Bsi bs en 01159 1 2003 (2004)

BS EN
1159-1:2003

BRITISH STANDARD

Advanced technical
ceramics — Ceramic
composites —
Thermophysical
properties —
Part 1: Determination of thermal
expansion

The European Standard EN 1159-1:2003 has the status of a
British Standard

ICS 81.060.30

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BS EN 1159-1:2003

National foreword
This British Standard is the official English language version of
EN 1159-1:2003. It supersedes DD ENV 1159-1:1994 which is withdrawn.
The UK participation in its preparation was entrusted to Technical Committee
RPI/13, Advanced technical ceramics, which has the responsibility to:
—

aid enquirers to understand the text;

—

present to the responsible international/European committee any
enquiries on the interpretation, or proposals for change, and keep the
UK interests informed;

—

monitor related international and European developments and
promulgate them in the UK.

A list of organizations represented on this committee can be obtained on
request to its secretary.
Cross-references
The British Standards which implement international or European
publications referred to in this document may be found in the BSI Catalogue
under the section entitled “International Standards Correspondence Index”, or
by using the “Search” facility of the BSI Electronic Catalogue or of
British Standards Online.
This publication does not purport to include all the necessary provisions of a

contract. Users are responsible for its correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.

Summary of pages
This document comprises a front cover, an inside front cover, the EN title page,
pages 2 to 15 and a back cover.
The BSI copyright notice displayed in this document indicates when the
document was last issued.

This British Standard was
published under the authority
of the Standards Policy and
Strategy Committee on
10 February 2004

Amendments issued since publication
Amd. No.

Date

Comments

© BSI 10 February 2004

ISBN 0 580 43383 8
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EUROPEAN STANDARD

EN 1159-1

NORME EUROPÉENNE
EUROPÄISCHE NORM

July 2003

ICS 81.060.30

Supersedes ENV 1159-1:1993

English version

Advanced technical ceramics - Ceramic composites Thermophysical properties - Part 1: Determination of thermal
expansion
Céramiques techniques avancées - Céramiques
composites - Propriétés thermophysiques - Partie 1:
Détermination de la dilatation thermique

Hochleistungskeramik - Keramische Verbundwerkstoffe Thermophysikalische Eigenschaften - Teil 1: Bestimmung
der thermischen Ausdehrung

This European Standard was approved by CEN on 23 May 2003.
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 Management Centre or to any CEN member.

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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 Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and United
Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: rue de Stassart, 36

© 2003 CEN

All rights of exploitation in any form and by any means reserved
worldwide for CEN national Members.

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Ref. No. EN 1159-1:2003 E

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EN 1159-1:2003 (E)

Contents

page

1

Scope ..............................................................................................................................................................4

2

Normative references ....................................................................................................................................4

3

Terms and definitions....................................................................................................................................4

4
4.1
4.2
4.3

Principle ..........................................................................................................................................................5
General............................................................................................................................................................5
Direct measurement ......................................................................................................................................5
Differential method ........................................................................................................................................5

5
5.1
5.2
5.3
5.4
5.5
5.6

Apparatus .......................................................................................................................................................5
Construction materials..................................................................................................................................5
Heating and cooling device ..........................................................................................................................5
Temperature measurement...........................................................................................................................5
Test piece mounting ......................................................................................................................................5
System for measuring and recording the thermal expansion...................................................................6
Test piece measurement ...............................................................................................................................6

6
6.1
6.2
6.3

Specimens ......................................................................................................................................................6
Test pieces......................................................................................................................................................6
Reference pieces ...........................................................................................................................................6
Dimensions.....................................................................................................................................................7

7

Procedure .......................................................................................................................................................7

8
8.1
8.2

Calculations....................................................................................................................................................7
Direct measurement ......................................................................................................................................7
Differential method ........................................................................................................................................8

9

Test report ......................................................................................................................................................9

Annex A (normative) Direct measurement apparatus ...........................................................................................12
A.1
Determination of measurement sensitivity ...............................................................................................12
A.2
Determination of
A ...................................................................................................................................13
Annex B (normative) Differential type measurement apparatus ..........................................................................14
B.1
Determination of measurement sensitivity S ............................................................................................14
B.2
Determination of
........................................................................................................................................14
Bibliography ..............................................................................................................................................................15

2

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Foreword......................................................................................................................................................................3


EN 1159-1:2003 (E)

Foreword
This document (EN 1159-1:2003) has been prepared by Technical Committee CEN /TC 184, "Advanced technical
ceramics" the secretariat of which is held by BSI.
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 January 2004, and conflicting national standards shall be withdrawn at the latest
by January 2004.
This document supersedes ENV 1159-1:1993.
EN 1159 'Advanced technical ceramics – Ceramic composites – Thermophysical properties' consists of four parts :


Part 1 : Determination of thermal expansion.



Part 2 : Determination of thermal diffusivity.



Part 3 : Determination of specific heat capacity.



Part 4: Determination of thermal conductivity

Annexes A and B are normative.

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According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,
Slovakia, Spain, Sweden, Switzerland and the United Kingdom.

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EN 1159-1:2003 (E)

1

Scope

This Part of EN 1159 describes methods for the determination of linear thermal expansion characteristics of
ceramic matrix composite materials up to 2 300 K, and is applicable to 10, 2D and nD materials.
The method describes general principles of construction calibration and operation of the equipment.

2

Normative references

This European Standard incorporates by dated or undated reference, provisions from other publications. These
normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For
dated references, subsequent amendments to or revisions of any of these publications apply to this European
Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the
publication referred to applies (including amendments).
EN 821-1, Advanced technical ceramics - Monolithic ceramics - Thermo-physical properties - Part 1 : Determination
of thermal expansion.
EN 60584-1, Thermocouples – Part 1: Reference tables (IEC 60584-1:1995)
EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC
17025:1999)
ISO 3611, Micrometer callipers for external measurement.

3

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ISO 6906, Vernier callipers reading to 0,02 mm.

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Terms and definitions

For the purposes of this European Standard, the following terms and definitions apply.
3.1
linear thermal expansion
positive or negative change in one dimension that occurs when a material is subjected to a change in temperature
3.2
linear thermal expansion coefficient at temperature T
derivative of the length L with respect to temperature at the temperature T, divided by the length at temperature T


T



1  dL 


T
L  dT 

(1)

3.3
mean linear thermal expansion coefficient between temperatures T1 and T2
linear thermal expansion between temperatures T1 and T2 divided by the temperature increment T1 to T2 and the
length at temperature T1
L  T2  L  T1 




 T1,T2 
   


L  T1 
 

(2)

3.4
representative volume element (R.V.E.)
minimum volume which is representative of the material considered
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EN 1159-1:2003 (E)

4
4.1

Principle
General

A test piece is heated and subsequently cooled, either at a specified uniform rate or using defined temperature
increments. Its change of length and its temperature are measured continuously or at regular frequent intervals
during the imposed temperature cycle.
One of two methods may be used to determine the linear thermal expansion coefficient, either by direct
measurement or by a differential method.

4.2

Direct measurement

In this method the variation in length of the test piece is measured directly. It is necessary to know the change in
dimensions of the test piece support system by previous calibration.
The test piece is placed in a specimen holder and is made to contact a displacement transducer by using a push
rod made of the same material as the holder. This assembly is put in a furnace. The differential expansion between
the test piece and the test piece holder is measured during the increase and the decrease in temperature.
The apparatus is shown in Figure 1.

4.3

Differential method

This method consists of measuring the changes in length between a reference piece (see 6.2) and the test piece.
Its is not therefore necessary to know the change in dimensions of the test piece support system.
The apparatus is shown in Figure 2.

5
5.1

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Apparatus
Construction materials

The test piece holder and the push rod shall be made from thermomechanically stable materials of the same type,
which shall be chemically inert and thermally compatible with the test piece material under the environmental
conditions of the test.
NOTE
For temperatures above 1 400 °C, it is necessary to employ a vacuum or inert gas atmosphere, with a non-oxide
material appropriate for the test environment, such as a grade of dense graphite.

5.2

Heating and cooling device

Furnace, capable of working in a controlled atmosphere when required, and of controlling the temperature of the
test piece to within 1 % of its mean temperature, expressed in K.

5.3

Temperature measurement

Thermocouples, in accordance with EN 60584-1, subject to the upper temperature requirements and environmental
consideration, except for tungsten-rhenium couples which may be used at higher temperatures, but are not
covered by EN 60584-1 should be individually calibrated. For temperature in excess of 2 000 K, infrared detectors
or any suitable device may be used.

5.4

Test piece mounting

The device used shall allow free axial movement of the test piece and of the reference piece in case of differential
measurement. The mechanical environment shall minimize stresses. For vertical measurement apparatus, the test
pieces shall be free standing and mechanically stable on the end-plate. For measuring apparatus which is
5
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EN 1159-1:2003 (E)

horizontal or inclined to the horizontal, the sideways movement or twist of the test piece shall be restricted, without
any restriction of axial movement, by a suitable arrangement.

5.5

System for measuring and recording the thermal expansion

System, capable of measuring displacements to an accuracy better than 0,1 m. The system shall allow recording
of the test piece temperauture and the displacement simultaneously. The system for measuring of displacements
shall be periodically calibrated in accordance with annex A for direct measurement or annex B for differential
measurement.

5.6

Test piece measurement

Device for measuring the test piece dimensions, with an accuracy better than 0,05 mm (e.g. micrometer in
accordance with ISO 3611 or callipers in accordance with ISO 6906).

6

Specimens

6.1

Test pieces

The dimensions of the test pieces depend on the type of apparatus used. For differential measurements the test
piece and the reference piece (see 6.2) shall have the same length L0 (see Table 1).
The test piece shall be cut in such a way that the axis of desired measurement is related to the principal fibre
orientations in accordance with agreement between parties to the measurement.

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6.2

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The end-faces of the length of the test piece shall be plane, parallel to each other and perpendicular to the long
axis.

Reference pieces

Reference materials shall be chosen so that their properties are as close as possible to the properties of the

material to be tested. The reference piece shall have a volume of the same order and if possible shall have the
same dimensions as the test piece (see Table 1).
For measurement at high temperature (over 2 000 K) under inert atmosphere, reference materials generally used
are either tungsten or highly purified graphite. Reference materials shall be procured from a certified laboratory.
NOTE
NIST in the USA is one laboratory which supplies reference materials. Highly purified 'POCO' graphite is largely
used as a reference for measurement at high temperature.

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EN 1159-1:2003 (E)
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6.3

Dimensions
Table 1 — Recommended test piece dimensions
Dimensions in millimeters
Material with small R.V.E. Material with large R.V.E.
(see 3.4) such as 1D or 2D
(see 3.4) such as nD

Tolerances

L0, total length

30

70


0,2

B, width

7

-

-

h, thickness

Depending on material and Depending on material and Depending on material and
equipment
equipment
equipment

 diameter

-

30

-

Parallelism


0,01


0,01

-

NOTE 1

A test piece volume of a minimum of 5 R.V.E. is recommended (see 3.4).

NOTE 2
The shape and dimensions of the test piece depend on the structure of reinforcement. In the case of material such
as 3D, a large test piece is often necessary when the representative volume element is important.

7

Procedure

In order to simplify calibration procedures, test pieces and reference pieces of the same length should be used. If
reference and test pieces have different lengths, then it is necessary to take into account a base line shift. In this
case, refer to EN 821-1.

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Measure the original length of the test piece at room temperature to an accuracy better than 0,2 mm.

Make sure that the equipment has been calibrated for the type of material prior to the test, according to the
procedure described in annex A for direct measurement [determination of S and
 A  ] and in annex B for
 
differential measurement (determination of S and
). If the test is to be performed in an inert or vacuum
environment, establish the environment before commencing heating.

Position the test piece in the equipment and proceed with heating or cooling at a rate of between 1 K/min and
5 K/mins, ensuring a fairly constant temperature gradient along and through the test piece. If the temperature is
changed in steps, the hold temperature shall be maintained until the length of the test piece shows no change for a
period of 5 mins.
In case of large test pieces, a stepwise temperature rise is recommended.
The mean linear thermal expansion coefficient shall be calculated as the average from the results of tests on three
test pieces.

8
8.1

Calculations
Direct measurement

Calculate the change in length,
l, of a length of the sample holder material equal to the original test piece length
L0, from the expression :

l
L0
A  T2 T1


(3)



using the calculated value of
l, obtain the change in length of
l of the test piece from the measured displacement
by S
x :
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EN 1159-1:2003 (E)

L
Sx
l

(4)

Calculate the mean linear thermal expansion coefficient of the test piece material from the expression:





l

(5)

L0  T2 T1 



where




is the mean linear thermal expansion coefficient of the test piece material, in K-1;


A

is the mean linear thermal expansion coefficient correction for the apparatus over the temperature
range used. It is determined from calibration (see annex A);

L0

is the initial length of the test piece at room temperature, in mm;


x

is the recorded displacement (in mm, volt, etc.) over the temperature range;

S

is the measurement sensitivity of the displacement recording system;

l

is the change in length of the sample holder material, in mm;


L

is the change in length of the test piece in mm;

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T2 – T1 is the temperature internal in K for which the change in length is measured.
A curve of

8.2

L
L0

versus T may be constructed.

Differential method

Calculate the mean linear thermal expansion coefficient of the test piece material from the expression:

L
R 
Sx 


R 
L0
L0
T2 T1 

(6)

where



is the baseline correction over the temperature range, which is introduced because of the possibility of
unequal response from the two pushrods;

L (R) is the initial reference piece length in mm at room temperature;


(R)

is the mean linear thermal expansion coefficient of the reference piece in K-1.

and other terms are as in 8.1.

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EN 1159-1:2003 (E)

9

Test report

The results shall be reported in accordance with EN ISO/IEC 17025 and the test report shall include the following
information:
a)

the name of the testing establishment;

b)

the date of the test ; a unique identification of the report and of each page, the name and address of the
customer and a signatory of the report;

c)

a reference to this European standard, i.e. "Determined in accordance with EN 1159-1”;.

d)

general description of the method used, i.e. Direct or Differential (see clause 4);

e)

method of calibration;

f)

description of the test piece : dimensions, preparation method, orientation, mass, volume;

g)

thermal cycle(s), number of hold periods, time at hold periods and temperature interval between holds;

h)

maximum temperature testing;

i)

testing atmosphere;

j)

hysteresis between the heating and cooling cycle for materials which show a repeatable behaviour;

k)

indication of the thermal cycles carried out on the test piece prior to the measurement;

l)

table of the mean linear thermal expansion coefficient at the temperature required;
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m) any features identifiable as phase changes or softening under load of the measuring device;
n)

all other relevant information and all incidents that may affect the results, including comments on the test or
test results.

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EN 1159-1:2003 (E)

1

Expansion ranging

8

Expansion amplifier

2
3

Y axis
X-Y recorder

9
10

Furnace
Sample

4
5

X ais
Temperature ranging

11
12

Push rod
LVDT

6
7

Correction factor
0° C reference

13
14

Sample holder
Programmer

15

Furnace power control

Figure 1 — Schematic of a direct measurement system

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Key


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EN 1159-1:2003 (E)

Key
1

Displacement measurement

8

Strength transducer

2
3

Data treatment (analog or digital)
Encoders

9
10

Strength measurement
Sample

4
5
6

Displacement signal
Displacement modules
Control in order to have F1 = C1 (C1 = adjustable constant)

11
12
13

Reference
Temperature measurement
Furnace

7

Control in order to have F2 = C2 (C2 = adjustable constant)

Figure 2 — Schematic of a differential measurement system

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EN 1159-1:2003 (E)

Annex A
(normative)
Direct measurement apparatus

A.1 Determination of measurement sensitivity
The sensitivity of the measurement device, S, requires to be calibrated if it is not based on a direct-reading dial
gauge or micrometer. This may be done either by using direct mechanical movement produced by using a certified
micrometer of sufficient accuracy, or by use of two certified thermal expansion reference materials as test pieces.
Calibration tests shall be made for mechanical movement in both directions, and then mean value of sensitivity

taken. Calibration should take place in the same environment and at the same heating rate as the measurements
on test piece. Any non-linearity shall be reported, and the apparatus shall be calibrated over the same range of
displacement as that to be used for any series of tests.
This procedure applies to linear displacement transducer measuring devices in particular.

Where two certified thermal expansion reference materials are available, the sensitivity is determined by use of the
expression:



Sx

A
L0 T

(A.1)

for the two materials:
Sx

1
 1

A
L0 T


2


(A.2)

Sx2

A
L0T

(A.3)

and by subtracting:


 L T
1
2 0



S 
x1 x2

(A.4)

where


1

and


2

are the mean thermal expansion coefficient of the two reference materials over the temperature
range T;

L0

is the initial length in mm of the two reference pieces at room temperature;

x1, x2

are the recorded displacements (in mm, volts…) over the temperature range T;

T

is the temperature interval for which the changes in length are measured;

S

is the measured sensitivity of the displacement recording system;


A

is the mean thermal expansion coefficient correction for the apparatus.

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NOTE


EN 1159-1:2003 (E)

A.2 Determination of


A 

R 


A

Sx
L0 T

(A.5)

where :





is the mean linear thermal expansion coefficient correction for the apparatus over the temperature
range used;


 R 

is the mean linear thermal expansion coefficient of the reference piece material;

x,

is the recorded displacement (in mm, volts, etc.) over the temperature range T;

S

is the measurement sensitivity of the displacement recording system;

L0

is the initial length of the test piece in mm;

T

is the temperature range in K over which the change is length is measured.

 




The mean linear thermal expansion coefficient
A is obtained by using a certified reference material of similar
thermal expansion to that of the material of the test piece holder and the push rod, and carrying out measurement
in accordance with the procedure given in clause 7. The value of

A is obtained by inserting calibrated and
experimental data for the reference material in the equation above.
The calibrated reference piece is certified by approved organizations. The dimensions of the test piece to be
measured and of the reference piece are identical within machining tolerances.
NOTE
The physical properties of the material to be measured and the reference material (expansion coefficient,
conductivity, emissivity) should be as close as possible. Measurements on the reference material and on the specimen should
be performed under identical experimental condition : type of environment, measuring kinetics, material for the specimen holder,
temperature measurement device.

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EN 1159-1:2003 (E)

Annex B
(normative)
Differential type measurement apparatus

B.1 Determination of measurement sensitivity S
Because of the differences between the differential dilatometers which can be used, the manufacturer's instructions
should be referred to for the determination of measurement sensitivity.

B.2 Determination of 
The calibration is carried out with two reference test pieces, one having significantly different thermal expansion
characteristics from the other.
The recorded displacement corresponds to the difference in expansion:
S x1
 L0
1 L0
2  T




(B.1)

by exchanging the positions of the reference pieces and by carrying our a new cycle, the displacement is now:
S x2
 L0
2 L0
1  T




(B.2)

the baseline correction is obtained by addition of the two equations:


21 S  x1
x2 


(B.3)



14
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EN 1159-1:2003 (E)

Bibliography

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ISO 31-4, Quantities and units – Part 4:Heat.

15
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BS EN
1159-1:2003

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