1、 ISO 2013 Fine ceramics (advanced ceramics, advanced technical ceramics) Determination of density and apparent porosity Cramiques techniques Dtermination de la masse volumique et de la porosit apparente INTERNATIONAL STANDARD ISO 18754 Second edition 2013-03-01 Reference number ISO 18754:2013(E) ISO
2、 18754:2013(E)ii ISO 2013 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2013 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 in
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4、eb www.iso.org Published in Switzerland ISO 18754:2013(E) ISO 2013 All rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Methods by impregnation with liquid 2 4.1 Apparatus 2 4.2 Test specimen . 2 4.3 Procedure 3 4.4 Accuracy of mass me
5、asurement . 4 4.5 Expression of results 5 5 Determination of geometric bulk density by measurement of dimensions and mass (method C) 5 5.1 Principle 5 5.2 Apparatus 6 5.3 Test pieces . 6 5.4 Procedure 6 5.5 Results 7 6 Test report . 7 ISO 18754:2013(E) Foreword ISO (the International Organization fo
6、r 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
7、 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. Internati
8、onal Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication
9、as an International Standard requires approval by at least 75 % of the member bodies casting a vote. 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.
10、ISO 18754 was prepared by Technical Committee ISO/TC 206, Fine ceramics. T h i s s e c o n d e d i t i o n c a n c e l s a n d r e p l a c e s t h e f i r s t e d i t i o n ( ISO 18754:2003), which has been technically revised.iv ISO 2013 All rights reserved INTERNATIONAL ST ANDARD ISO 18754:2013(E)
11、 Fine ceramics (advanced ceramics, advanced technical ceramics) Determination of density and apparent porosity 1 Scope This International Standard specifies methods for the determination of the apparent solid density, bulk density, apparent density and geometric bulk density of fine ceramics. NOTE T
12、hese methods are not appropriate for the determination of an apparent porosity greater than 10 %. For materials with higher porosity, the accuracy of the measurement may not be satisfactory. The method may also not give a satisfactory open porosity result if it is less than 0,5 % 2 Normative referen
13、ces The following referenced documents 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 386:1977, Liquid-in-glass laboratory ther
14、mometers Principles of design, construction and use ISO 758:1976, Liquid chemical products for industrial use Determination of density at 20 degrees C ISO 13385-1:2011, Geometrical product specifications (GPS) Dimensional measuring equipment Part 1: Callipers; Design and metrological characteristics
15、 EN 1006:2009, Advanced technical ceramics Monolithic ceramics Guidance on the selection of test pieces for the evaluation of properties ISO/IEC 17025:2005, General requirements for the competence of testing and calibration laboratories 3 T erms an d definiti ons For the purposes of this document, t
16、he following terms and definitions apply. 3.1 open pores pores that are penetrated by an immersion liquid, or that are connected to the atmosphere, either directly or via one another 3.2 closed pores pores that are not penetrated by the immersion liquid, or that are not connected to the atmosphere 3
17、.3 bulk volume the sum of the respective volumes of the solid material, the open pores and the closed pores 3.4 apparent solid volume the sum of the respective volumes of the solid material and the closed pores 3.5 apparent solid density the ratio of the mass of the dry material to its apparent soli
18、d volume ISO 2013 All rights reserved 1 ISO 18754:2013(E) 3.6 bulk density the ratio of the mass of the dry material to its bulk volume 3.7 apparent porosity the ratio of the volume of the open pores in a body to its bulk volume 3.8 theoretical density TD density of pore-free material 3.9 geometric
19、bulk density the mass per unit total volume of a material including all porosity accessible and inaccessible from the surface, the volume being calculated from linear dimensions 4 Methods by impregnation with liquid 4.1 Apparatus 4.1.1 Drying oven, capable of being controlled at 110 C 5 C. 4.1.2 Bal
20、ance, accurate to 0,1 mg for a test specimen under 10 g and 0,001 % of the mass of a test specimen for a specimen over 10 g. 4.1.3 Heating apparatus, in which the specimen may be boiled. 4.1.4 Thermometer, in accordance with ISO 386 with an accuracy of 1 C. 4.1.5 Immersion liquid, distilled water or
21、 de-ionized water may be used for materials that do not react with water. For materials that are sensitive to contact with water, a suitable organic liquid shall be used. 4.1.6 Halter or basket, capable of supporting the test pieces in liquid in order to take suspended mass measurements. 4.1.7 Suspe
22、nding wire, of diameter not more than 0,25 mm. The wire should be cleaned and de- greased. Where specimens of small mass are used, the suspending wire having a smaller diameter or the addition of a dilute solution of a suitable surfactant is recommended, because the error caused by the surface tensi
23、on of the liquid on the wire cannot be neglected. 4.1.8 Evacuating equipment, (in the vacuum method) capable of reducing the pressure to a value not greater than 2,5 kPa, and with a means of measuring the pressure used. 4.2 Test specimen The volume of each specimen shall be not less than 0,1 cm 3 .2
24、 ISO 2013 All rights reserved ISO 18754:2013(E) When the volume of each individual test specimen is less than this value, a sufficient number of test specimens shall be taken so that the total volume of the specimens reaches the minimum of volume. In this case, the volume of each individual test spe
25、cimen shall be not less than 0,04 cm 3 . NOTE In the case where the volume of test specimen is less than 0,04 cm 3 , a geometric measurement for the machined specimen may be used only for the determination of bulk density. For the determination of the bulk density and apparent porosity, mercury poro
26、simetry may be applied. However, a combination of a stereological measurement on a polished surface of the test specimen by microscopy is recommended for the reliability. Any dust and chips liable to become detached during further handling shall be removed from the surface of each test piece. Test s
27、pecimens shall have smooth surfaces to sponge out droplets of the immersion liquid from the surface, since roughness limits the accuracy of the mass of the soaked test specimen. 4.3 Procedure 4.3.1 General Drying in a desiccator (see 4.3.2) and the procedure according to 4.3.3, 4.3.4 and 4.3.6 shall
28、 only be carried out if the test specimen has open porosity, i.e. the density is less than 95 % of the theoretical density. If the test specimen has no open porosity, the mass of the dry test specimen m 1is equal to the mass of the soaked test specimen m 3and the apparent solid density is equal to t
29、he bulk density and the apparent porosity is 0. NOTE Open porosity can be recognized if the measured weight value changes during weighing (see 4.3.5). 4.3.2 Determination of mass of dry test specimen Weigh the test specimen in a dry state. If the test specimen has open porosity, dry the test specime
30、n in a drying oven (4.1.1) controlled at 110 C 5 C, allow it to cool to room temperature in a desiccator and weigh. If the test specimen has no open porosity, the specimen can be dried, e.g. with a towel, and weighed. The mass thus determined is the mass of the dry test specimen, m 1 . For the test
31、specimen which may possibly break during boiling, determine the mass of the dry test specimen after the apparent mass of the immersed test specimen and the mass of the soaked test specimen have been determined. 4.3.3 Boiling method (method A) Immerse the test specimen in the heating apparatus (4.1.3
32、) taking care that the test specimen is covered with water at all time, boil for 3 h or more and allow to cool to room temperature. Water at ambient temperature may be used to cool the test specimen to room temperature. In this way the soaked test specimen is obtained. The boiling method shall not a
33、pply to materials that react with water. In the boiling method, an organic liquid shall not be used as the immersion liquid if the liquid vapours are explosive and toxic. 4.3.4 Vacuum method (method B) Place the test specimen in an airtight container (see 4.1.8), evacuate to a pressure of less than
34、2,5 kPa and maintain it for 15 min in order to remove all the air from the open pores of the test specimen. Introduce the immersion liquid (4.1.5) so that the test specimen is covered completely. Gradually release the vacuum to atmospheric pressure and allow the test specimen to remain in the immers
35、ion liquid for an additional 30 min. During the introduction of the immersion liquid, the vacuum pump shall be in continuous operation and be stopped upon completion of the introduction. ISO 2013 All rights reserved 3 ISO 18754:2013(E) For materials that react with water, a suitable organic liquid s
36、hall be used as the immersion liquid. In this case, the organic immersion liquid should be low volatile and nontoxic. The vapour pressure of the organic immersion liquid shall be less than 2,5 kPa at the temperature of the test. NOTE Distilled paraffin and dibutyl phthalate may be used. 4.3.5 Determ
37、ination of apparent mass of (if necessary immersed) test specimen Place the test specimen in the halter or basket (4.1.6) and suspend the basket in the immersion liquid using the thin wire (4.1.7). Using the balance (4.1.2), measure the suspended mass while completely immersed in the immersion liqui
38、d. Remove the specimen from the halter or basket and reweigh the halter or basket when immersed in the immersion liquid to the same depth as when the test specimen was in place. Subtract the apparent mass of the immersed halter or basket from that when it contained the test specimen. The mass thus o
39、btained is the apparent mass of the immersed test specimen, m 2 . Determine the temperature of the immersion liquid using the thermometer (4.1.4). 4.3.6 Determination of mass of soaked test specimen If the test specimen has no open porosity, the mass of the dry test specimen m 1is equal to the mass
40、of the soaked test specimen m 3 . The following procedure shall only be carried out if the test specimen has open porosity, i.e. the density is less than 95 % of the theoretical density. Remove the test specimen from the liquid, sponge it rapidly and carefully with a wet absorbent cloth such as a ga
41、uze or chamois leather, to remove droplets of the immersion liquid from the surface of the test specimen and weigh it. The mass thus obtained is the mass of the soaked test specimen, m 3 . The absorbent cloth or the chamois leather shall previously have been completely saturated with the immersion l
42、iquid and lightly wrung out in order to avoid drawing out the liquid from the pores of the test specimen. 4.3.7 Determination of the density of the immersion liquid Determine, to the nearest 1 kg/m 3 , the density 1of the liquid used as the immersion liquid at the temperature of the test. For water,
43、 the density is given in Table 1 as a function of temperature between 10 C and 30 C. For an organic liquid, use the method given in ISO 758. Table 1 Density of water as a function of temperature between 10 C and 30 C Temperature C 1kg/m 3 Temperature C 1kg/m 3 Temperature C 1kg/m 3 10 11 12 13 14 15
44、 16 999,7 999,6 999,5 999,4 999,2 999,1 998,9 17 18 19 20 21 22 23 998,8 998,6 998,4 998,2 998,0 997, 8 997, 5 24 25 26 27 28 29 30 997, 3 997,0 996,8 996,5 996,2 995,9 995,6 4.4 Accuracy of mass measurement The mass measurement shall be made to the nearest 0,1 mg for a test specimen under 10 g and
45、0,001 % of the mass of a test specimen for a specimen over 10 g.4 ISO 2013 All rights reserved ISO 18754:2013(E) 4.5 Expression of results 4.5.1 Apparent solid density The apparent solid density is the ratio of the mass of the dry material to its apparent solid volume and is given by Formula (1). Th
46、e density shall be calculated to the second decimal place. a m mm 1 12 1(1) where a is the apparent solid density, expressed in kilograms per cubic metre; m 1 is the mass of the dry test specimen, expressed in kilograms; m 2 is the apparent mass of the immersed test specimen, expressed in kilograms;
47、 1 is the density of the immersion liquid at the temperature of the test, expressed in kilograms per cubic metre. 4.5.2 Bulk density The bulk density is given by Formula (2). The density shall be calculated to the second decimal place. b m mm 1 32 1(2) where b is the bulk density, expressed in kilog
48、rams per cubic metre; m 3 is the mass of the soaked test specimen, expressed in kilograms. 4.5.3 Apparent porosity The apparent porosity is the ratio of the volume of the open pores in a body to its bulk volume and is given by Formula (3). The porosity shall be calculated to the first decimal place.
49、 a mm mm 31 32 100 (3) where a is the apparent porosity, expressed as a percentage by volume. 5 Determination of geometric bulk density by measurement of dimensions and mass (method C) 5.1 Principle A test piece of uniform geometry within specified tolerances is dried and weighed. Its volume is determined by measurement of the appropriate dimensions. The geometric bulk density (see 3.9) is calculated as mass per unit volume. ISO 2013 All rights reserved 5 ISO 18754:2013(E) 5
