Process Control Verification to Prevent Hydrogen Embrittlement in Plated or Coated Fasteners - An Introduction to ASTM Standard Test Method F1940 J. Barton Boodey, Ph.D., RSL Technology Center, Inc., Richboro, PA An ASTM F16.93 task group of industry experts was established to investigate the use of an alternate process control method using the incremental step loading (ISL) technique per ASTM F1624. The result of this task group was Standard Test Method F1940 which allows the quantitative statistical evaluation of finishing processes for damage from internal hydrogen embrittlement (IHE). Any process can be evaluated on a periodic basis with specimens as compared to qualifying each lot of fasteners being plated or coated. The test method consists of a mechanical test for the evaluation and control of the potential for IHE that may arise from various sources of hydrogen in a process. A complete discussion of the standard and its supporting data will be presented. For more information contact: Bart Boodey RSL Technology Center, Inc. 975 Second Street Pike Richboro, PA 18954 Phone: 215/357-8111 Fax 215/357-5887 e-mail Jbboodey@aol.com 707708 Introduction. An ASTM F16.93 task group. made up of industry experts, was established to investigate the use of an alternate process. control method using the incremental step loading (ISL) technique per ASTM F1624. ‘The result of this task group was ASTM Standard Test Method F1940 entitled: “Process Control Verification to Prevent Hydrogen Embrittlement in Plated or Coated Fasteners’. This method allows the quantitative statistical evaluation of finishing processes for damage from internal hydrogen embrittlement (IHE). This standard 1s intended to be used as a qualification test for new or revised plating or coating processes and as a_ periodic inspection audit for the control of a plating ‘or coating process. Summary of Test Method ‘The purpose of this process control method 1s to prevent, to the extent possible, internal hydrogen émbrittlement (IHE) of fasteners by monitoring the plating or coating process. This method applies to externally threaded tensile fasteners that can also be loaded in bending during installation and is limited to evaluating hydrogen induced embrittlement due only to processing (HE) and not due to environmental exposure (EHE). in addition, the method is limited to ferrous fasteners that are susceptible to time- delayed fracture caused by the diffusion of hydrogen under stress. The process is quantitatively monitored on a periodic basis with a minimum number of specimens as compared to qualifying each lot of fasteners being plated or coated. Trend analysis is utilized to ensure quality as compared to statistical sampling analysis of each Jot of fasteners. This test method consists of a mechanical test for the evaluation and control of the potential for IHE that may arise from various sources of hydrogen in a plating or coating process. This method uses a notched square bar specimen that conforms to ASTM F519, Type le, except that the ‘radius is increased to accommodate the deposition of a larger range of platings and coatings, Figure 1 ‘These specimens are of a fixed geometry, certified to have been heat treated to a hardness range of 50-52 HRC, and certified to exhibit sensitivity to embrittlement from trace amounts of residual hydrogen in steel will be processed with actual parts. The unstressed test specimens are processes with fasteners in accordance with the specified process being qualified. The specimen is then tested under incremental step load in four point bending. The test is, an accelerated (<24h) method that measures the threshold for hydrogen stress cracking that is used to quantify the amount of residual hydrogen in the specimen. ‘Terminology To aid in the use of the standard, a Uist of terms used is provided which includes: Process ...A defined event or sequence of events which may include pretreatments, plating or coating, and post treatments that are being evaluated or qualified. THE ... Internal Hydrogen Embrittlement - Test conducted in alr Embrittlement due to residual hydrogen from processing. EHE Environmental —_ Hydrogen Embrittlement - Test conducted in a specified environment - Embrittlement due to hydrogen introduced into steel from external sources. NFS(B) ... Notched fracture strength in air of a bare specimen in bending at loading rates of 50 to 250 ksi/min (850 to 1700 MPa/ min) NFS(B)r1624 ..- Notched fracture strength in air ofa bare specimen in bending at ASTM F1624 step loading rates. Threshold ... The maximum load at the ‘onset of cracking that 1s Identified by a 5% drop in load of NSF(BIF1624 under displacement control. ISLth ... threshold from an incremental step load test on a plated or processed specimen.Test Specimen ‘The proper manufacture of the test ‘specimens is critical to the success of this test method. The test specimen is a 0.4W- Notched Square Bar Bend Specimen: 0.4W- SqB(B), as shown in Fig. | and is made from AISI 4340 steel per AMS 6415. The notch 1s in the LS-orientation and has a stress concentration factor of Kt=3.1 20.2. Each test specimen blank is heat treated per AMS 2759 to meet the hardness Fequirement of 50HRC - 52HRC. The surface finish of the notch is 16 RMS or better with the other surfaces at 32 RMS or better S\or= | t All dimensions except for the length are produced after quenching and tempering to final hardness. The 0.40" (1mm) dimension 1s produced by ‘low stress grinding The notch is first rough machined by wire EDM to within 0.020" (0.5 mm) of the final notch depth and then low stress ground to the final depth. No chemical or mechanical cleaning is allowed after final machining and straightening after final heat treatment is prohibited. Prior to plating or coating, all specimens are protected during storage to prevent corrosion. A suitable means of protection is to coat the specimen with a corrosion preventive compound. 0.40" (10 mp 726 9a" amare ae qo Adjacent Sites erro _—_ + 4, 7-1 0.40" (10 mm) aha Fe F varosem J Se eae ous (6mm) ‘Tolerances unless otherwise ee ot ian a2 mm) 30, $0.01 meh (20-2 mam) {700K 20.007 inch (20.02m0m) “” we oar o>mm Fig. 1. Dimensional Requirements for a 0.4W-Notched Square Bar Bead Specimen. 709710 Lot and Sensitivity Testing The uniformity of specimens and their mechanical properties and sensitivity to IHE must be demonstrated for each lot of specimens. A lot consists of only those specimens cut from the same heat of ste! in the same orientation. heat treated together in the same furnace, quenched and tempered together, and subjected to the same manufacturing processes. The inspections are conducted prior to the purchase of the specimens by the manufacturer. A certification report for each lot is required. The specimens are considered suitable for test purposes if the ‘sampling and inspection results conform to the requirements in Tables 1 and 2. TABLE 1 Lot Acceptance Criteria for 0.4W- Notched Square Bar Bend Specimens. Sampling Item of Each Requirement /Method Lot Hardness* 5% | SOHRC - 52HRC per ASTM E18. Round the average of three readings per imen per ASTM E29. Dimensions | 100% | Meet tolerances of corresponding drawings. Notch dimension verified with shadow graphie projection at 50x to 100x. Notched Fracture} 10¢a _| NFS(B) of each specimen must be Strength in within #5% of the average. Bending, NFS(B ) "If the hardness requirements of any of je sampled specimens are not satial . only those specimens of the lot that are individually inspected for conformance to these requirements shall be used for testing. ‘Table 2 Sensitivity Test Requirements of Specimens. Bare in air ‘h specimen tested shall have shold =85% of the average notched nd fracture strength, NFS(B) {Table 1}.| vs SCE tn 3.5% NaCl [Solution in D1193 Type TV Reagent Water reshold < 50% of the average notched Bare @ potential of -1.2V fies specimen tested shall have id fracture strength NFS(B) {Table 1}.Process Control Testing ‘The specimens, as received. are processed and qualified with the fasteners. It 1 important that the specimens be exposed to the same process as the fasteners, for the test to be valid. Even if the fasteners do not require a degreasing and cleaning process prior to plating or coating, the specimens are to be degreased to remove the corrosion preventive ‘compound and then cleaned in acetone and placed in the process with the fasteners. An application guideline, to be used as a template for the use of this standard, 1s provided in Appendix X2 of ASTM F1940. After the specimens have _ been processed, incremental step loads and hold times under displacement control are used to detect the onset of subcritical crack growth, or threshold that is used to quantify the amount of restdual hydrogen in a specimen. A specific incremental step load and holding time protocol in accordance with ASTM F1624_—_ is prescribed, (Table 3). Instrumented testing equipment with “adjustable constant displacement loading is required as described in both ASTM F1624 and F1940. To measure the threshold, ISLth-air- of a plated 0.4W-SqB(B) specimen, the plated notched bend specimens are tested in air in four point bending under displacement control at_ ASTM F1624 loading rates (Table 3). The threshold is the maximum load at the onset of cracking. The onset of cracking is defined as a 5% drop in load with respect to NFS(B)F1624 under displacement control, ‘Table 9 Minimum requirements fora step loading profile for accelerated (s24h) Joad_ threshold determination. Optional Limits Since embrittlement related to hydrogen content varies with hardness and other composition, actual fasteners made of low-strength steel_might have more tolerance for residual hydrogen due to the process and might not need the rigorous Tequirement set forth in this standard for threshold. Therefore, adjustments in threshold requirements can be made once a correlation is established. As an example, NFSroce HR Th |YNFSro2 AH Th |NESyore AR Th 10 1 ij 6 18 Es 115 20 12 7 19 20 116 20 13 2 110 6 17 40 14 74 tou 100 118 50. 15 B 1 105, 119 55, 16 3 1_1s]|__ 110 120 o 17 i o Low a threshold of less then 75% of the fracture strength, which is not necessarily hydrogen free can be considered adequate for many applications of lower strength steels. To obtain this correlation between actual production fasteners and threshold levels in this standard, the threshold level or hydrogen tolerance level for the production fasteners can be measured using ASTM F1624._— An example of an ‘adjustment to the threshold is shown in the ASTM F1940's Appendix X1. 7mne Interpretation of Results If the threshold in air of the specimen is 2 75% NFS(B)F1624, then the process is considered as to not produce sulflicient hydrogen to induce time delayed THE failures in the plated or coated fasteners. If the threshold in air of the specimen is < 75% NFS(B)F1624. then the process 1s considered potentially embrittling If any test results are marginal or suspect, ie < 75% NFS(B)F 1624. the actual product lot can be tested in accordance with ASTM F1624 to determine if the threshold of the actual fastener 1s 2 90% of the bend ultimate strength of the fastener. Again Appendix X1 of ASTM F1940 illustrates how fasteners can be tested in four point bending to determine this threshold value. Summary The efforts of an ASTM F16.93 task group has resulted in anew ASTM standard for process control verification to prevent hydrogen embrittlement in plated or coated fasteners. ‘The test method utilizes an accelerated (s24h) step loading protocol with certified test specimens that measures the threshold for hydrogen stress cracking which Is used to quantify the amount of residual hydrogen co-deposited during the processing. ‘The standard was designed to allow for optional limits for fastener materials that are known to be less sensitive to IHE. This provision will allow these materials to be processed in lines with thresholds lower than 75%. Sensitive and high strength fasteners would then be processed only in lines exhibiting process control at thresholds greater than 75% to ensure the potential for IHE is minimized.