JIS-Z-3197-1999-R2004-ENG.pdf

STD-JIS Z 3397-ENGL 3779 I 4933608 0563385 57T JIS JAPANESE I N D U STR IAL STANDARD Translated and Published by Japanese Standards Association Testing methods for soldering fluxes ICs 25.160.50 Descriptors : soldering, fluxes (materials), resins (natural), corrosion tests, sampling methods testing Reference number : JIS Z 3197 : 1999 (E) 29 S Z 3197 : 1999 Foreword This translation has been made based on the original Japanese Industrial Standard revised by the Minister of International Trade and Industry through deliberations at Japanese Industrial Standards Committee in accordance with the Industrial Standardization Law. Consequently JIS Z 3197 : 1986 is replaced with JIS Z 3197 : 1999. In this revision, IS0 9455, Soft soldering fluxes-Test methods has been basically employed for the purpose of preparing Japanese Industrial Standard conformed with the International Standards, and this Standard has been made in consideration of domestic technological property at the present time. Attention is drawn to the possibility that some parts of this Standard may conflict with a patent right, application for a patent after opening to the public, utility model right or application for registration of utility model after opening to the public which have technical properties. The relevant Minister and the Japanese Industrial Standards Committee are not responsible for identifying the patent right, application for a patent after opening to the public, utility model right or application for registration of utility model after opening to the public which have the said technical properties. Date of Establishment: 1972-11-01 Date of Revision: 1999-03-20 Date of Public Notice in Official Gazette: 1999-03-23 Investigated by: Japanese Industrial Standards Committee Divisional Council on Welding JIS Z 3197: 1999, First English edition published in 2000-05 Translated and published by: Japanese Standards Association 4-1-24, Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN In the event of any doubts arising as to the contents, the original JIS is to be the final authority. O JSA 2000 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 microfilm, without permission in writing from the publisher. Printed in Japan Z 3197 : 1999 Contents Page Introduction . 1 1 2 3 4 5 6 6.1 6.2 7 7 . 1 7.2 7 . 3 7.4 Scope Normative references Definitions Classification of fluxes and components . Classification of testing methods and types of tests General conditions of tests Standard conditions of tests Test piece Test piece and sample Test materials Reagent Apparatus and device . Sampling method . 1 1 1 2 2 6 6 6 6 6 6 6 6 7 . 4 . 1 Resin flux cored solder . 6 7.4.2 Solder paste 7 7.4.3 Liquid flux 7 7.4.4 Solid flux . 7 8 Testing methods . 8 8 . 1 Testing of contents 8 8.1.1 Resistivity test of aqueous solution . 8 8.1.2 Flux content test 9 8.1.3 Test of solid content 10 8.1.4 Activator content test . 11 8.1.4.1 Organic activator content test 11 8.1.4.1.1 Acid value test (resin and organic) . 11 Z 3197 : 1999 8.1.4.1.2 8.1.4.2 Acid value test (aqueous solution) Test of halide activator content 8.1.4.2.1 Potentiometric titration method 8.1.4.2.2 Volhard method (total halide in water-soluble flux) . 8 . 1 . 4 . 2 . 3 Silver chromate paper test (quality of halide) . 8.1.4.2.4 Color reaction method (fluoride content test) . 8.2 Physical characteristic test 8.2.1 Viscosity test 8.2.2 Specific gravity test . 8.2.3 Color number test 8.2.4 Flash point test 8.3 Soldering behavior test . 8.3.1 Flw effect test . 8.3.1.1 Flux expansion method 8.3.1.2 Wetting balance method 8 . 3 . 2 Flux spattering test . 8 . 3 . 2 . 1 8.3.2.2 Flux spattering test of resin flux cored solder Spattering test of liquid flux 8.3.3 Foaming test . 8.4 Corrosion test . 8.4.1 8.4.2 8.5 8 . 5 . 1 8.5.2 Ionic residue test . 8.5.3 Insulation resistance test . 8 . 5 . 4 Voltage-applied moisture resistance test-migration test . Copper plate corrosion test Copper mirror corrosion test . Characteristic test after soldering . Dryness test (evaluation of flux residue viscosity) . Attached Table 1 Corresponding International Standard Attached Table 2 Normative references . 14 17 17 19 21 23 23 23 24 24 24 24 24 24 26 30 30 31 32 34 34 38 39 39 42 44 47 51 51 JAPANESE INDUSTRIAL STANDARD JIS Z 3197 : 1999 Testing methods for soldering fluxes Introduction This Japanese Industrial Standard specifies the fluxes for soldering used in electronics and communication equipments, etc. The first edition was is- sued in 1972 and then being revised several times afterward. The fluxes for soldering used in electronics implementation require reliable per- formance, quality and reliability after application, and severe quality on products. IS0 specified the testing methods relating to quality included those contents as IS0 9455 Soft soldering fluxes-Test methods, and have established Part-1, 3, 5, 6, 13, 14, 15 in sequence. This Standard is the revised Japanese Industrial Standard to conform with the International Standard on mainly fluxes for soldering used in electronic and electri- cal equipments, and has added the items not specified in the corresponding Interna- tional Standard. The items, viscosity test, specific gravity test, color number, flashing point test, and foaming test and ionized residual, are not included in the corresponding stan- dard. 1 Scope This Japanese Industrial Standard specifies the testing method for sol- dering fluxes (hereafter referred to as “flux”) mainly used for wiring electric equip- ments, electronic equipments, communication equipments, and parts and components of these equipments. Remarks : The corresponding International Standards to this Standard are listed in Attached Table 1. 2 Normative references The standards shown in the Attached Table 2 contain provisions which, through reference in this text, constitute provisions of this Stan- dard. The most recent edition of those normative references shall apply. 3 Definitions The main terms in this Standard shall be those specified in JIS Z 3001 and others shall be as follows. resin type flux and activated rosin, etc. The soldering flux based on resin such as rosin (colophony) organic type flux The soldering flux based on organic acid. There are two types; one is water-based flux added with various organic activators and the other is alcohol or other solvents based flux added with organic activators. inorganic type flux The fluxes based on water-soluble materials such as glyc- erin, polyethylene glycol, polyoxyethylene glycol, etc. and based on non-water- soluble materials such as wax, Vaseline, etc. Those have strong active power by inorganic acid and inorganic salt, but their residuals have strong corrosive- ness. halide content Activator content determined as chlorine, which is added by mixing or by chemical method to improve solderability of flux. Bromine and iodine also apply. -,-,- STD.JIS Z 3297-ENGL 1777 4933b08 05b3290 937 I 2 Z 3197 : 1999 I 2. Synthetic resin purified water Distilled water and ion exchanged water with specific resis- tivity of 5 O00 a m or over at 20 “C. I 2. Amine halide synthetic resin Resins such as organic ester of pentaerythritol, derivatives of phenol or creosol, styrene-maleic acid resin, acrylic resin. Most of them can be used for extreme low residual flux. 1. Resin dewetting State of molten brazing filler metal or solder in which, after wet- ted with a base metal, it is contracted to burst open. One of the failed solder- ing. solder paste Pasty flux suspended with solder powder and flux. Various com- ponents have been mixed to prevent the both from separating, and to produce proper viscosity, thixotropy and printability. a. Denatured rosin 4 Classification of fluxes and components The classification and compositions of fluxes to be covered by this Standard are shown in Table 1. Table 1 Classification and composition of fluxes 3. Inorganic Class I Main component 1. Rosin (Colophony) a. Water-soluble a. Ammonium halide b. Zinc halide c. Tin halide b. Non-water-soluble d. Phosphoric acid e. Hydroacid halide Components Activation 1. No activator added 1. Water-base 2. Organic 2. Solvent-base 3. Organic acid, organic acid salt of amine Fluoride F. (contained) N. (not contained) Form A. Liquid B. Solid C. Paste 5 Classification of testing methods and types of tests The testing methods of flux shall be classified into contents test, physical performance test, behavior at soldering, corrosive test and performance after soldering, etc. and the kinds of methods shall be 24 as shown in Table 2. -,-,- STD=JIS Z 3197-ENGL 1999 . M 4933608 05b3191 . Y U L 3 .- : E V V m R n N - 4 2 m Y Y m C e m - ri o m 4 J m e% x s N 2; rl STD-JIS Z 3197-ENGL 1999 b 4933608 U5b3193 b4b = 5 Z 3197 : 1999 m m m a Y 8 2 $ J 3 1 O 3 3 lo 3 1 I 3 3 U O f z m M E : a m .- - U m Y I _ g m fi 8 E fi E o fi a a V i Y a Y o 4 . 3 O a c d Q Li a V U - o 4 Y m Y Y a l Y m m : ,“ ci 4 STD-JIS Z 3177-ENGL 1799 6 Z 3197 : 1999 6 General conditions of tests 582 m 6.1 Standard conditions of tests The test shall, unless otherwise specified, be conducted under conditions of temperature 20 “C class 15 (k 15 OC) and relative hu- midity 65 % class 20 (h 20 %) specified in JIS Z 8703. However, in the case of dis- agreement on the judgment of the measured values under the standard conditions, the test shall be made at temperature 20 “C class 2 ( f 2 OC) and 65 % class 5 ( f 5 %) as specified in JIS Z 8703. 6.2 Test piece Unless otherwise specified, 3 pieces of specimen shall be prepared and tested for each test item, when the test is to be made on test piece. 7 Test piece and sample 7.1 3283, solder paste, liquid flux and solid flux specified in JIS Z 3284. Test materials The test materials shall be the resin flux specified in JIS Z 7.2 Reagent Reagents are as follows. a) Acetone specified in JIS K 8034 b) 2-propanol (isopropyl alcohol) specified in JIS K 8839 7.3 Apparatus and device a) Soxhlet extractor b) c) Hot plate adjustable to temperature (200 f 5) “CI Thermoregulator adjustable to temperature (100 h 5) “CI d) Ordinary laboratory apparatus 7.4 Sampling method The sampling method of test materials shall be those speci- fied in Table 2 and sample shall be taken as shown below. 7.4.1 Resin flux cored solder Resin flux cored solder shall be sampled as follows. a) Product itself Use the dried product itself as test piece after washing the sur- face with acetone and rinsing first with purified water and then with 2-propanol. 25 mass % 2-propanol solution About 150 g of resin flux shall be cut off and the both ends shall be sealed after crushed. Clean the surface with cloth con- taining acetone. Putting the piece into a beaker and pour enough purified water, and boil it for about 5 to 6 min. Dry it after rinsing with acetone. Cut the piece into slices of about 2 to 3 mm thickness by razor or scissors without dam- aging the cut face and the surface. The both sealed ends shall be destroyed. Put the slices into the clean pipe of Soxhlet extractor and extract with 2-pro- pano1 or appropriate solvent (1) until the recovered condensate becomes trans- parent. The flux extract poured in a beaker shall be evaporated and dried in a thermoregulator at (100 k 5) “C. Then the flux test solution shall be adjusted to have precise 25 mass % of solid contents with solvent used at extraction. Note (1) At extraction or adjustment of flux test solution, if the flux can not dissolve in 2-propanol, appropriate solvent miscible with purified wa- ter shall be used. b) 4 -,-,- STD-JIS Z 3197-ENGL 1994 = 4933608 0563395 419 W 7 Z 3197 : 1999 7.4.2 Solder paste Solder paste shall be sampled as follows. a) Product itself Take the product itself as a sample, and use it after stirring several times to make it homogeneous. b) Pasty fluxes If the user requires assessing only the flux in the pasty flux, the same flux in the solder paste shall be obtained from the manufacturer. If the flux can not be obtained, the following procedures shall be applied to extract the flux from the solder paste. After measuring the tare mass of a 300 ml beaker I (Wz), put (100 * 2) g of the soldering paste (W,) with 0.1 g accuracy. Add 100 ml of 2-propanol or appropriate solvent(? into the beaker and boil it for about 3 min on a hot plate of (150 f 5) OC, stirring with a glass bar to prevent it from bump- ing. After keeping it stationary for about 1 min, filter the solution through coarse filter paper and pour the warm supernatant liquor into a 300 ml beaker II, whose mass of tare has been weighted. There is no need to filter the whole solution and the filtered liquor may not be clear. Further, the above extraction proce- dure shall be repeated until the extraction becomes colorless, and the extraction shall be done with 30 ml of 2-propanol or other appropriate solvent(2). The bea- ker shall be heated in a thermoregulator at (100 k 5) O C in 20 min or more until the residual in the beaker will be completely dried, evaporating the solvent from the beaker. Weighing the mass of the beaker, evaporation shall be repeated to have a specified mass. The extracted mass of flux (W3) shall be calculated from the formula (1). (1) F = Wi - (W3 - Wz) where, F : mass of extracted flux (g) Wi : mass of solder paste sampled (g) W 2 : mass of beaker I (g) W3 : mass of beaker I, containing powder of solder (g) Then, the beaker II containing the extract shall be heated on a hot plate to evaporate the solvent until to have flux quantity (F) of formula (i). The non- volatile residual shall be taken as pasty flux in the solder paste. Note (2) At the extraction or making solution of flux, if the flux can not dis- solve in 2-propanol, appropriate other miscible solvent shall be used. 7.4.3 Liquid flux Liquid flux shall be sampled as follows. a) Product itself Product itself shall be used as specimen. 7.4.4 Solid flux Solid flux shall be sampled as follows. a) Product itself Product itself shall be used as specimen. b) 25 mass % 2-propanol solution Using 2-propanol or other appropriate sol- vent(3), flux specimen solution of 25 mass %, containing solid part shall be pre- pared. Note (3) At the extraction or making solution of flux, if the flux can not dis- solve in 2-propanol, appropriate other miscible solvent shall be used. -,-,- 8 Z 3197 : 1999 8 Testing methods 8.1 Testing of contents 8.1.1 Resistivity test of aqueous solution Resistivity test of aqueous solution shall be as follows. This test is to be carried out to determine the mass of conduc- tive materials in flux, and specifies the procedure of measuring resistivity of extracted water from a solution containing a certain level of