NIL-C-13924C § dune 1980 Sopenstoc MIL-C-U3924B 30 March 1966 MILITARY SPECIFICATION COATING, OXIDE, BLACK, FOR FERROUS MPTALS ‘This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers black oxide coatings applied to fer- rous metals (wrought iron, carbon, low alloy, and corrosion resistant steels). Black oxide coatings, with or without a supplementary preservative treatment (see 3.11), may be used where a black surface 15 required. Only very Limited corrosion protection, under mildly corrosive conditions, 15 obtained as a reault of black oxide coating (see 6.1). Black coatings are included in this specification wath limitations as noted in 1.2. 1,2 Claserts ion. Black oxide coatings covered by this specification shall be of the following clas 8 as specified (see 6.4). Class 1 - Alkaline oxidizing process (for wrought iron, ca! Ralleable irons, plain carbon, and low alloy steels). Class 3 - Pused salt oxidizing process (for corrosion resistant steel alloys which are tempered at 900 F (482 C) or higher). Class 4 - Alkaline oxidizing process (for 300 series corrosion resistant steel alloys only). APPLICABLE DOCUMENTS 2.1 The following documents, of the issue in effect on date of invitation for bids or request for proposal, form a part of this specification to the extent specifred herein. Lire ere 7 beneficial comaents (recommendations, additions, deletions) and any pertinent Jdata which may be of use in derroving this document should be addressed to: Director, US Army Materials and Mechanics Research Center, ATTN: DRXMR-LS, Watertown, HA 02172 by using the self-addressed Standardization Docunent Improvement Proposal (DD Porm 1426) appearing at the end of this document or ty| etter.mti-c-13924C SPECIFE :ATIONS FEDERAL nt-C-490 - “leaning Method and Pretreatment of Ferrous Surfaces for Organic Coatings W-L-a00 - wubricacing O11, General Purpose, Preservative, (Water- Displacing, Low Temperature) MILITARY MIL-S~5002 - Surface Treatments and Inorganic Coatings for Metal Surfaces of Weapons Systems MIL~C-16173 - Corrosion Preventive Compound, Solvent Cutback, Cold- Application pOD-P-.6.23. - Phosphate Coatang, Heavy, Manganese or Zinc Base (For Ferrous Metals) STANDARDS mrurTes MIL-S7D-105 - Sampling Procedures and Tables for Inspection by Attrioutes RANDBD:K= MILITARY MIL-HDBK=20. - Phosphating and dlacx Oxide Coating of Ferrcas Metals (Copies of specifications, standacds, drawings, and oublications required by suppliers in connection with specific procurement f ~ctions should be obtained fron the procuring activity or as directed by the contracting officer.) 2.2 Other punlications. The following document forms a part of this specification t. the extent specified herein. Unless otherwise indicated, the issue in effect on date of invitation for bids or request for proposal snail apply. AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) STANDARDS B 117 - Method of Salt Spray (Fog) Testing \apelication for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Pniladelpmia, Pennsylvania 19103.) 3. UEQUIREMENTS 3.1 Materials. The materials for the blackening processes shall be selected by the contractor. The selected materials shall result in black coatings meeting all the applicable requirements of this specification.MIL-C-13924C 3.2 Preparation of basis petal. Prior to the application of the black coatings, the basis metal shall be thoroughly cleaned as prescribed in WIL-5-5002. Cleaning materials and methods shall be at the option of the con- tractor. The cleaning process shall be performed without measurable abrasion or erosion. The cleaned surfaces shall be free of rust, scale, grease, 011, paint, or other foreign matter. ‘ALL pacts which are colé formed or vhich contain residi auch ag may be produced by cold straighten- ing, shall be given a stress relief treatment in accordance with MIL-S-5002 before cleaning and coating. 3.2.2 Coating as a final process. Unless otherwise specified, the black coatings shall be applied after all machining, forming, welding, cold straightening and heat treatment have been completed. 3.3. Application of black coatings. The coating shall conform to the class specified. The specified black coating shall be applied under controlled time and temperature conditions. All equipment together vith solutions or baths shall be properly maintained and kept free of dirt or possible contaminants. ‘The selected process shall not reduce the hardness of the parts being pro- cessed or expose the parts to temperatures in the temper brittle range of the material, nor shall it cause embrittlement of the steel. 3.3.1 Surface attack. The process shall not result in any attack of the sucface, either pitting or intergranular. Dsily determination for this behavior shall be made using a microscopic method and examined at 8 magni- fication which will clearly establish the condition. Parts with pitted sur- faces or showing intergranilar attack shall be rejected. 3.4 Alkaline oxidizing solutions (class 1). Class 1 oxide coatings shall be formed from a boiling alkaline-oxidizing solution. 3.4.1 Rinsing. Class 1 black oxide coated pieces shall be rinsed immediately after processing in a stagnant vara rinse at 140 to 190 F (60 to 88 C) followed by thorough cold water rinsing to effect complete removal of blackening solution. 3.4.2 Chromic acid dip. After the cold water rinse (see 3.4.1) the pieces shall be dipped for a minimum of 30 seconds in a 0.06 percent solution (8 o2. chromic acid per 100 gallons water) of chromic acid maintained at a temper: ture of 150 to 190 F (66 to 88 C) and a pH of 2 to 3. After the chromic acid dip, parte shall be dried without further rinsing by using warm dry air.MIL-C-13924C 3.5 Fused salt oxidizing (class 3). The temperature of the molten oxidiz~ ing salt of class 3 shall not be higher than 900 F (482C). After suitable amersion, the treated parts shall be withdrawn, cooled from eight to ten minutes and rinsed in bot water, 190 F (88 C), followed by thorough cold water rinsing to effect complete removal of blackening solution. After rinsing, the parts shall be dried by warm dry air and given a chromic acid dip as outlined in 3.4.2. 3.6 Alkaline oxsdszing (class 4). The black coating of class 4 shall be processed in accordance with instructions furnished by the suppliers of the raw materials and the resulting coating shall conform to the applicable requirements of this specification. 3.7 Coverage and color. The class 1, 3, and 4 coatings (see 1.2) shall cover the basis metal completely and shall pass the smut test. ‘The color shall be a uniform black. A slight amount of smut, which is inherent in the process, shall not be cause for rejection. There shall be no indication of any reddish-brown or green snut when tested as in 4.4.1, Smut “spottaness” shall be classified as unsatisfactory requiring reprocessing. 3.8 Quality coating (oxalic acid spot test for classes 1 and 3). The black oxide coatings of classes 1 and 3, prior to the application of a preservative, shall pasa the oxalic acid spot test for a good quality coating (figure 3) as specified in 4.4.2. 3.9 Resistance to salt spray (fog) (class 4 AIST ype 300 series corrosion zesietant steel only). The black coating, of class 4 (300 series only), prior to the application of a prservative, shall show no signs of corrosion after 96 hours of exposure in the salt spray test (see 4.4.3). 3:10 Treatment of high strength steel. When specified, steel parts having an ultinate tensile strength of 200,000 psi (1379 MPa) or above shall be baked at 375 + 25 F (191 + 14 C) for three hours or more or given an equivalent enbrittlement relief treatment after application of the oxide coating. Coated springs or other parts subject to flexure shall not be flexed prior to the baking operation. When specified by the procuring activity, nigh strength steel parts sha!l be tested in accordance with 4.4.4 for embrittlement relief, If an embrittlement relief bake 15 required, it shall follow the chromic acid rinse. The embrittlement relief precedes the supplmentary Preservative treatwent. 3.11 Supplementary preservative. Materials for supplementary preservative treatments and methods of application shall be in accordance with the appli- cable requirements of the end item specification, of as otherwise specified. Unless otherwise specified, the supplementary preservative treatment shall be applied tc the ciean and dry parts immediately following the hot dilute chromic acid dip.MiL-c~13924C 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the con- tract of purchase order, the supplier 1s responsible for the performance of all inspection requirements as specified herein. Except as otherwise speci- fied, the supplier may utilize his ovn facilities or any commercial laboratory acceptable to the Government. The Government reserves the right to perform any of the inspections set forth in the specification where such inspections are deened necessary to assure that supplies and services conform to pre- scribed requirements. 4.2 Lot. A lot shall consist of coated parts of the same class, same basis metal, and approximately the same size and shape and coated under similar con- ations. A maximum of 8 hours continuous production shall constitute a lot. 4.3. Sampling. Single sample plan for normal inspection of the classifi~ cation of defects shall be in accordance with MIL-STO-105. 4.3.1 Sampling for nondestructive tests (visual inspection, coverage, golor, smut, and workmanship). Samples shall be selected at random from each inspection lot an accordance with MIL-STD-10S, inspection level I, and acceptable quality level (AQL) equal 1.0 percent defective. 4.3.2 Sampling for destructive tests (oxalic acid spot test, salt spray test, and embrittlenent relief test). Samples shall be selected at random From eacn inspection lot in accordance vith MIL-STD-105, inspection level S-1 and acceptable quality level (AQ) equal to 1.0 percent defective. 4.4 Test procedures. 4.41 Smut test. Test shall be made prior to application of corrosion Prevent ive compound or after vapor degreasing. Each black oxide coated piece shall be inspected visually under atrong light to assure a satisfactory appearance. Each sample shall also be wiped with a clean white cloth for apdacations of smut (ses 3.7). A slight amount of smut which 1s inherent in the process 15 acceptable for all classes of coatings and shall not be cause for rejection.MIL-C-13924C 4.4.2 Oxalic acid spot test (classes 1 and 3). The black oxide coated pieces of classes 1 and 3 only, prior to the application of a preservative, shall be handled with clean cotton gloves or the equivalent. Each sample shall have deposited, on one flat spot of the black oxide coated surface, three drops (0.2 ml) of a five percent solution of oxalic acid. The reaction shall be observed after 30 seconds and up to eight minutes. After eight minutes the panel shall be rinsed and compared to figures 1, 2, and 3. A laght grey center with a lighter border color (figure 1) indicates a poor quality coating. A grey-black center with a light border (figure 2) indicates a borderline quality coating. The coating shall conform co the good quality coating of Figure 3 to be acceptable. A black or dark broun center with a laght border (figure 3) indicates a good quality coating. A good quality coating may show a light border, indicating exposure of metal around the drops. Parts shall therefore be judged only on the color and expesure of the meta’ under the drops. 4.4.3 Resistance to salt spray (class 4). The coated pieces of class 4 (AISI type 300 series Corrosion resistant steel) shall be subjected to a $ percent salt spray (fog) test in accordance with ASTM B 117. Exposure tine for the black coatings, prior to the application of a preservative, or after vapor degreasing, shall comply with the requirements of 3.9. 4.4.4 Embrittlement relief. To test for embrittlement, the use of notched tensile samples may be used when specified. Samples selected in accordance with 4.3.2 for determining compliance with 2.10, shall be subjected to a sus- tained tensile teat as specified by the procuring civity, or using loads applicable to the parts as contained herein. The articles or pacts shall be held under the load for at least 200 hours unless otherwise specified, and then examined for cracks. The lot shall be rejected af any coated part develops cracks or fails by fracture. 4.4.4.1 Fasteners. Parts such as steel fasteners, threaded or not threaded, which are used for mechanical joining of metal shall be subjected to 2 sustained tensile loading not less than 75 percent of the material specifi- cation minimum ultimate tensile strength. 4.4.4.2 Spring pins, lock rings, etc. Parts such as spring pins, lock rings, etc., which are installed in holes as rods shall be similarly assembled using the applicable parts specification as drawing tolerances which impose the maximum sustained tensile stress on the coated parts. 4.4.4.3 Other parts. Other parts, that will be subjected to a sustained static tensile load in excess of 25 percent of the material specification minamun tensile yield strenyth in service use, shall be subjected to a sus- taaned tensile load equal to 75 percent of the material specification minimum tensile yield strength.y mrt-c-139240 5. PACKAGING 5:1 Preparation for delivery 1s not applicable to this specification. 6. ores 6.1 Intended use. Black oxide coatings are particularly suited for moving parts that cannot tolerate the dimensional build-up of more corrosion resistant finish. They are not recommended on parts going into long-term storage. Sometimes, long term storage is required and a protective pre- servative fluid 1s recommended or a desiccated package is utilized. The coatings present a pleasing black appearance frequently employed for decor- ative purposes or decrease in light reflection. A supplementary water displacing preservative coating such as MIL-C-16173, grade 3 or VV-L-800 or comparable material which will provide equal or superior corrosion protection may be specified. CAUTION: Hagh strength steel (Rockwell C40 or greater hardness) May be subjected to “caustic embrittlement" that could lead to spontaneous cracking if under internal or applied stress during the blackening treatment. 6.1.1 Organic finishes. Black oxade coatings are not primarily used as Pretreatment coatings for paint and lacquer. A phosphate base coating (T7-C-490, type I, of DOD-P-16232, type Z, class 3) gives better corrosion reexstance and is preferred, 6.2 Ordering data. Purchasers should exercise any desired options offered herein, and procurement documents should specify the following: a, Tatle, number, and date of this specification. b. Class of coating (see 1.2). ©. Enbrittlement relief treatment and test, if applicable (see 3.10 and 4.4.4). 3.12 and 6.1). | Supplementary preservative treatment if required 6.3 Miscellaneous notes. 6.3.1 Dimensional change. Black oxide coatings on iron and steel should Produce no appreciable dimensional change of the treated piece. The dinen- sions shown on the drawings are, therefore, the dimensions after the appli- cation of the coatings.MIL-C-13924C 6.3.2 Processing. Contractors may employ one of a number of trade-name black-finashing oxidizing materials or prepared chemical mixtures to apply the black oxide coating. The processing details should conform to MIL-HDBK-205, or as recommended by the raw material supplier. Table T provides an outline of the various processes. TABLE 1, Materials and processing procedures. Process and Approximate Approximate Applicability to possible processing immersion ferrous metals chemicals temperature __tane 1 carbon steels, Alkaline dor? 5 to 60 mn low alloy steels, oxidizing, tanks wrought irons, aod, boiling at cast and malle- ——NaNO3, 285 - 205 F able irons water (aa ~ 152 6) 3 For corrosion Fuzed sett Molten bath 30 mn resistant steel oxadazing 750 - 950 F alloys vmich Razer 207 (399 - 4-0) are tempered st and/or 300 r (482 Cc) £3Cr207 or higher 4 Tor 300 series cor- Alkalane 250 - 265 F 15 to 30 mn rosion resisten: oxidizing, (221 - 130 6) ste! alloys, proprietary only compounds plus water. 6.2.3 Cast_and malleanle irons. Cast and malleable irons may o¢ ‘0 effectively treated in clase @ proprietary bathe. They have not been included an table I because of the class 4 salt spray requirement. 6.3.4 Class 4 coatings. Corrosion resisting steels of minimum composition 17 Cr ~ 7 #1 can be effectively blackened by this process.- MIL~C-13924 6.3.5 Ransing. In order to obtain effective removal of blackening solution and ensure thorough rinsing, a combination of spray canses with tank rinses or a properly operated double counterflow rinse operation may be advantageous. Use of such a system may belp reduce the amount of water required to obtain a desired rinsing craterion and facilitate meeting the EPA standard. Custodians Preparing activity Army - MR Arey - MR Navy - 0S ar Force - 11 Project No. MPFP-0147 Review actavities: Army = AR, MI, BA Navy - aS. Air Force - 99 User activity: Army - ME, AV Navy - SH Air Force ~ 68MIL-C~13924C ra ire Femara Tema OIAVOD AIT¥Ob GoD ¥ ONLAVOO LITIVOd EAITHSGOE ¥ ‘MIIV09 LITTVND Hood ¥ SORTIVOD AGIXO MOVIG MO SISHL LOds dTov OTTO 4INSTRUCTIONS: In « continuing effort to maks our stundariination documents batter, the DoD promdes thu form for use ip ‘eubmitting comments and suggetions for Improvements All usr of military standardisation documenta are invited to provide sugzetions. ‘Thin form may be detached, folded along the lines indicated, taped along the loose edge (DO NOT STAPLE} , and mailed, In block 6, be a wpeciSc ue pomible about particular problem ere euch ws wording which required interpretation, wat oo ripd, restrict, Jones, ambyuous, or was meompatile, and pve proposed wording changes which would allenats the ‘probleme. Eater in block 6 any remarks not rusted to a epecific paragraph of the document If block 7 is filled out, a8 scknowledgement will be malled to you within 30 days to lt you know that your comments ware received and are being considered. NOTE This form may not be used Lo request copies of documents, sor to request waivers, deviations, or clarification of specifiation reqairements on current contract Comments submitied on this form do not constitute or imply suthonsation ‘0 waive any portion of the referenced documents) or to amend contractual requirements. Paid cna Bae oe) (Foi sona tte ne) weceseany ‘DEPARTMENT OF THE NAVY | | I | rrat ey UTED stares ‘Orriciat suSINERE PENALTY FOR PRIVATE UsE 8300 BUSINESS REPLY MAIL TOSTAGE WILL BE PAIO BY THE DEPARTMENT OF THE NAVY Director US Army Materials and Mechanice Research Center ATIN: DRXMR-SSs Watertown, MA 02172STANDARDIZATION DOCUMENT IMPROVEMENT PROPOSAL {See Instructions ~ Revere Se) 7 OCUMENT HOMER ae ‘DOCOMENT TITLE fy ADDRESS Greet, City, iaw, ZIP Code) [e TYFE OF ORGANIZATION ia one] LO venoon O usm [D) smnuracrunen —— ( orwen stream | fe PROBLEM AREAS (5 Peer toh Number and Wording fe REM ARS fie Wawe OF BOeMITTER Hat Pint Mi) ~ Options! WORK TELEPHONE NUMBER fnciods Ave Cour) Options! DD serv, 1426 e-WeRTLIWG ABORERS vat Cy, tau IP Cada] ~ Ootnal PREVIOUS EDITION 1 OBSOLETE SS10N (YVMDDY |