ISO 17092-2005 Fine ceramics (advanced ceramics advanced technical ceramics) - Determination of corrosion resistance of monolithic ceramics in acid and alkaline.pdf

1、 Reference number ISO 17092:2005(E) ISO 2005INTERNATIONAL STANDARD ISO 17092 First edition 2005-11-01 Fine ceramics advanced ceramics, advanced technical ceramics Determination of corrosion resistance of monolithic ceramics in acid and alkaline solutions Cramiques techniques Dtermination de la rsist

2、ance la corrosion des cramiques monolithiques dans des solutions acides et alcalines ISO 17092:2005(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are em

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5、oblem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2005 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and micro

6、film, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 20

7、05 All rights reservedISO 17092:2005(E) ISO 2005 All rights reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Terms and definitions. 1 4 Apparatus 2 5 Test solutions 2 6 Test specimens . 3 7 Test procedure 3 8 Calculations. 4 9 Test report . 5 Annex A (informative) Gene

8、ral information. 6 Annex B (informative) Interlaboratory evaluation of the test method 7 Bibliography . 9 ISO 17092:2005(E) iv ISO 2005 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The

9、 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-gove

10、rnmental, 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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. T

11、he 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 as an International Standard requires approval by at least 75 % of the member bodies casting a vot

12、e. 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. ISO 17092 was prepared by Technical Committee ISO/TC 206, Fine ceramics. INTERNATIONAL STANDARD IS

13、O 17092:2005(E) ISO 2005 All rights reserved 1 Fine ceramics advanced ceramics, advanced technical ceramics Determination of corrosion resistance of monolithic ceramics in acid and alkaline solutions 1 Scope This International Standard describes the test method for determining the corrosion resistan

14、ce of fine ceramics in acid and alkaline solutions, such as sulfuric acid and sodium hydroxide. This International Standard is designed to provide an assessment of the mass changes and dimensional changes of test specimens following the corrosion test immersed in the corrosive liquids, and to assess

15、 whether corrosion has a significant effect on the subsequent strength. This test method may be used for development of materials, quality control, characterization, and design-data generation purposes. NOTE The units and numerical values given in in this standard are based on traditional units and

16、are appended for information. 2 Normative references 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) appli

17、es. ISO 3611, Micrometer callipers for external measurement ISO 3696, Water for analytical laboratory use Specification and test methods ISO 4287, Geometrical Product Specifications (GPS) Surface texture: Profile method Terms, definitions and surface texture parameters ISO 6353-2, Reagents for chemi

18、cal analysis Part 2: Specifications First series ISO 6906, Vernier callipers reading to 0,02 mm ISO 7500-1, Metallic materials Verification of static uniaxial testing machines Part 1: Tension/compression testing machines Verification and calibration of the force-measuring system ISO 14704:2000, Fine

19、 ceramics (advanced ceramics, advanced technical ceramics) Test method for flexural strength of monolithic ceramics at room temperature 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 corrosion resistance resistance against corrosion of fine

20、ceramic material due to reaction with corrosive species in the surrounding environment, including chemical reactions at grain boundaries and secondary phases ISO 17092:2005(E) 2 ISO 2005 All rights reserved3.2 flexural strength maximum nominal stress at fracture of a specified elastic beam loaded in

21、 bending 4 Apparatus 4.1 Corrosion testing apparatus, for example, any suitable apparatus capable of maintaining the test solution in a quiet boiling state and also maintaining the test solution at a constant concentration The test container shall be made of glass or polytetrafluoroethylene, and sha

22、ll have a capacity of about 1 litre. The test container should be connected to a glass vertical-type condenser, having a sufficient cooling area, by a tapered ground joint. The test apparatus shall be equipped with a thermometer for monitoring the solution temperature. Since the severe boiling state

23、 may cause mechanical damage to test specimens, the “quiet boiling state” is preferable. NOTE 1 A device, such as a basket or a system of suspension wires resistant to the corrosive medium, may be used to prevent contact between test specimens, and to raise them off the bottom of the vessel. Alterna

24、tively, the test specimens may be placed in a PTFE-lined chemical digestion vessel with the reagent, sealed and heated to the required test temperature. If this approach is employed, it shall be recorded in the test report. NOTE 2 “Quiet boiling” refers to the level of bubble (vapour) formation in t

25、he liquid at a low enough level and frequency to eliminate movement of the test specimen. 4.2 Drying device, for example an oven, capable of achieving constant mass of the test specimens by maintaining a temperature of 105 C to 120 C. 4.3 Testing machine for flexural strength, capable of applying a

26、uniform crosshead speed. The testing machine shall be in accordance with ISO 7500-1, with an accuracy of 1 % of the indicated force at fracture. 4.4 Test fixture for flexural strength, of three- or four-point flexure configuration in accordance with 5.2 of ISO 14704:2000. NOTE The recommended fixtur

27、e is fully articulated and of the four-point-1/4 point configuration with the two outer bearings at a distance of 40 mm. The corresponding total length of the test specimen is 45 mm or more. 4.5 Micrometer, such as that shown in ISO 3611 but with a resolution of 0,002 mm for measuring the specimen d

28、imensions. The micrometer shall have flat anvil faces such as those shown in ISO 3611. The micrometer shall not have a ball tip or sharp tip, since these might damage the specimen. Alternative dimension-measuring instruments may be used, provided that they have a resolution of 0,002 mm or finer. 4.6

29、 Vernier callipers, in accordance with ISO 6906, with a resolution of 0,05 mm or finer for measuring the length of the test specimen. Alternative dimension-measuring instruments may be used, provided that they have a resolution of 0,05 mm or finer. 4.7 Balance, with a sensitivity of at least 0,1 mg.

30、 5 Test solutions Sulfuric acid or sodium hydroxide solution is used for the test solution. For sulfuric acid solution, prepare the solution of 3 mol/l 6 N concentration with guaranteed reagent as specified in ISO 6353-2, and distilled water or demineralized water as specified in ISO 3696. For sodiu

31、m hydroxide solution, prepare the solution of 6 mol/l 6 N concentration with guaranteed reagent as specified in ISO 6353-2 and distilled water or demineralized water. For solutions other than sulfuric acid and sodium hydroxide, prepare the solution of which the concentration becomes 3 mol/l. It is r

32、ecommended to use the solution volume of 0,5 litre for each corrosion test. ISO 17092:2005(E) ISO 2005 All rights reserved 3 SAFETY PRECAUTIONS Appropriate safety precautions must be employed when preparing and handling these solutions. 6 Test specimens The test specimen for the corrosion test shall

33、 be prepared in accordance with Clause 6 of ISO 14704:2000. The standard test specimens shall have cross-sectional dimensions of 3,00 mm 0,20 mm thickness, and 4,00 mm 0,20 mm width. The length shall be more than 35 mm for 30 mm test fixtures or more than 45 mm for 40 mm test fixtures. All the surfa

34、ces shall be machined, and the surface roughness shall be not more than 0,2 mRa as defined in ISO 4287. Edges shall be rounded or chamfered. Any machining procedure and the surface quality of the test specimens shall be reported. The minimum number of test specimens shall be 10 for each corrosion co

35、ndition to be tested, and at least 10 test specimens shall be used for flexural strength measurements before the corrosion test. Means shall be taken to identify individually similar test specimens, but shall not be marked or scribed in a way that might affect the result of the test. If strength cha

36、nges are not to be determined, any test specimens in terms of size and shape may be used. NOTE A graphite pencil mark may be a suitable means of marking test specimens of most types. 7 Test procedure 7.1 Measurements of dimensions and mass of specimens Measure the width (b) and thickness (h) of each

37、 test specimen at several places using the micrometer (4.5) with a resolution of 0,002 mm. Measure the overall length (L T ) with the vernier callipers (4.6) with a resolution of 0,05 mm. For other shapes of test specimen, measure relevant dimensions at several different places (e.g. diameter and th

38、ickness of a disc). Wash and degrease the test specimens. Place in the oven (4.2) and heat to a temperature of 105 C to 120 C until their mass is constant. Remove and store in a desiccator. When cooled to room temperature, weigh each to the nearest 0,1 mg using the balance (4.7). Store in the desicc

39、ator until tested. NOTE For the majority of fine ceramics (advanced ceramics, advanced technical ceramics), the washing and degreasing conditions have little effect on the subsequent corrosion properties, and water and solvents are removed by the subsequent oven treatment. However, some materials, e

40、.g. boron nitride or beta-alumina, may be influenced by any washing process. Care should be taken to ensure that any cleaning process used does not affect the results of the corrosion test. 7.2 Corrosion test Heat the test container (4.1) filled with test solution to a quiet boiling state. Then plac

41、e the test specimens gently on the bottom of the container and maintain the boiling state continuously for 24 h. The test specimens allowed in a single container are of the same material and the maximum number of test specimens is ten. New test solution shall be used in every test. After conducting

42、the corrosion test, take the test specimen out from the test container, and wash sufficiently with distilled or demineralized water. Dry at 105 C to 120 C until constant mass is achieved, and transfer to a desiccator quickly. NOTE Appropriate care must be taken when opening the vessel and inserting

43、the test specimens to avoid splashing. 7.3 Measurements of mass and dimensional changes Weigh the test specimens individually to the nearest 0,1 mg. If appropriate, remeasure the external dimensions of the test specimens for the determination of dimensional changes. NOTE The accuracy of re-measureme

44、nt of specimen dimensions will depend on the nature and extent of the corrosion, particularly the degree of pitting or of skin formation. For materials which corrode badly, it may not be possible to obtain accurate dimensional data using the micrometer. It may be more appropriate to determine a resi

45、dual unaffected specimen cross-section by studying a polished cross-section by microscopy. ISO 17092:2005(E) 4 ISO 2005 All rights reserved7.4 Measurements of flexural strength Measure the flexural strength of the corroded and the control test specimens in accordance with ISO 14704. If the nature of

46、 the corroded surface has to be changed in order to undertake the strength tests, this shall be reported in the test report. A fully articulating fixture (4.4) should be used for flexural strength measurements of the corroded specimens because they may not meet the parallelism requirements in ISO 14

47、704 for use of a semi-articulating fixture. NOTE A semi-articulating fixture may be used if the post-corrosion parallelism requirements are satisfied. 7.5 Particular features Record any particular features associated with the condition of the corroded surfaces, the appearance of fractured cross-sect

48、ions, etc. NOTE Microstructure observation of the corroded layer in the cross-section using scanning electron microscopy and analysis of the corroded layer using an electron probe micro-analyzer may be useful characterization methods. Measurements of dissolved elements in test solutions may also be

49、useful. 8 Calculations 8.1 Flexural strength Use the appropriate calculation procedures in ISO 14704 to determine the average strength and standard deviation for the control batch and for each corrosion test. Report average and standard deviations of the strengths along with test-fixture specifics (e.g. the outer and inner spans and whether semi-articulating or fully articulating). 8.2 Mass change Compute the mass change per unit nominal surface area of the test specimen (C) in accordance with the formu