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ASTM A1093 - A 1093M - 15.pdf

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ASTM A1093 - A 1093M - 15.pdf

Designation A1093/A1093M − 15Standard Specification forElectrolytic Plasma Treatment Processing of ConductiveMaterials1This standard is issued under the fixed designation A1093/A1093M; the number immediately following the designation indicates theyear of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification covers the requirements for cleaning,coating, or surface modification, or combinations thereof, ofconductive materials, primarily metals.1.2 This specification covers any conductive materialtreated or processed by the electrolytic plasma process EPPincluding products designated as long products, including wireand fine wire; flat-rolled materials; fasteners; connectors; bolts;assemblies; structural materials; hardware items; and medicalitems.1.3 Products created under this process shall specificallyspecify requirements for the specific product being processedusing the EPP process.1.4 This specification is applicable for orders in eitherinch-pound or SI units.1.5 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in non-conformancewith the standard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards2A90/A90M Test Method for Weight [Mass] of Coating onIron and Steel Articles with Zinc or Zinc-Alloy CoatingsA924/A924M Specification for General Requirements forSteel Sheet, Metallic-Coated by the Hot-Dip ProcessB487 Test Method for Measurement of Metal and OxideCoating Thickness by Microscopical Examination ofCross SectionD2200 Practice for Use of Pictorial Surface PreparationStandards and Guides for Painting Steel SurfacesF519 Test Method for Mechanical Hydrogen EmbrittlementEvaluation of Plating/Coating Processes and Service En-vironments2.2 SSPC Standard3SSPC-VIS 1 Guide and Reference Photographs for SteelSurfaces Prepared by Dry Abrasive3. Terminology3.1 Definitions of Terms Specific to This Standard3.1.1 anode, npositively charged device within the plasmareactor.3.1.2 applied potential, ndirect current dc voltage ap-plied between two electrodes, anode and cathode.3.1.3 aqueous plasma, nuse of water as the source of theH2–HH 2e.3.1.4 cathode, nnegatively charged work piece within theplasma reactor.3.1.5 electrolyte, naqueous solution containing ions ca-pable of conducting electric current.3.1.6 micro-roughness, nfeatures formed as a result of thekinetic energy produced from the implosion and rapid quench-ing phenomenon that occur during electro-plasma technologyEPT processing.3.1.7 plasma, ncollection of free moving electrons andions capable of conducting electric current.3.1.7.1 DiscussionIn this case, the gas is hydrogen and theion is H. Energy is required to make plasma. Withoutsustaining energy, plasma recombines into molecularhydrogen, H.1This test method is under the jurisdiction of ASTM Committee A05 onMetallic-Coated Iron and Steel Products and is the direct responsibility ofSubcommittee A05.12 on Wire Specifications.Current edition approved Oct. 1, 2015. Published November 2015. DOI10.1520/A1093A1093M-15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standard’s Document Summary page onthe ASTM website.3Available from the Society for Protective Coatings, 40 24th St., 6th Floor,Pittsburgh, PA 15222.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.8 plasma reactor, ndevice housing that confines theplasma within the work zone containing the electrolyte, whichallows the formation of plasma.3.1.9 salts, nrefers to the soluble metal salts used withinthe aqueous plasma process.3.1.10 surface morphology, nunique surface characterizedby the presence of micro-craters and spheroids created by theelectro-plasma process.3.2 Acronyms3.2.1 EPPElectro-plasma processing3.2.2 EPTElectro-plasma technology4. Electro-Plasma Process EPP44.1 Electro-plasma processes EPP are a hybrid of conven-tional electrolysis and atmospheric plasma processes. All theindependent studies lead to a common observation that, at acertain value of voltage between two electrodes in an aqueouselectrolyte, will lead to deviation from Faraday’s normalelectrolytic regime. Applied voltage is significantly greaterwhen compared to the conventional electrolysis leading to theanalogous phenomenon that is accompanied by the formationof a continuous plasma envelope around either the cathode orthe anode with the presence of luminous discharge or glowplasma. The critical factors that influence the formation of thecontinuous plasma envelope include applied potential, electro-lyte temperature, geometry of the electrodes, nature andproperties of the electrolyte, and flow dynamics of the electro-lyte and work piece. Most of the studies are concentrated onthe anodic regime.NOTE 1In the EPT process described here, the work piece is thecathode and it is negatively charged. Plasma forms on the cathode. Theanode is the positively charged electrode.Electro-plasma technology EPT is used to engineer metalsurfaces in the cathodic regime, but it can be used in the anodicregime depending on desired results. EPT processing is adynamic process that involves delivery of aqueous electrolyteinto a confined chamber EPT reactors on the surface of thework piece. Balance between electrolyte flow and plasmagenerations ensures a uniform treatment of the metal surfaces.4.2 EPP is an environmentally friendly technology appliedin a closed-loop system.NOTE 2There are no solid wastes generated from EPT. Vaporgenerated during the process can be captured and returned.5.1 In a cathodic regime with an electrolyte of near neutralsalts, cleaning of a metal surface can be achieved. EPT caneffectively remove lubricants, dirt, metal oxide scale, and soforth from metal surfaces. Organic materials are disassociatedinto their gaseous components, thick oxides are broken andblasted off the surface, and thin residual oxide layers arereduced back to their pure metallic element.5.2 EPT cleaning uses thermal shock, electrical current,chemical reaction, and kinetic energy in the form of cavitation.5.3 Plasma formed on the surface of the work piece in aliquid electrolyte results in unique surface characteristics and aunique morphology micro-roughness.6. Electro-Plasma Cleaning Process6.1 Electro-plasma cleaning of a continuous length of aconductive metal is accomplished by passing the item throughan appropriately designed reaction chamber. The number ofreactors required is speed-dependent and they are run intandem.6.2 The reactor chamber is supplied with electrolyte in acontrolled method.6.3 A large potential is set between the anode and cathodework piece, normally in the range of 25 to 250 V.6.4 Luminous plasma is generated at the work piece surfaceand the work piece is cleaned of contaminants and oxides.6.5 The work piece then passes through a hot 70 80C[160 180F] water spray rinse and is dried.6.6 The product can now be collected on a typical packageor it can go directly into EPT deposit reactors for coating witha variety of metals and alloys.7. Testing Requirements Cleaning7.1 The degree of cleaning is typical for a specific industrybut is typically done by comparing the appearance of the dirtycomponent to the cleaned component and, therefore, is anattribute rating. In this case, it is recommended that the surfacebe examined under a magnification of 20 for signs of residuallubricant, soils, and oxides. A minimum of at least three areasshould be observed and the estimate of cleanliness recorded.Arating is developed by estimating the percent of the field thatcontains no signs of residual lubricant, soils, or oxides. Theaverage of these estimate observations are recorded and used torate the level of cleanliness. The actual cleanliness level of aspecimen may vary widely and still be acceptable for theintended end use. The user will be responsible for determiningthe minimum level of their particular application. It has beenthe experience when using EPT that the surface is 99 to 100 free of any visual contamination.8. Electro-Plasma Deposition8.1 EPT has the ability to deposit metal and alloy coatingssuch as zinc, nickel, zinc-nickel, nickel-copper, molybdenum,tin, and so forth. EPT coatings exhibit excellent adhesion withthe substrate and are deposited at significantly high depositionrates as compared to conventional electrolytic processes. EPThas also been used to alloy metals such as molybdenum onto4The electrolytic plasma process, Patent number US 6585875 is covered by apatent. Interested parties are invited to submit information regarding the identifica-tion of an alternatives to this patented item to the ASTM International Headquar-ters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend.ASTM International takes no position respecting the validity of any patent rightsasserted in connection with any item mentioned in this standard. Users of thisstandard are expressly advised that determination of the validity of any such patentrights, and the risk of infringement of such rights, are entirely their ownresponsibility.A1093/A1093M − 152another metal’s surface. The science of electro-plasma deposi-tion is reviewed in the publication “Electro-Plasma Technol-ogy Science and Engineering – An Overview.”5EPT deposi-tion does not follow typical electro-plating principles. Thetransport of ions from the electrolyte to the cathode is notlimited by what is known as the boundary layer. In EPT themetallic ions are transported on plasma bubbles and, in simpleterms, hurled at exceptionally high velocities to the cathode.This accounts for the higher deposition rates compared tonormal electro-plating rates and eliminates the phase boundarydiffusion layer that limits the rates in conventional systems.9. Electro-Plasma Deposition Process9.1 Electro-plasma deposition of a continuous length of aconductive metal is accomplished by passing the item throughan appropriately designed reactor chamber. The number ofreactors required is dependent upon speed and the thickness ofdeposit desired, and they are run in series. Deposits can bemade as a single layer of a mono-metal or an alloy. Depositscan also be in separate and distinct layers of different metals.Very thin layers of some metals can be alloyed with the surfaceof the substrate such as molybdenum.9.2 The reactor chamber is supplied with electrolytes con-taining the metal ions to be deposited and supplied in acontrolled method.9.3 A large potential is set between the anode and cathodework piece, normally in the range of 25 to 250 V. In EPT,Faraday’s law does not apply as with normal electro-platingprocesses.9.4 Luminous plasma is generated at the work piece and thewire or other work piece is coated with the metal ionscontained in the electrolyte.9.5 The work piece then passes through a hot 70 80C[160 180F] water spray rinse and is dried.9.6 The product can now be collected on a typical packageor it can go directly into a second set of deposition reactors forcoating another metal.9.7 The last step is to rinse the coated product with hotwater and dry before packaging.9.8 IntermetallicWith EPT deposition, there is no inter-metallic zone created.9.9 Mechanical properties such as tensile strength andtorsion will not change because of the process. EPT also willnot cause any hydrogen embrittlement. The process parametersshould be controlled to make sure that the work piece is notoverheated during the process. The tensile test data for as-drawn compared to as-EPT-zinc-coated and as-EPT-cleanedwire shows that the tensile strength is not changed. Testsaccording to Test Method F519 have shown that the EPTprocess does not cause hydrogen embrittlement.10. Testing Requirements Coating10.1 Testing is highly dependent on the user requirements.10.2 AdhesionThe coating shall show no signs of flakingwhen the samples are bent or twisted as described in thefollowing10.2.1 RoundWraps should be made around mandrel ofthe same diameter as the test sample minimum of five turnsand examined under 10 magnification.10.2.2 WireTo determine ductility and coating adhesion,wire can be wrapped around its own diameter, five wraps onwithout breaking of the wire or delamination of the coating.10.2.3 SheetA 180 bend examined under 10 magnifica-tion.10.3 DuctilityThe coated samples shall be broken intension and the fracture observed at 10 magnification, and thecoating will show ductile flow to point of fracture withoutseparation between coating and substrate.10.4 ThicknessThe specific thickness shall be agreed be-tween the purchaser and manufacturer. The following methodsmay be used to verify the average thickness.10.4.1 Electrical PermeabilityUsing a standard of knownthickness of the same coating material can provide a relativemeasurement.10.4.2 X-Ray DiffractionUsing a standard of known thick-ness of the same coating material can provide a relativemeasurement.10.4.3 Metallographic MeasurementTest Method B487.Asample can be prepared in cross section, polished, and viewedat an appropriate magnification to allow microscopic measure-ment of the perpendicular thickness of the coating.Aminimumof three points spaced around the cross section evenly butincluding thicker and thinner spots to arrive at an averagethickness.10.4.4 Weight Measurement by Stripping the CoatingTestMethod A90/A90M. Selecting a sample of appropriate size,normally 5 to 20 g, and the initial weight is recorded. Thecoating is dissolved with the appropriate chemical agent. Thesample is rinsed in deionized DI water and dipped in acetoneand allowed to dry. Reweigh the sample and record the newweight. Using the density of the coating material, calculate theaverage thickness on the cross section.11. Coating Properties11.1 Coating Weight MassUse the following relation-ships to estimate the coating thickness from the coating weightfor zinc mass1 oz⁄ft2weight 5 1.7 mil coating thickness 1and17.14 g⁄m2weight 5 1 coating thickness 2where1 oz/ft2 305.15 g/m211.2 Coating Weight Mass Tests11.2.1 Coating weight mass tests shall be performed inaccordance with the requirements of Specif

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