SAE AS 6171 10-2016 Techniques for Suspect Counterfeit EEE Parts Detection by Thermogravimetric Analysis (TGA) Test Methods.pdf

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1、_SAE Technical Standards Board Rules provide that: “This report is published by SAE to advance the state of technical and engineering sciences. The use of this report is entirelyvoluntary, and its applicability and suitability for any particular use, including any patent infringement arising therefr

2、om, is the sole responsibility of the user.”SAE reviews each technical report at least every five years at which time it may be revised, reaffirmed, stabilized, or cancelled. SAE invites your written comments and suggestions.Copyright 2016 SAE InternationalAll rights reserved. No part of this public

3、ation may be reproduced, stored in a retrieval system or transmitted, in any form or by any means, electronic, mechanical, photocopying,recording, or otherwise, without the prior written permission of SAE.TO PLACE A DOCUMENT ORDER: Tel: 877-606-7323 (inside USA and Canada)Tel: +1 724-776-4970 (outsi

4、de USA)Fax: 724-776-0790Email: CustomerServicesae.orgSAE WEB ADDRESS: http:/www.sae.orgSAE values your input. To provide feedback on thisTechnical Report, please visithttp:/standards.sae.org/AS6171/10AEROSPACESTANDARDAS6171/10Issued 2016-10Techniques for Suspect/Counterfeit EEE Parts Detection by Th

5、ermogravimetric Analysis (TGA) Test MethodsRATIONALEThis method was created to provide guidance for those unfamiliar with TGA towards its application to the detection of counterfeit electronic parts. Additionally this document is intended to provide guidelines for the application of TGA and to defin

6、e the compliance requirements for laboratories using this technique.INTRODUCTIONThermogravimetry is a method in which the sample is exposed to a precisely controlled temperature environment while continuously monitoring weight change. TGA provides a relatively fast means to identify gross difference

7、s (filler content, compositional percentages, temperatures at which various constituents volatilize, etc.) between parts and thus determine if an unknown part is suspect counterfeit. The sample can be a liquid or a solid and weight change can be measured either during controlled heating or while the

8、 sample is maintained at a constant temperature (isothermal period). Weight loss occurs due to decomposition or loss of volatile constituents within the sample; decomposition occurs at unique temperatures, thus TGA can provide an indirect compositional analysis of the sample. Additionally, this tech

9、nique can determine the amount of volatile matter within a material, the class of volatile matter as defined by the temperature at which the matter volatilizes, the amount of combustible material within a material, and the ash or filler content of a material.In the context of counterfeit detection t

10、his method can allow for direct comparison of the composition of one sample against another. This will be particularly useful when authentic samples or standards are available for comparison purposes. To cite a few examples, TGA can provide compositional comparison of solid materials, such as plasti

11、c encapsulation from integrated circuits, or liquid materials, such as, electrolyte saturated paper from within an electrolytic capacitor. TGA can also be used to analyze the composition of oils within a transformer or the volatilization of lubricants from a bearing.Additionally, it can be used to d

12、etermine the moisture content within a polymer. Testing per this method could range from completely non-destructive, if testing an entire device within its rated temperature range to mostly destructive, if removing a large section of the DUT as a sample, as in the case of the electrolyte from a capa

13、citor.SAE INTERNATIONAL AS6171/10 Page 2 of 18TABLE OF CONTENTS1. SCOPE 42. REFERENCES 42.1 Applicable Documents 42.1.1 SAE Publications. 42.1.2 ASTM Publications 42.1.3 Other Publications. 42.2 Terms and Definitions . 52.3 Acronyms 53. EQUIPMENT AND OTHER SUPPLIES 53.1 Thermogravimetric Analyzer .

14、53.2 Other Equipment. 53.3 Preparatory Equipment . 54. TEST SAMPLE . 65. MATERIALS HANDLING, STORAGE, AND SAMPLE PREPARATION 66. DESCRIPTION OF METHODOLOGY 76.1 Compositional Analysis. 76.2 Highly Volatile Material Content Analysis . 86.3 Thermal Stability Analysis. 86.4 Other Analysis. 87. CONTROLS

15、 AND CALIBRATION 88. ANALYSIS AND INTERPRETATION OF DATA. 98.1 Compositional Analysis. 108.1.1 Weight Loss 108.1.2 Onset Temperature. 118.1.3 Combustible Material Content. 128.1.4 Ash/filler Content. 128.2 Highly Volatile Material Content Analysis . 128.3 Thermal Stability Analysis. 139. REPORTING O

16、F RESULTS . 1410. QUALIFICATION AND CERTIFICATION . 1410.1 Personnel Qualification . 1410.1.1 Level 3 - Advanced Interpretation (Typically an Engineer or Scientist) 1410.1.2 Level 2 - Basic Interpretation (Typically a Technician) . 1510.1.3 Level 1 - Operation (Typically an Operator) 1510.2 Safety 1

17、511. NOTES 1511.1 Revision Indicator 15APPENDIX A EXAMPLE OF APPLICATION OF TGA FOR COUNTERFEIT DETECTION 16SAE INTERNATIONAL AS6171/10 Page 3 of 18FIGURE 1 DIRECT COMPARISON OF DATA 9FIGURE 2 COMPOSITIONAL ANALYSIS . 11FIGURE 3 ONSET CALCULATION 11FIGURE 4 THERMAL STABILITY ANALYSIS . 13TABLE 1 REF

18、ERENCE TEST METHODS. 7TABLE 2 EXAMPLE TGA PROFILE FOR COMPOSITIONAL ANALYSIS 8TABLE 3 EXAMPLE TGA PROFILE FOR VOLATILE MATERIAL CONTENT ANALYSIS. 8TABLE 4 EXAMPLE TGA PROFILE FOR THERMAL STABILITY ANALYSIS . 8TABLE 5 REQUIRED TEST REPORT INFORMATION. 14SAE INTERNATIONAL AS6171/10 Page 4 of 181. SCOP

19、EThis test method provides the capabilities, limitations, and suggested possible applications of TGA as it pertains to the detection of counterfeit electronic components. Additionally, this document outlines requirements associated with the application of TGA including: equipment requirements, test

20、sample requirements, methodology, control and calibration, data analysis, reporting, and qualification and certification.If AS6171/10 is invoked in the contract, the base document, AS6171 General Requirements shall also apply.2. REFERENCES2.1 Applicable DocumentsThe following publications form a par

21、t of this document to the extent specified herein. The latest issue of SAE publications shall apply. The applicable issue of other publications shall be the issue in effect on the date of the purchase order. In the event of conflict between the text of this document and references cited herein, the

22、text of this document takes precedence. Nothing in this document, however, supersedes applicable laws and regulations unless a specific exemption has been obtained.2.1.1 SAE PublicationsAvailable from SAE International, 400 Commonwealth Drive, Warrendale, PA 15096-0001, Tel: 877-606-7323 (inside USA

23、 and Canada) or +1 724-776-4970 (outside USA), www.sae.org.AS6171 Test Methods Standard: General Requirements, Suspect/Counterfeit Electrical, Electronic, and Electromechanical Parts2.1.2 ASTM PublicationsAvailable from ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA

24、19428-2959, Tel: 610-832-9585, www.astm.org.ASTM D972 Standard Test Method for Evaporation Loss of Lubricating Greases and OilsASTM D2288 Standard Test Method for Weight Loss of Plasticizers on HeatingASTM D3850 Standard Test Method for Rapid Thermal Degradation of Solid Electrical Insulating Materi

25、als by Thermogravimetric Method (TGA)ASTM D6370 Standard Test Method for Rubber - Compositional Analysis by Thermogravimetry (TGA)ASTM E1131 Standard Method for Compositional Analysis by ThermogravimetryASTM E1582 Standard Practice for Calibration of Temperature Scale for ThermogravimetryASTM E1868

26、Standard Test Method for Loss-On-Drying by ThermogravimetryASTM E2040 Standard Test Method for Weight Scale Calibration of Thermogravimetric AnalyzersASTM E2550 Standard Test Method for Thermal Stability by Thermogravimetry2.1.3 Other PublicationsIDEA-STD-1010 Acceptability of Electronic Components

27、Distributed in the Open MarketIPC-TM-650, Method 2.4.24.6 Decomposition Temperature (Td) of Laminate Material Using TGAIPC/JEDEC J-STD-020 Moisture/Reflow Sensitivity Classification for Nonhermetic Solid State Surface Mount DevicesSAE INTERNATIONAL AS6171/10 Page 5 of 18IPC/JEDEC J-STD-033 Handling,

28、 Packing, Shipping and Use of Moisture/Reflow Sensitive Surface Mount DevicesJESD-625 Requirements for Handling Electrostatic Discharge Sensitive (ESD) DevicesMIL-STD-883, Method 50112.2 Terms and DefinitionsSee 2.2.5 of AS6171 General Requirements.2.3 AcronymsSee 2.3 of AS6171 General Requirements.

29、3. EQUIPMENT AND OTHER SUPPLIES3.1 Thermogravimetric AnalyzerThis method requires a Thermogravimetric Analyzer that shall consist of:a. A microbalance capable of continuously measuring to the nearest 0.001 mg.b. A furnace capable of heating from room ambient temperature to at least 1000qC. Additiona

30、lly, the furnace must be capable of both maintaining a constant temperature over time and heating at a controlled, constant rate of 0qC/minute to 50qC/minute over the above range.c. A programmable calibrated temperature controlling device capable of operating the furnace throughout the entire desire

31、d TGA profile. The device shall be able to maintain the temperature ramp rate within 0.1qC/minute.d. Temperature sensor or thermocouple.e. A thermally and dimensionally stable, nonreactive sample holder (typically platinum or alumina).f. A computer and software capable of recording weight as a funct

32、ion of temperature and time. Time shall be recorded in at least 0.1 minute intervals and temperature in at least 0.1qC intervals.3.2 Other Equipmenta. Inert purge gas (argon, nitrogen, or other gas as recommended by the equipment manufacturer) at least 99.99% pure;b. Reactive purge gas (compressed a

33、ir or oxygen) if performing compositional analysis;c. A gas flow regulator capable of maintaining a constant gas flow within 5 mL/min and, unless the specific test requires only one purge gas, the ability to switch between at least two different purge gases;d. Purge gas drier to remove moisture from

34、 the gas for compressed air.3.3 Preparatory EquipmentClean, non-contaminating preparatory equipment (scalpels, tweezers, pipette, etc.) needed to extract the sample from the DUT.SAE INTERNATIONAL AS6171/10 Page 6 of 184. TEST SAMPLEThe sample can be the entire DUT or a portion of material removed fr

35、om the DUT. The sample can be a liquid or a solid with a typical weight between 10 mg and 30 mg. Sample weight can be as low as 1 mg or as high as the balance allows; however, the sample shall be of sufficient weight to produce a noticeable response on the thermogravimetric analyzer.When comparing m

36、aterials, samples of like weight (within 50% of each other) shall be used. The dimensions of samples being compared should be similar. The samples extracted should be visually of the same composition.NOTE: It is important that samples being compared are extracted in a similar manner to ensure that e

37、ach sample contains the same constituents of the DUT. For instance, when extracting a piece of the epoxy molding compound for a plastic encapsulated component, if the reference sample does not contain the die and bond wires but does contain ink, the DUT sample should likewise contain an equivalent a

38、mount of ink but no die and bond wires.Ideally, the sample should be of a homogenous material and if solid, reduced into small pieces so as to fit into the sample holder. If the sample is ground, care should be taken not to induce excess heat to the sample. Different homogenous materials shall be se

39、parated from the DUT into separate samples, when possible, and tested independently. Liquid materials shall be thoroughly mixed prior to sample extraction. Depending on the need, non-homogenous materials can be tested but will likely require special data analysis. Additionally, when appropriate, liq

40、uid samples may be loaded frozen or in a sealed pan with a small hole pierced in the lid; if frozen, a subambient attachment to cool the furnace to -20qC is recommended.A Level 3 person shall select the procedure applied to liquid samples.Typically, one sample is tested per material; however, averag

41、ing results of multiple samples taken from the same material can provide more precise results.If a material is known to be heterogeneous, and homogeneous samples cannot be extracted (such as when testing a coating on a plastic substrate or electrolyte on paper) and the material is of sufficient size

42、, three heterogeneous samples shall be tested and their results averaged. 5. MATERIALS HANDLING, STORAGE, AND SAMPLE PREPARATIONESD sensitive items shall be handled from receipt to delivery in accordance with ANSI/ESD S20.20 or JESD 625. Moisture sensitive items shall be handled from receipt through

43、 delivery in accordance with the requirements of IPC/JEDEC J-STD-20 and J-STD-033. Refer to the requirements in 3.9.5 of AS6171 General Requirements.NOTE: IDEA-STD-1010 Sections 7.1 and 7.3 provide workstation guidelines.All materials, including samples and sample preparation and analysis devices, s

44、hall be handled according to best lab practices, as applicable (i.e., care taken not to contaminate samples, clean work areas and equipment, etc.).If performing a compositional analysis on a solid, the sample shall be preconditioned. If performing a volatile material content analysis or chemical abs

45、orption analysis, potentially including moisture, the sample shall not be preconditioned. Liquid and semi-solid samples shall not be preconditioned, under any circumstances.If preconditioning is required and the testing is meant to be destructive, the solid samples shall be baked for a minimum of 2

46、hours at 105qC 2qC and then allowed to cool to room temperature for at least hour in a desiccator. If preconditioning is required and the testing is meant to be nondestructive, then the sample shall not be baked above the maximum storage temperature. In the latter situation, the actual preconditioni

47、ng time and temperature shall be selected in accordance with component manufacturer recommendation or by mutual agreement with the user/requester. The sample shall be visually examined before and after drying to ensure no physical change or discoloration occurs. It may be necessary to run both dried

48、 and as received samples.SAE INTERNATIONAL AS6171/10 Page 7 of 186. DESCRIPTION OF METHODOLOGYThe purge gas flow rate and the temperature sensor position shall be maintained as set during the thermogravimetric analyzer calibration. If these are changed since the most recent calibration, the thermogr

49、avimetric analyzer shall be recalibrated.Table 1 lists reference test methods that may be followed in their entirety or modified to suit the sample and goal of the testing. During the analysis the weight loss/gain versus temperature and/or weight loss/gain versus time shall be recorded.Table 1 - Reference test methodsProperties Sample MethodComposition Analysis Solid or Liquid ASTM D3850, ASTM E1131, ASTM D6370, or IPC-TM-65