. An example is given in Annex B.
5.4 Test specimens
The test specimens shall be representative of the material.
This criterion is generally met by test specimens containing the maximum number of representative
volume elements compatible with the volume of the crucible. If this number is less than five, several
solutions are possible:
a) the test specimens should have an exact number of representative volume elements;
b) the material should be cut into pieces, and a number of similar test pieces should be tested and an
average value determined.
5.5 Temperature calibration
A temperature calibration curve for the furnace using the same heating rate as for the determination
of the specific heat capacity is established by using the melting points of standard reference materials
(see, for example, Annex C).
Thermocouples shall be calibrated in accordance with IEC 60584-1.
5.6 Test procedure for the determination of C
p
5.6.1 General
Depending on the necessity or not of using a calibration factor K for the calorimeter, two methods can
be used:
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Method 1: measurements requiring the knowledge of the K factor; in this case, care shall be taken in
order to ensure that the calibration is valid for all the measurements to be taken.
NOTE Generally, this can be done by running a test using a test specimen with well-known properties.
Method 2: measurements requiring the use of a reference standard material during a series of tests.
5.6.2 Method 1: Measurements requiring the knowledge of the K factor
5.6.2.1 Determination of the K factor
The calibration factor K is obtained by electrical calibration. It is determined from the ratio of a known
amount of power dissipated in a resistor to the steady-state calorimetric output signal.
5.6.2.2 Measurements with the specimen for the determination of the C
p
5.6.2.2.1 General
A series of measurements shall always be referenced to a baseline measurement performed under
experimental conditions identical to the other measurements in the series. The type of crucible used
depends on the type of test specimen and on the temperature range, and shall be the same for the series
of measurements. The mass of all empty crucibles used in the series shall not differ by more than 5 %.
5.6.2.2.2 Test sequence for the stepwise heating method (see Figure 1)
5.6.2.2.2.1 Generation of the baseline
See Figure 1.
a) weigh the two empty crucibles to the nearest 0,1 mg;
b) place the two crucibles in the calorimeter;
c) set the calorimeter heating rate, initial and final temperature, and cooling rate;
NOTE Generally, the heating rate is in the range 1 K/min to 20 K/min.
d) heat to an initial temperature, and wait for the temperature to be stabilized at the initial
temperature;
e) heat at a constant rate to final temperature of the first step while recording the calorimeter output
signal, until the final temperature is reached and stabilized in order to obtain a baseline;
f) repeat c) to e) for the number of steps required;
g) co
...
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