化学镀镍相关标准与规范
化学镀镍的质量检测与相关标准
化学镀镍的质量检测与相关标准一、化学镀镍的质量检测：※外观按主要表面的外观可为光亮、半光亮或无光泽。
除另有规定,当用目视检查,表面应均匀,不应有麻点、裂纹、起泡、分层或结瘤等缺陷。
※表面粗糙度如果需方规定了粗糙度，应按GB 3505的规定进行测定。
镀层的表面粗糙度一般不会优于镀前基体的表面粗糙度。
※厚度主要表面镀覆的自催化镍-磷合金和底层的最小厚度及测量方法应由需方规定。
※弯曲试验将试样沿直径最小为12mm的或试样厚度4倍的心轴绕180°用4倍的放大镜检查，有无脱皮，起泡。
※硬度如果需方要求硬度值，应按GB 9790规定的方法，在热处理后测量，其结果应在需方规定的硬度值的±10％以内。
※镀层的耐蚀性参照ASTM-B-117进行， 如果需要，需方应规定镀层的耐蚀性及其试验和评价方法。
二. 化学镀镍的相关标准： 序号 标准号 标准名1 GB/T13913—92 自催化镍-磷镀层技术要求和试验方法2 ISO 4527—1987 自催化镍磷镀层——规范和试验方法3 ASTM B656—79 金属上工程用自催化镀镍标准实施方法4 MIL-C -26074—B 美国 军用规范 化学镀镍层技术要求5 AMS- 2404—A航空材料规范 化学镀镍7 NACE T—6A—54美国 腐蚀工程师学会文件 化学镀镍层8 DEF STD 03-5/1 英国 材料的化学镀镍9 NFA-91—105 法国 化学镀镍层特性和测试方法10 DIN50966—1987 德国 功能用化学镀镍11 RAL-RG660 德国 硬铬和化学镀镍层的质量保证12 ONORMC2550—1987 化学镀镍磷镀层—技术要求杰昌金属表面处理技术有限公司提供。
化学镀镍的一般操作规范
化学镀镍的一般操作规范简介成形的化学镀镍工艺是在1946年被发现及发展的，1955年美国通用运输公司（GA TC）建成了第一条化学镀镍生产线和第一个商品化学镀镍溶液。
20世纪80年代，化学镀镍工艺有了巨大的发展，研究和应用达到一个新的水平。
按照合金成分分类，化学镀镍可以分为镍-磷合金和镍-硼合金两大类。
从应用领域来讲，镍-磷合金使用更为普遍。
化学镀镍-磷合金按照溶液的pH可以分为碱性和酸性化学镀镍，碱性化学镀镍主要用于预镀的打底层，以提高电镀层与基体的结合力，在铝轮毂的电镀中有较成功的应用。
酸性化学镀镍工艺是目前化学镀镍中应用最为广泛的工艺，按镀层中的磷含量又可分为低磷（2%~5%）、中磷（6%~9%）和高磷（10%以上）。
化学镀镍工艺因为镀层均匀，亮度好，耐蚀性及耐磨性优良而被广泛应用于多个领域。
1. 化学镀镍的周期定义化学镀镍溶液在使用中的管理与维护非常重要，它与电镀液的管理与维护不同，化学镀镍液中的镍离子等多种成分时刻在不断变化，均需要外加补充，否则溶液不能正常进行。
化学镀镍溶液的好坏一般通过能够获得质量稳定镀层的周期（循环系数MTO）来评判。
目前市场销售的化学镀镍溶液多数分为A、B、C三种组份，周期数可以做到6~8，对镀层质量要求不严格的可以做到12个周期甚至以上。
1个周期的定义是，当溶液中主盐的添加量达到了开缸剂量时为一个周期，以1L溶液为例，开缸量一般为60毫升/升，在使用过程中，当A剂的补充量达到了60毫升时，该化学镀镍溶液就已使用一个周期。
2. 化学镀镍溶液的过程控制2.1应准确计算槽体容积和零件的表面积看似再简单不过的问题，但很多时候都难以做到。
化学镀镍溶液的消耗及补充与装载量有直接的关系，因此，溶液的装载量应得到重视。
装载量就是所要施镀零件的表面积与溶液体积之比值。
一般控制在1~1.5 dm2/L为最佳，过大（>2.5 dm2/L）或过小（<0.5 dm2/L）对溶液的稳定性都不好。
ASTM B-733-97 金属表面化学镀镍磷层规范标准
Designation:B733–97Standard Specification forAutocatalytic(Electroless)Nickel-Phosphorus Coatings on Metal1This standard is issued under thefixed designation B733;the number immediately following the designation indicates the year of original adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.A superscript epsilon(e)indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1.Scope1.1This specification covers requirements for autocatalytic (electroless)nickel-phosphorus coatings applied from aqueous solutions to metallic products for engineering(functional)uses.1.2The coatings are alloys of nickel and phosphorus pro-duced by autocatalytic chemical reduction with hypophosphite. Because the deposited nickel alloy is a catalyst for the reaction, the process is self-sustaining.The chemical and physical properties of the deposit vary primarily with its phosphorus content and subsequent heat treatment.The chemical makeup of the plating solution and the use of the solution can affect the porosity and corrosion resistance of the deposit.For more details,see ASTM STP265(1)2and Refs(2)(3)(4)and(5) also refer to Figs.X1.1,Figs.X1.2,and Figs.X1.3in the Appendix of Guide B656.1.3The coatings are generally deposited from acidic solu-tions operating at elevated temperatures.1.4The process produces coatings of uniform thickness on irregularly shaped parts,provided the plating solution circu-lates freely over their surfaces.1.5The coatings have multifunctional properties,such as hardness,heat hardenability,abrasion,wear and corrosion resistance,magnetics,electrical conductivity provide diffusion barrier,and solderability.They are also used for the salvage of worn or mismachined parts.1.6The low phosphorus(2to4%P)coatings are microc-rystalline and possess high as-plated hardness(620to750HK 100).These coatings are used in applications requiring abra-sion and wear resistance.1.7Lower phosphorus deposits in the range between1and 3%phosphorus are also microcrystalline.These coatings are used in electronic applications providing solderability,bond-ability,increased electrical conductivity,and resistance to strong alkali solutions.1.8The medium phosphorous coatings(5to9%P)are most widely used to meet the general purpose requirements of wear and corrosion resistance.1.9The high phosphorous(more than10%P)coatings have superior salt-spray and acid resistance in a wide range of applications.They are used on beryllium and titanium parts for low stress properties.Coatings with phosphorus contents greater than11.2%P are not considered to be ferromagnetic.1.10The values stated in SI units are to be regarded as standard.1.11The following precautionary statement pertains only to the test method portion,Section9,of this specification.This standard does not purport to address all of the safety concerns, if any,associated with its use.It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limita-tions prior to use.2.Referenced Documents2.1ASTM Standards:B368Test Method for Copper-Accelerated Acetic Acid-Salt Spray(Fog)Testing(CASS Testing)3B374Terminology Relating to Electroplating3B380Test Method of Corrosion by the Corrodkote Proce-dure3B487Test Method for Measurement of Metal and Oxide Coating Thicknesses by Microscopical Examination of a Cross Section3B499Test Method for Measurement of Coating Thick-nesses by the Magnetic Method:Nonmagnetic Coatings on Magnetic Basis Metals3B504Test Method for Measurement of Thickness of Me-tallic Coatings by the Coulometric Method3B537Practice for Rating of Electroplated Panels Subjected to Atmospheric Exposure3B567Method for Measurement of Coating Thickness by the Beta Backscatter Method3B568Method for Measurement of Coating Thickness by X-Ray Spectrometry31This specification is under the jurisdiction of ASTM Committee B-08on MetalPowders and Metal Powder Products and is the direct responsibility of Subcom-mittee B08.08.01on Engineering Coatings.Current edition approved July10,1997.Published October1997.Originallypublished as B733–st previous edition B733–90(1994).2The boldface numbers given in parentheses refer to a list of references at theend of the text.3Annual Book of ASTM Standards,V ol02.05.1Copyright©ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959,United States.B571Test Methods for Adhesion of Metallic Coatings3B578Test Method for Microhardness of Electroplated Coatings3B602Test Method for Attribute Sampling of Metallic and Inorganic Coating3B656Guide for Autocatalytic Nickel-Phosphorus Deposi-tion on Metals for Engineering Use3B667Practice for Construction and Use of a Probe for Measuring Electrical Contact Resistance4B678Test Method for Solderability of Metallic-Coated Products3B697Guide for Selection of Sampling Plans for Inspection of Electrodeposited Metallic and Inorganic Coatings3B762Method for Variable Sampling of Metallic and Inor-ganic Coatings3B849Specification for Pre-Treatment of Iron or Steel for Reducing the Risk of Hydrogen Embrittlement3B850Specification for Post-Coating Treatments of Iron orSteel for Reducing the Risk of Hydrogen Embrittlement3 B851Specification for Automated Controlled Shot Peening of Metallic Articles Prior to Nickel,Autocatalytic Nickel, Chromium,or As A Final Finish3D1193Specification for Reagent Water5D2670Method for Measuring Wear Properties of Fluid Lubricants(Falex Method)6D2714Method for Calibration and Operation of an Alpha LFW-1Friction and Wear Testing Machine6D3951Practice for Commercial Packaging7D4060Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser8E60Practice for Photometric Methods for Chemical Analy-sis of Metals9E156Test Method for Determination of Phosphorus in High-Phosphorus Brazing Alloys(Photometric Method)10 E352Test Methods for Chemical Analysis of Tool Steels and Other Similar Medium-and High-Alloy Steel9F519Test Method for Mechanical Hydrogen Embrittle-ment11G5Practice for Standard Reference Method for Making Potentiostatic and Potentiodynamic Anodic Polarization Measurements12G31Practice for Laboratory Immersion Corrosion Testing of Metals12G59Practice for Conducting Potentiodynamic Polarization Resistance Measurements12G85Practice for Modified Salt Spray(Fog)Testing122.2Military Standards:MIL-R-81841Rotary Flap Peening of Metal Parts13MIL-S-13165Shot Peening of Metal Parts13MIL-STD-105Sampling Procedures and Tables for Inspec-tion by Attribute132.3ISO Standards:ISO4527Autocatalytic Nickel-Phosphorus Coatings—Specification and Test Methods143.Terminology3.1Definition:3.1.1significant surfaces—those substrate surfaces which the coating must protect from corrosion or wear,or both,and that are essential to the performance.3.2Other Definitions—Terminology B374defines most of the technical terms used in this specification.4.Coating Classification4.1The coating classification system provides for a scheme to select an electroless nickel coating to meet specific perfor-mance requirements based on alloy composition,thickness and hardness.4.1.1TYPE describes the general composition of the de-posit with respect to the phosphorus content and is divided into five categories which establish deposit properties(see Table1). N OTE1—Due to the precision of some phosphorus analysis methods a deviation of0.5%has been designed into this classification scheme. Rounding of the test results due to the precision of the limits provides for an effective limit of4.5and9.5%respectively.For example,coating with a test result for phosphorus of9.7%would have a classification of TYPE V,see Appendix X4,Alloy TYPEs.4.2Service Condition Based on Thickness:4.2.1Service condition numbers are based on the severity of the exposure in which the coating is intended to perform and minimum coating thickness to provide satisfactory perfor-mance(see Table2).4.2.2SC0Minimum Service,0.1µm—This is defined by a minimum coating thickness to provide specific material prop-erties and extend the life of a part or its function.Applications4Annual Book of ASTM Standards,V ol03.04.5Annual Book of ASTM Standards,V ol11.01.6Annual Book of ASTM Standards,V ol05.02.7Annual Book of ASTM Standards,V ol09.02.8Annual Book of ASTM Standards,V ol06.01.9Annual Book of ASTM Standards,V ol03.05.10Discontinued;see1992Annual Book of ASTM Standards,V ol03.05. 11Annual Book of ASTM Standards,V ol15.03.12Annual Book of ASTM Standards,V ol03.02.13Available from Standardization Documents Order Desk,Bldg.4Section D, 700Robbins Ave.,Philadelphia,PA19111-5094,Attn:NPODS.14Available from American National Standards Institute,11W.42nd St.,13th Floor,New York,NY10036.TABLE1Deposit Alloy TypesType Phosphorus%wtI No Requirement for PhosphorusII1to3III2to4IV5to9V10and aboveTABLE2Service ConditionsCoating Thickness RequirementsService ConditionMinimum CoatingThicknessSpecificationµm in.(mm)SC0Minimun Thickness0.10.000004()SC1Light Service50.0002()SC2Mild Service130.0005()SC3Moderate Service250.001()SC4Severe Service750.003()include requirements for diffusion barrier,undercoat,electrical conductivity and wear and corrosion protection in specialized environments.4.2.3SC1Light Service ,5µm—This is defined by a minimum coating thickness of 5µm for extending the life of the part.Typical environments include light-load lubricated wear,indoor corrosion protection to prevent rusting,and for soldering and mild abrasive wear.4.2.4SC2Mild Service ,13µm—This is defined by mild corrosion and wear environments.It is characterized by indus-trial atmosphere exposure on steel substrates in dry or oiled environments.4.2.5SC3Moderate Service ,25µm—This is defined by moderate environments such as non marine outdoor exposure,alkali salts at elevated temperature,and moderate wear.4.2.6SC4Severe Service ,75µm—This is defined by a very aggressive environment.Typical environments would include acid solutions,elevated temperature and pressure,hydrogen sulfide and carbon dioxide oil service,high-temperature chlo-ride systems,very severe wear,and marine immersion.N OTE 2—The performance of the autocatalytic nickel coating depends to a large extent on the surface finish of the article to be plated and how it was pretreated.Rough,non uniform surfaces require thicker coatings than smooth surfaces to achieve maximum corrosion resistance and minimum porosity.4.3Post Heat Treatment Class —The nickel-phosphorus coatings shall be classified by heat treatment after plating to increase coating adhesion and or hardness (see Table 3).4.3.1Class 1—As-deposited,no heat treatment.4.3.2Class 2—Heat treatment at 260to 400°C to produce a minimum hardness of 850HK100.4.3.3Class 3—Heat treatment at 180to 200°C for 2to 4h to improve coating adhesion on steel and to provide for hydrogen embrittlement relief (see section 6.6).4.3.4Class 4—Heat treatment at 120to 130°C for at least 1h to increase adhesion of heat-treatable (age-hardened)alumi-num alloys and carburized steel (see Note 3).4.3.5Class 5—Heat treatment at 140to 150°C for at least 1h to improve coating adhesion for aluminum,non age-hardened aluminum alloys,copper,copper alloys and beryl-lium.4.3.6Class 6—Heat treatment at 300to 320°C for at least 1h to improve coating adhesion for titanium alloys.N OTE 3—Heat-treatable aluminum alloys such as Type 7075can undergo microstructural changes and lose strength when heated to over 130°C.5.Ordering Information5.1The following information shall be supplied by the purchaser in either the purchase order or on the engineering drawing of the part to be plated:5.1.1Title,ASTM designation number,and year of issue of this specification.5.1.2Classification of the deposit by type,service condi-tion,class,(see 4.1,4.2and 4.3).5.1.3Specify maximum dimension and tolerance require-ments,if any.5.1.4Peening,if required (see6.5).5.1.5Stress relief heat treatment before plating,(see6.3).5.1.6Hydrogen Embrittlement Relief after plating,(see 6.6).5.1.7Significant surfaces and surfaces not to be plated must be indicated on drawings or sample.5.1.8Supplemental or Special Government Requirements such as,specific phosphorus content,abrasion wear or corro-sion resistance of the coating,solderability,contact resistance and packaging selected from Supplemental Requirements.5.1.9Requirement for a vacuum,inert or reducing atmo-sphere for heat treatment above 260°C to prevent surface oxidation of the coating (see S3).5.1.10Test methods for coating adhesion,composition,thickness,porosity,wear and corrosion resistance,if required,selected from those found in Section 9and Supplemental Requirements.5.1.11Requirements for sampling (see Section 8).N OTE 4—The purchaser should furnish separate test specimens or coupons of the basis metal for test purposes to be plated concurrently with the articles to be plated (see 8.4).6.Materials and Manufacture6.1Substrate —Defects in the surface of the basis metal such as scratches,porosity,pits,inclusions,roll and die marks,laps,cracks,burrs,cold shuts,and roughness may adversely affect the appearance and performance of the deposit,despite the observance of the best plating practice.Any such defects on significant surfaces shall be brought to the attention of the purchaser before plating.The producer shall not be responsible for coatings defects resulting from surface conditions of the metal,if these conditions have been brought to the attention of the purchaser.6.2Pretreatment —Parts to be autocatalytic nickel plated may be pretreated in accordance with Guide B 656.A suitable method shall activate the surface and remove oxide and foreign materials,which may cause poor adhesion and coating poros-ity.N OTE 5—Heat treatment of the base material may effect its metallur-gical properties.An example is leaded steel which may exhibit liquid or solid embrittlement after heat treatment.Careful selection of the pre and post heat treatments are recommended.TABLE 3Classification of Post Heat TreatmentCLASS DescriptionTemperature(°C)Time (h)1No Heat Treatment,As Plated2Heat Treatment for Maximum Hardness TYPE I260202851632084001TYPE II 350to 3801TYPE III 360to 3901TYPE IV 365to 4001TYPE V375to 40013Hydrogen Embrittlement and Adhesion on Steel180to 2002to 44Adhesion,Carburized Steel and Age Hardened Aluminum 120to 1301to 65Adhesion on Beryllium and Aluminum140to 1501to 26Adhesion on Titanium300–3201–46.3Stress Relief:6.3.1Pretreatment of Iron and Steel for Reducing the Risk of Hydrogen Embrittlement—Parts that are made of steel with ultimate tensile strength of greater than1000Mpa(hardness of 31HRC or greater),that have been machined,ground,cold formed,or cold straightened subsequent to heat treatment,shall require stress relief heat treatment when specified by the purchaser,the tensile strength to be supplied by the purchaser, Specification B849may be consulted for a list of pre-treatments that are widely used.6.3.2Peening—Peening prior to plating may be required on high-strength steel parts to induce residual compressive stresses in the surface,which can reduce loss of fatigue strength and improve stress corrosion resistance after plating. (See Supplementary Requirements).6.3.3Steel parts which are designed for unlimited life under dynamic loads shall be shot peened or rotaryflap peened.N OTE6—Controlled shot peening is the preferred method because there are geometry’s where rotaryflap peening is not effective.See S11.2. 6.3.3.1Unless otherwise specified,the shot peening shall be accomplished on all surfaces for which the coating is required and all immediate adjacent surfaces when they contain notches,fillets,or other abrupt changes of section size where stresses will be concentrated.6.4Racking—Parts should be positioned so as to minimize trapping of hydrogen gas in cavities and holes,allowing free circulation of solution over all surfaces to obtain uniform coating thickness.The location of rack or wire marks in the coating shall be agreed upon between the producer and purchaser.6.5Plating Process:6.5.1To obtain consistent coating properties,the bath must be monitored periodically for pH,temperature,nickel and hypophosphite.Replenishments to the plating solution should be as frequent as required to maintain the concentration of the nickel and hypophosphite between90and100%of set point. The use of a statistical regimen to establish the control limits and frequency of analysis may be employed to ensure quality deposits are produced.6.5.2Mechanical movement of parts and agitation of the bath is recommended to increase coating smoothness and uniformity and prevent pitting or streaking due to hydrogen bubbles.6.6Post Coating Treatment for Iron and Steel for Reducing the Risk of Hydrogen Embrittlement—Parts that are made of steel with ultimate tensile strengths of1000Mpa(hardness of 31HRC or greater),as well as surface hardened parts,shall require post coating hydrogen embrittlement relief baking when specified by the purchaser,the tensile strength to be supplied by the purchaser.Specification B850may be con-sulted for a list of post treatments that are widely used.6.6.1Heat treatment shall be performed preferably within1h but not more than3h of plating on plated after plating of steel parts to reduce the risk of hydrogen embrittlement.In all cases,the duration of the heat treatment shall commence from the time at which the whole of each part attains the specified temperature.6.6.2High-strength steel parts with actual tensile strengths greater than1000MPa(corresponding hardness values300 HV10,303HB or31HRC)and surface hardened parts shall be processed after coating in accordance with Specification B850.6.7Heat Treatment After Plating to Improve Adhesion—To improve the adhesion of the coating to various substrates,the heat treatments in Table3should be performed as soon as practical after plating(see4.3).6.8Heat Treatment After Plating to Increase Hardness: 6.8.1To increase the hardness of the coating a heat treat-ment of over260°C is required.Table3describes the heat treatment for maximum hardness.6.8.2See Appendixes3and4and Guide B656;Figs.X1.2 and Figs.X1.3.6.8.3A heat treatment at260°C for greater than20h should be used to reduce the loss of surface hardness and strength of some ferrous basis metals.Avoid rapid heating and cooling of plated parts.Sufficient time must be allowed for large parts to reach oven temperature.N OTE7—The length of time to reach maximum hardness varies with the phosphorus content of the deposit.High phosphorus deposits may require longer time or a higher temperature,or both.Individual alloys should be tested for maximum hardness attainable,especially for condi-tions of lower temperatures and longer times.N OTE8—Inert or reducing atmosphere or vacuum sufficient to prevent oxidation is recommended for heat treatment above260°C.Do not use gas containing hydrogen with high-strength steel parts.7.Requirements7.1Process—The coating shall be produced from an aque-ous solution through chemical reduction reaction.7.2Acceptance Requirements—These requirements are placed on each lot or batch and can be evaluated by testing the plated part.7.2.1Appearance:7.2.1.1The coating surface shall have a uniform,metallic appearance without visible defects such as blisters,pits, pimples,and cracks(see9.2).7.2.1.2Imperfections that arise from surface conditions of the substrate which the producer is unable to remove using conventional pretreatment techniques and that persist in the coating shall not be cause for rejection(see 6.1).Also, discoloration due to heat treatment shall not be cause for rejection unless special heat treatment atmosphere is specified (see section5.1.9).7.2.2Thickness—The thickness of the coating shall exceed the minimum requirements in Table2as specified by the service condition agreed to prior to plating(see9.3).After coating and if specified,the part shall not exceed maximum dimension on significant surface(see section5.1.3).N OTE9—The thickness of the coating cannot be controlled in blind or small diameter deep holes or where solution circulation is restricted. 7.2.3Adhesion—The coating shall have sufficient adhesion to the basis metal to pass the specified adhesion test(see9.4 and Test Methods B571).7.2.4Porosity—The coatings shall be essentially pore free when tested according to one of the methods of9.6.The test method,the duration of the test,and number of allowable spots per unit area shall be specified(see section5.1.10and9.6).7.3Qualification Requirements—These requirements are placed on the deposit and process and are performed on specimens to qualify the deposit and plating process.The tests for these qualification requirements shall be performed monthly or more frequently.7.3.1Composition—Type II,III,IV,V deposits shall be analyzed for alloy composition by testing for phosphorus(see 9.1).The weight percent of phosphorus shall be in the range designated by type classification(see4.1).7.3.2Microhardness—The microhardness of Class2depos-its shall be determined by Test Method B578(Knoop).For Class2coatings,the microhardness shall equal or exceed a minimum of850(HK100(or equivalent Vickers)(see4.3and 9.5).The conversion of Vickers to Knoop using Tables E140 is not recommended.7.3.3Hydrogen Embrittlement—The process used to de-posit a coating onto high strength steels shall be evaluated for hydrogen embrittlement by Test Method F519.8.Sampling8.1The purchaser and producer are urged to employ statis-tical process control in the coating process.Properly performed this will ensure coated products of satisfactory quality and will reduce the amount of acceptance inspection.8.1.1Sampling plans can only screen out unsatisfactory products without assurance that none of them will be accepted.(7)8.2The sampling plan used for the inspection of a quantity of coated parts(lot)shall be Test Method B602unless otherwise specified by purchaser in the purchase order or contract(see section5.1.11and S.11.1).N OTE10—Usually,when a collection of coated parts(the inspection lot8.2)is examined for compliance with the requirements placed on the partsa relatively small number of parts,the sample,is selected at random and inspected.The inspection lot is then classified as complying or not complying with the requirements based on the results of the inspection sample.The size of the sample and the criteria of compliance are determined by the application of statistics.The procedure is known as sampling inspection.Three standards Test Method B602,Guide B697, and Test Method B762contain sampling plans that are designed for the sampling inspection of coatings.Test Method B602contains four sampling plans,three for use with tests that are nondestructive and one for use with tests that are destructive.The purchaser and producer may agree on the plan(s)to be used.If they do not, Test Method B602identifies the plan to be used.Guide B697provides a large number of plans and also gives guidance on the selection of a plan.When Guide B697is specified,the purchaser and producer need to agree on the plan to be used.Test Method B762can be used only for coating requirements that have a numerical limit,such as coating thickness.The last must yield a numerical value and certain statistical requirements must be met.Test Method B762contains several plans and also gives instructions for calculating plans to meet special needs.The purchaser and producer may agree on the plan(s)to be used.If they do not,Test Method B762 identifies the plan to be used.An inspection lot shall be defined as a collection of coated parts which are of the same kind,that have been produced to the same specification, that have been coated by a single producer at one time or approximately the same time under essentially identical conditions,and that are submit-ted for acceptance or rejection as a group.8.3All specimens used in the sampling plan for acceptance tests shall be made of the same basis material and in the same metallurgical condition as articles being plated to this specifi-cation.8.4All specimens shall be provided by the purchaser unless otherwise agreed to by the producer.N OTE11—The autocatalytic nickel process is dynamic and a daily sampling is recommended.For Coatings requiring alloy analysis and corrosion testing weekly sampling should be considered as an option. 9.Test Methods9.1Deposit Analysis for Phosphorus:9.1.1Phosphorus Determination—Determine mass% phosphorus content according to Practice E60,Test Methods E352,or Test Method E156on known weight of deposit dissolved in warm concentrated nitric acid.9.1.2Composition can be determined by atomic absorption, emission or X-rayfluorescence spectrometry.N OTE12—Inductively coupled plasma techniques can determine the alloy to within0.5%.The following analysis wavelength lines have been used with minimum interference to determine the alloy.Ni216.10nm Cd214.44nm Fe238.20nmP215.40nm Co238.34nm Pb283.30nmP213.62nm Cr284.32nm Sn198.94nmAl202.55nm Cu324.75nm Zn206.20nm9.2Appearance—Examine the coating visually for compli-ance with the requirements of7.2.1.9.3Thickness:N OTE13—Eddy-current type instruments give erratic measurements due to variations in conductivity of the coatings with changes in phosphorus content.9.3.1Microscopical Method—Measure the coating thick-ness of a cross section according to Test Method B487.N OTE14—To protect the edges,electroplate the specimens with a minimum of5µm of nickel or copper prior to cross sectioning.9.3.2Magnetic Induction Instrument Method—Test Method B499is applicable to magnetic substrates plated with auto-catalytic nickel deposits,that contain more than11mass% phosphorus(not ferromagnetic)and that have not been heat-treated.The instrument shall be calibrated with deposits plated in the same solution under the same conditions on magnetic steel.9.3.3Beta Backscatter Method—Test Method B567is only applicable to coatings on aluminum,beryllium,magnesium, and titanium.The instrument must be calibrated with standards having the same composition as the coating.N OTE15—The density of the coating varies with its mass%phospho-rus content(See Appendix X2).9.3.4Micrometer Method—Measure the part,test coupon, or pin in a specific spot before and after plating using a suitable micrometer.Make sure that the surfaces measured are smooth, clean,and dry.9.3.5Weigh,Plate,Weigh Method—Using a similar sub-strate material of known surface area,weigh to the nearest milligram before and after plating making sure that the part or coupon is dry and at room temperature for eachmeasurement.Calculate the thickness from the increase in weight,specific gravity,and area as follows:coating thickness,µm510W/~A3D!(1) where:W=weight gain in milligrams,A=total surface area in square centimetres,andD=grams per cubic centimetres(see Appendix X2).9.3.6Coulometric Method—Measure the coating thickness in accordance with Test Method B504.The solution to be used shall be in accordance with manufacturer’s recommendations. The surface of the coating shall be cleaned prior to testing(see Note14).9.3.6.1Calibrate standard thickness specimens with depos-its plated in the same solution under the same conditions. 9.3.7X-Ray Spectrometry—Measure the coating thickness in accordance with Test Method B568.The instrument must be calibrated with standards having the same composition as the coating.N OTE16—This method is only recommended for deposits in the as-plated condition.The phosphorus content of the coating must be known to calculate the thickness of the deposit.Matrix effect due to the distribution of phosphorus in layers of the coating also effect the measurement accuracy and require that calibration standards be made under the same conditions as the production process.9.4Adhesion:9.4.1Bend Test(Test Methods B571)—A sample specimen is bent180°over a mandrel diameter43the thickness(10mm minimum)of the specimen and examined at43power magnification forflaking or separation at the interface.Fine cracks in the coating on the tension side of the bend are not an indication of poor adhesion.Insertion of a sharp probe at the interface of the coating and basis metal to determine the adhesion is suggested.N OTE17—Appropriate test specimens are strips approximately25to50 mm wide,200to300mm long and3to6mm thick.9.4.2Impact Test—A spring-loaded center punch with a point having2to3mm radius is used to test adhesion of the coating on nonsignificant surfaces of the plated part.Make three closely spaced indentations and examine under103 magnification forflaking or blistering of the coating,which is cause for rejection.9.4.3Thermal Shock—The coated part is heated to200°C in an oven and then quenched in room temperature water.The coating is examined for blistering or other evidence of poor adhesion at43magnification.9.5Microhardness—The microhardness of the coating can be measured by Test Method B578using Knoop indenter and is reported in Knoop Hardness Number(HK).It will vary depending on loads,type of indenter,and operator.A100g load is recommended.The rhombic Knoop indenter gives higher hardness readings than the square-base pyramidal Vickers diamond indenter for100to300g loads,see Ref(6).For maximum accuracy,a minimum coating thickness of75µm is recommended.Conversions of Vickers or Knoop hardness number to Rockwell C is not recommended.N OTE18—On thick(75µm+)coatings on steel a surface microhardness determination is permissible.9.6Porosity—There is no universally accepted test for porosity.When required,one of the following tests can be used on the plated part or specimen.9.6.1Ferroxyl Test for Iron Base Substrates—Prepare the test solution by dissolving25g of potassium ferricyanide and 15g of sodium chloride in1L of distilled water.After cleaning,immerse the part for30s in the test solution at25°C. After rinsing and air drying,examine the part for blue spots, which form at pore sites.9.6.2Boiling Water Test for Iron-Base Substrates—Completely immerse the part to be treated in a vesselfilled with aerated water at room temperature.Apply heat to the beaker at such a rate that the water begins to boil in not less than15min,nor more than20min after the initial application of heat.Continue to boil the water for30min.Then remove the part,air dry,and examine for rust spots,which indicate pores. N OTE19—Aerated water is prepared by bubbling clean compressed air through distilled water by means of a glass diffusion disk at room temperature for12h.The pH of the aerated water should be6.7+0.5.9.6.3Aerated Water Test for Iron-Base Substrates—Immerse the part for4h in vigorously aerated Type IV or better water(see Specification D1193)at2562°C temperature and then examine the part for rust spots.9.6.4Alizarin Test for Aluminum Alloys—Wipe the plated part or specimen with10mass%sodium hydroxide solution. After3min contact,rinse,and apply a solution of alizarin sulfonate prepared by dissolving1.5g of methyl cellulose in90 mL of boiling water to which,after cooling,0.1g sodium alizarin sulfonate,dissolved in5mL of ethanol is added.After 4min contact,apply glacial acetic acid until the violet color disappears.Any red spots remaining indicate pores.9.6.5Porosity Test for Copper Substrates—Wipe the plated part or specimen with glacial acetic acid.After3min,apply a solution of potassium ferrocyanide prepared by dissolving1g of potassium ferrocyanide and1.5g methyl cellulose in90mL of boiling distilled water.The appearance of brown spots after 2min indicate pores.9.7Other Test Methods—Test methods which have been developed that are equal to or better than these may be substituted.The precision and bias requirements will vary for each type of test.If an alternate test is specified it shall be agreed upon between the producer and the purchaser.10.Rejection and Rehearing10.1Part(s)that fail to conform to the requirements of this standard may be rejected.Rejection shall be reported to the producer promptly in writing.In the case of dissatisfaction occurs with the results of a test,the producer may make a claim for a hearing.Coatings that show imperfections may be rejected.11.Certification11.1When specified in the purchase order or contract,the purchaser shall be furnished certification that the samples representing each lot have been processed,tested and inspected as directed in this specification and the requirements havebeen。
化学镀镍
（1）浓氨水（密度：0.91g/ml）。 （2）紫脲酸胺指示剂（紫脲酸胺：氯化钠=1：100）。 （3）EDTA容液 0.05mol，按常规标定。
分析方法： 用移液管取出 10ml冷却后的化学镀镍液于 250ml的锥形瓶中，并加入 100ml蒸馏水、 15ml浓氨水、约 0.2g指示剂，用标定后的EDTA溶液滴定，当溶液颜色由浅棕色变至紫色 即为终点。 镍含量的计算： C Ni2＋ = 5.87 M•V (g/L) 式中 M——标准EDTA溶液的摩尔浓度； V——耗用标准EDTA溶液的毫升数。 2．还原剂浓度
4.大面积假镀除去杂质或更换部分镀液
5.用活性炭处理镀浴
6.缩短工作转移时间
7.按规范进行热处理
PH值变化快
1.前处理溶液带入污染
2.槽负载过大
3.镀浴PH值越出缓冲范围
1.改进镀前清洗工序
2.减少装载量
3.检查、调整PH值至最佳操作范围之内
镀层粗糙
1.镀浴中悬浮不溶物
2.镀前清洗不够
3.PH值过高
化学除油是利用碱溶液的皂化作用和表面活性物质对非皂化性油脂的乳化作用，除去工 件表面上的各种油污的。化学除油的温度通常取在 60-80 度之间，工件除油效果一般为目 测，即工件表面能完全被水润湿就是油污完全除尽的标志。一般的除油液由氢氧化钠、碳酸 钠、磷酸三钠、水玻璃、乳化剂等组成。
电化学除油分阴极除油和阳极除油，在相同的电流下，阴极除油产生的氢气比阳极除油 产生的氧气多一倍，气泡小而密，乳化能力大，除油效果更好。但容易造成工件氢脆和杂质 在阴极析出的现象。阳极除油虽没有这些缺点但可能造成工件表面氧化和溶解。目前常用正 负极交换的化学除油法。电化学除油液配方与化学除油的配方相似。
电镀专用镍技术要求
电镀专用镍技术要求1化学成分
电镀专用镍的化学成分应符合表1规定。
表1电镀专用镍的化学成分
化学成分,%
（Ni+Co）不小于
Co
不大于
杂质含量，不大于
C Si P S Fe Cu Zn As
99.970.02
0.010.0020.0010.0010.0040.0050.00080.0008 Cd Sn Sb Pb Bi Al Mn Mg 0.00030.00030.00030.00080.00030.0010.0010.001
注：镍加钴含量由减量法确定。
2规格尺寸
2.1电镀专用镍厚度：8～15mm
2.2电镀专用镍大板规格：880×880±10mm；880×860±10mm。
2.3电镀专用镍小块（剪切）规格：50×50±5mm；25×25±3mm。
2.4电镀专用镍规格尺寸亦可根据需方要求进行剪切与加工。
3外观质量
3.1电镀专用镍表面洁净，无污泥、油污等。
3.2电镀专用镍边缘不得有树枝状结粒及密集气孔（允许修整）。
3.3电镀专用镍表面不得有直径大于2mm的密集气孔，直径0.5～2mm 密集气孔区总面积不得超过镍板单面面积的10%。
3.4电镀专用镍表面高度大于2mm的密集结粒区总面积不得超过镍板单面积10%。
注：25mm×25mm镍板面积上有5个以上气孔或结粒称为密集气孔区或密集结粒区。
4内部质量
电镀专用镍内部应无夹杂、电解液等缺陷。
5其他要求
如需方对电镀专用镍化学成分、物理规格有特殊要求，可由供需双方协商，并在订货单中注明。
化学银及化学镍电镀标准
修改内容
修改依据
签名及日期
核准
审核
制作
外观要求
2. 化
产品类型
电镀后无变形,划伤.发黄,起泡,露底,颗粒等现象. 表面化学镀材质及膜厚
五金类
化学镍
见电镀图
可靠性测试
1.盐雾48H不能发黄,起泡等现象. 2.焊锡性能良好. 3.附着力测试不可脱皮. 4.需符合ROHS环保要求
外观要求 电镀后无变形,划伤.发黄,起泡,露底,颗粒等现象.
修改记号
文件编号
版本/版次
A.0
化学银及化学镍标准
一 ：
生效日期
页码
1/1
为规范统一镀化学银及化学镍的工艺和膜厚，特制定以下标准。
二 ： 三 ：
1. 化
产品类型
表面化学镀材质及膜厚
五金类
化学银
0.2um-0.5um
可靠性测试
1.硫化钾测试:2分钟不可发黑,起泡等现象. 2.附着力测试不可脱皮. 3.需符合ROHS环保要求
化学镀镍注意事项
化学镀镍注意事项化学镀镍是一种常用的表面处理技术，主要用于金属制品的防腐蚀、提高硬度和美观度。
在进行化学镀镍过程中，需要注意以下几个事项：1. 清洁表面：在进行化学镀镍前，必须确保待处理的金属表面干净无油污、氧化物等杂质。
可以使用酸洗、碱洗等方法将金属表面清洗干净，以确保化学镀镍层与基体金属之间的结合力。
2. 防止氧化：在清洗完金属表面后，应避免表面暴露在空气中，防止金属表面再次氧化。
可以将待处理的金属部件置于密封容器中，或进行表面保护处理，如涂覆一层保护膜等。
3. 控制镀液浓度：化学镀镍的过程中需要用到一定浓度的镀液。
在进行镀液配置时，应准确控制其浓度，以保证其性能稳定。
镀液浓度过高会造成镀层过厚、晶粒粗化等问题，浓度过低则会影响镀层的质量。
在使用中需进行定期的浓度检测和调整。
4. 控制镀液温度：化学镀镍的过程中也需要保持一定的温度范围。
温度过高会引起镀层的开裂、弯曲等问题，温度过低则会导致镀液粘度增大、镀层质量下降。
需根据不同金属的镀液温度特性进行调整，确保温度稳定。
5. 控制镀液pH值：镀液的pH值是影响化学镀镍过程的重要参数之一。
pH值过高或过低都会影响镀层的均匀性和质量。
具体的pH值范围需要根据具体的镀液配方进行调整，一般在操作过程中需进行定期的pH检测和调整。
6. 电流密度控制：在进行化学镀镍过程中，需要通过施加电流来实现金属离子的还原，并在基体金属表面沉积出金属镍层。
电流密度是控制镀层厚度和质量的重要参数之一。
过高的电流密度会引起镀层结构的不均匀性和孔隙度增大，过低则会造成镀层过薄。
需根据所需的镀层厚度和质量要求进行调整。
7. 保持搅拌：镀液中的金属离子需要与基体金属表面发生化学反应，形成镀层。
因此，在进行化学镀镍过程中，需保持镀液的充分搅拌，以促进金属离子和基体金属之间的接触和反应。
这可以通过机械搅拌或气体搅拌等方式实现。
8. 防止气泡和悬浮物：在化学镀镍过程中，镀液中不可避免地会产生气泡和悬浮物。
镀化学镍的工艺流程和注意事项
镀化学镍的工艺流程和注意事项下载温馨提示：该文档是我店铺精心编制而成，希望大家下载以后，能够帮助大家解决实际的问题。
文档下载后可定制随意修改，请根据实际需要进行相应的调整和使用，谢谢!并且，本店铺为大家提供各种各样类型的实用资料，如教育随笔、日记赏析、句子摘抄、古诗大全、经典美文、话题作文、工作总结、词语解析、文案摘录、其他资料等等，如想了解不同资料格式和写法，敬请关注!Download tips: This document is carefully compiled by the editor. I hope that after you download them, they can help yousolve practical problems. The document can be customized and modified after downloading, please adjust and use it according to actual needs, thank you!In addition, our shop provides you with various types of practical materials, such as educational essays, diary appreciation, sentence excerpts, ancient poems, classic articles, topic composition, work summary, word parsing, copy excerpts,other materials and so on, want to know different data formats and writing methods, please pay attention!镀化学镍是一种常用的表面处理工艺，在工业生产中有着广泛的应用。
化学镀镍综述
化学镀镍综述化学镀镍，又称为无电解镀镍，是在金属盐和还原剂共同存在的溶液中靠自催化的化学反应而在金属表面沉积了金属镀层的新的成膜技术。
电镀是利用外电流将电镀液中的金属离子在阴极上还原成金属的过程。
而化学镀是不外加电流，在金属表面的催化作用下经控制化学还原法进行的金属沉积过程。
因不用外电源直译为无电镀或不通电镀。
由于反应必须在具有自催化性的材料表面进行，美国材料试验协会（ASTMB-347）推荐用自催化镀一词（Autocatalytic plating）。
对化学镀镍而言，我国1992年颁布的国家标准(GB/T13913-92)则称为自催化镍－磷镀层（Autocatalytic Nickel Phosphorus Coating），其意义与美国材料试验协会的名称相同。
由于金属的沉积过程是纯化学反应（催化作用当然是重要的），所以将这种金属沉积工艺称为“化学镀”最为恰当，这样它才能充分反映该工艺过程的本质。
从语言学角度看Chemical,Non electrolytic,Electroless三个词主是一个意义了，直译为无电镀一词是不确切的。
“化学镀”这个术语目前在国内外已被大家认同和采用。
化学镀镍所镀出的镀层为镍磷合金，按其磷含量的不同可分为低磷、中磷、高磷三大类：·磷含量低于3%的称为低磷；·磷含量在3-10%的为中磷；·磷含量高于10%的为高磷；其中中磷的跨度比较大，一般我们常见的中磷镀层为6-9%的磷含量。
当然，本站主要介绍的是化学镀镍磷合金，有时为了方便我们简称化学镀了，而且EN也是化学镀镍简称。
但化学镀不仅此一种镀种，比较成熟的还有化学镀铜，化学镀金，化学镀锡，还有一种复合镀层。
其它镀种的市场占有量不足总量的1%，本站不做重点介绍。
化学镀层的物理性质与化学性质密度：镍的密度在20℃时为8.91。
含磷量1%-4%时为8.5；含磷量7%-9%时为8.1；含磷量10%-12%时为7.9。
AMS2404D化学镀镍
AMS2404D化学镀镍(中文)化学镀镍1. 范围 1.1. 目的这个规格说明涵盖在不同材料上度化学镍的工艺要求。
1.2．应用这种材料过去常被用作提供统一的构造形状，去提高抵抗防腐蚀性，或改善它的可焊性，但它的作用不仅仅局限在这些应用上，这种材料已被用做服务于 1000°F(540℃)尽管它的抗腐蚀作用会随着服务的温度增加而消弱。
1.3.分类这种规格的电镀分类如下：等级一. 除了氢脆化的减除，不进行电镀加热处理。
等级二. 加热处理在 450°F（232℃）或者以上，使材料变坚硬。
等级三. 加热处理在 375°F（191℃）去核实非热处理合金的粘附性。
等级四. 加热处理在 250°F（121℃）去核实热处理合金的粘附性。
1.3.1 除非有细节的规定，一般采用等级一。
1.4.安全或危险材料：当描述和被引用的材料，方法，应用和步骤在这个规格中也许会涉及使用危险材料。
这个规格没有指明在这种使用中会涉及到危险。
这是使用者的责任去确保和熟悉危险材料的安全和正当使用，以及采取必要预防措施确保参与人员的健康和安全。
2.应用文件：下面出版的版本是这个指定范围类规格下的一部分，引用的最新版本在购买订单之日起生效。
2.1.ASTM 出版： ASTM B 117:盐沫测试装置。
ASTM B 487:在横截面下用显微镜测量金属和氧化层厚度。
ASTM B 499:通过磁性法测量膜厚度，无磁性膜在磁性金属上。
ASTM B 568：通过 X 射线的光谱学去测量膜的厚度。
ASTM B 571：金属膜的粘附性。
ASTM B636：螺旋状镀金属膜的内部压力测试。
ASTM748：通过显微镜扫描横截面测量金属膜的厚度。
ASTM764：对不同镍材料进行逐个表层的厚度测试(STEP 测试)。
ASTM384: 材料显微硬度测试。
ASTM519：电镀过程和飞机维修化学中，机械氢脆化测试。
化学镀镍相关标准与规范
化学镀镍相关标准与规范化学镀镍过程的标准和规范有许多，几乎各国都有自己的标准，这些标准和规范是由许多学科的专业人员共同制定的，为了方便我国技术人员参考，现将其中比较重要的一些标准名称列出：国际标准：ISO 4527(1987),ISO/TC107 自催化镍磷镀层-规范和试验方法(Autocatalyticnickel-phosphoruscoatings-specification and test methods)中国：自催化镍－磷镀层技术要求和试验方法 GB/T 13913－92美国：ASTM B733-97 金属上自催化镍磷镀层标准规范(Standard Specification for Autocatalytic(Electroless) Nickel-Phosphorous Coatings on Metal)ASTMB656-91 工程用金属自催化镍磷沉积标准（Standard Guide for Autocatalytic (Electroless)Nickel-Phosphorus on Metals for Engineering Use）ASTM B656-79 金属上工程用自催化镀镍标准实施办法（该标准于2000年废止）MILC 26074B-军用规范，化学镀镍层的技术要求（Coatings，Electroless Nickel Requirements for Military）AMS 2404A-航空材料规范化学镀镍(Electroless Nickel Plating)AMS 2405-航空材料规范化学镀镍，低磷(Electroless Nickel Plating，Low Phosphrous) NACE T-6A-54 美国腐蚀工程师学会文件化学镀镍层英国：DEE STD 03-5/1 材料的化学镀镍层(Electroless Nickel Coatings of Material)法国：NFA 91-105 化学镀镍层特性和测试方法（Dépôt Chimique s de Nickel-Propciétés Caractéristiques atMéthodes Déssais德国：DIN 50966(1987) 功能化学镀镍层RAL-RG 660(第二部分)（1984）硬铬和化学镀镍层的质量保证苏联标准：ΓOCT 9.305-84奥地利：ÖNOrm c2550(1987) 化学镀镍磷镀层-技术要求和测试日本标准：JISH 8654-89 金属上自催化镍磷镀层H8645-99 ??解ンツケル?りんめフき11.1 国际标准ISO4527该国际标准于1987年发布，论述了含磷2~15wt%的化学镀镍，并阐述了实际的沉积和预处理步骤。
化学镀镍的一般操作规范
化学镀镍的一般操作规范简介成形的化学镀镍工艺是在1946年被发现及发展的，1955年美国通用运输公司（GA TC）建成了第一条化学镀镍生产线和第一个商品化学镀镍溶液。
20世纪80年代，化学镀镍工艺有了巨大的发展，研究和应用达到一个新的水平。
按照合金成分分类，化学镀镍可以分为镍-磷合金和镍-硼合金两大类。
从应用领域来讲，镍-磷合金使用更为普遍。
化学镀镍-磷合金按照溶液的pH可以分为碱性和酸性化学镀镍，碱性化学镀镍主要用于预镀的打底层，以提高电镀层与基体的结合力，在铝轮毂的电镀中有较成功的应用。
酸性化学镀镍工艺是目前化学镀镍中应用最为广泛的工艺，按镀层中的磷含量又可分为低磷（2%~5%）、中磷（6%~9%）和高磷（10%以上）。
化学镀镍工艺因为镀层均匀，亮度好，耐蚀性及耐磨性优良而被广泛应用于多个领域。
1. 化学镀镍的周期定义化学镀镍溶液在使用中的管理与维护非常重要，它与电镀液的管理与维护不同，化学镀镍液中的镍离子等多种成分时刻在不断变化，均需要外加补充，否则溶液不能正常进行。
化学镀镍溶液的好坏一般通过能够获得质量稳定镀层的周期（循环系数MTO）来评判。
目前市场销售的化学镀镍溶液多数分为A、B、C三种组份，周期数可以做到6~8，对镀层质量要求不严格的可以做到12个周期甚至以上。
1个周期的定义是，当溶液中主盐的添加量达到了开缸剂量时为一个周期，以1L溶液为例，开缸量一般为60毫升/升，在使用过程中，当A剂的补充量达到了60毫升时，该化学镀镍溶液就已使用一个周期。
2. 化学镀镍溶液的过程控制2.1应准确计算槽体容积和零件的表面积看似再简单不过的问题，但很多时候都难以做到。
化学镀镍溶液的消耗及补充与装载量有直接的关系，因此，溶液的装载量应得到重视。
装载量就是所要施镀零件的表面积与溶液体积之比值。
一般控制在1~1.5 dm2/L为最佳，过大（>2.5 dm2/L）或过小（<0.5 dm2/L）对溶液的稳定性都不好。
化学镍金操作规范
目录壹，制程原理一，槽液功能贰，制程控制一，制程流程二，制程控制参数参，药液维护一，配槽浓度二，槽液，滤芯更换时间肆，镍控制器原理一，镍控制器面板二，镍控制器校正三，注意事项伍，镍槽的起镀步骤一，新配槽起镀操作步骤二，停机后起镀操作步骤三，假镀板数量之计算四，PH之设定陆，异常分析与对策柒，生产时注意事项捌，重工流程化学镍金操作规范（中文版）Rev.A1一，槽液功能：1．酸性清洁槽（Acid Cleaner）:主要功能有二：（1）可移去板面油脂及氧化物：（2）润湿板面。
2．微蚀槽（Micro Etch）: SPS/H2SO4 system , for these processes.主要功能：（1）移去污染物；（2）提供铜表面适当的粗糙度；（3）提供化学镍较佳的附着。
3．预浸槽（Pre-dip）:主要功能：（1）避免污染物带入活化槽（保护钯槽）；（2）提供酸性环境以避免不必要的副反应。
4．活化槽（Activator）:靠铜和钯之间离子交换产生晶重层，以利镍的沉积。
反应式如下：Cu + Pd2+→Cu2+ + Pd5．化学镍槽（Electroless Nickel）:(1)在铜表面镀上一层平坦而且均一可焊之镍层；（2）提供极佳的抗腐蚀性（保护铜面）。
6．浸金槽（immersion gold）靠金和镍之间的置换镀一层细密的金层。
反应式如下：2Au++ Ni →2Au + Ni2+贰，制程控制注意事项:1．以上条件视实际状况而定。
2．后浸槽做细线路时才使用。
3．◎：半开；○：1/4开。
4．微蚀量控制在60-100μ″。
5．预浸的时间必须在3分钟以上。
6．活化及镍槽之间水洗勿太久，以避免钯钝化，产生跳镀；镍槽及金槽之间水洗勿太长，以避免镍钝化，造成脱金。
7．微蚀槽以后水洗必须使用纯水。
注意事项:(1)操作条件视实际状况而定(2) H2SO4为CP级浓硫酸(3)Ni: 6.0g/L=100%; 5.7g/L=95%; 6.3g/L=105%参，药液维护（1）配槽时先加半槽纯水，再加药水。
表面处理之化学镀镍规范及制程讲解
Print Date: 22-Nov-19
Foxsemicon Integrated Technology Inc.
CONFIDENTIAL
Presenter:
4
化學鎳配方及反應方程式
Quality Assurance
主成份: • (1)硫酸鎳 (2)次磷酸二氫鈉 (3)絡合劑 (4)pH調整劑（氨水、氫氧化鈉）
Print Date: 22-Nov-19
Foxsemicon Integrated Technology Inc.
CONFIDENTIAL
Presenter:
8
鍍鎳
Quality Assurance
如圖所示，經過兩次鋅置換,在化鎳與之反應瞬間(起鍍前幾分鐘),化鎳可以說是 用快速結合方式去包圍鋅置換,因此才產生優良附著力, 起鍍第一層化鎳時﹐鎳層 立即包圍鋅置換顆粒﹐鋅置換層已經瞬間改變成化鎳層﹐所以說看不出鋅的置換 層換
Outgassing： Analysis of adsorbed organic compounds on coupon surface by automated thermal desorption (ATD) and GCMS.
Adhesion:依照ASTM B571中熱沖擊的方法測試COUPON
自然氧化物則用鹼咬去除------TL-252,但同產生新的氧化物,在ENP制程中,鹼 咬加長時間有助於將表面氧化層及材料雜質咬除及咬鬆
新的氧化物則用酸咬去除------HF/HNO3,去除Si,在ENP制程中,此步驟可以
加長時間,有助於將Si-Mg固熔體(雜質)徹底去除
MgO, CuO,Feo 新的氧化物則用酸洗去除------HNO3,得到近乎純Al表面
化学镀镍
使用过程中稳定性的监控，如果上述试验出现混浊时间明显加快，说明化学镀镍浴处于不稳定状态。 4.一般工艺 在化学镀镍前，金属制品表面前处理包括：研磨抛光、除油、除锈、活化等过程，化学镀镍中经常使用的金属前处理方 法与电镀工艺中的类似。研磨、抛光等物理方法，我们不做讨论。下面主要介绍一些化学处理方法。
1.什么是化学镀镍 化学镀镍，又称为无电解镀镍或自催化镀镍，是通过溶液中适当的还原剂使金属离子在金属表面靠自催化的还原作用而 进行的金属沉积过程。
化学镀溶液的分类方法很多，根据不同的原则有不同的分类法。按 PH 值分为酸性镀液和碱性镀液，酸性镀液 PH 值一般在 4～6，碱性镀液 PH 值一般大于 8，碱性镀液因其操作温度较低，主要用于非金属材料的金属化（如塑料，陶 瓷等）；按还原剂类型不同有次亚磷酸盐、胺基硼烷、硼氢化物以及肼做还原剂的化学镀镍溶液；按温度分类则有高温 镀液（80～95℃）、低温镀液（60～70℃）以及室温镀液；按镀层磷含量可分为高磷镀液、中磷镀液和低磷镀液，高磷 镀液含磷量 9%～12%（质量），镀层呈非磁性、非晶态，在酸性介质中有很高的耐腐蚀性。利用镀层非磁性，主要用于 计算机硬盘的底镀层、电子仪器防电磁波干扰的屏蔽等以及工件的防腐镀层；中磷镀液获得的镀层含磷量为 6%～9%（质 量），此类镀液沉积速率快、稳定性好、寿命长，镀层既耐腐蚀又耐磨，在工业中应用最为广泛，如汽车、电子、纺织 机械、石油化工机械、食品工业、办公设备、精密机械工业等；低磷镀液含磷量 0.5%～5%（质量），此类溶液所得到的 镀层硬度高、耐磨，特别是在碱性介质中的耐腐蚀性能明显优于中磷和高磷镀层。近年来还开发了三元镍-磷合金镀液， 有镍铬磷、镍铜磷、镍钴磷等多种镀液。 2.检测标准 GB/T13913—92 自催化镍-磷镀层技术要求和试验方法 ISO4527(1987),ISO/TC107 自催化镍磷镀层——规范和试验方法 ASTM B656——79 美国 金属上工程用自催化镀镍标准实施方法 MILC 26074B 美国 军用规范 化学镀镍层技术要 求 AMS 2404A——航空材料规范 化学镀镍 AMS 2404——航空材料规范 化学镀镍，低磷 NACE T—6A—54 美国 腐蚀工程师学会文件 化学镀镍层 DEF STD 03-5/1 英国 材料的化学镀镍 NFA-91-105 法国 化学镀镍层特性和测试方法 DIN 50966(1987)德国 功能用化学镀镍 RAL-RG660 第二部分(1984)德国 硬铬和化学镀镍层的质量保证 ONORM C2550(1987)奥地利 化学镀镍磷镀层—技术要求和测试 3.化学镀镍溶液成分分析 为了保证化学镀镍的质量，必须始终保持镀浴的化学成分、工艺技术参数在最佳范围（状态），这就要求操作者经常进 行镀液化学成分的分析与调整。 1.Ni2＋浓度
化学镀镍相关标准与规范
化学镀镍相关标准与规范化学镀镍过程的标准和规范有许多，几乎各国都有自己的标准，这些标准和规范是由许多学科的专业人员共同制定的，为了方便我国技术人员参考，现将其中比较重要的一些标准名称列出：国际标准：ISO 4527(1987),ISO/TC107 自催化镍磷镀层-规范和试验方法(Autocatalyticnickel-phosphoruscoatings-specification and test methods)中国：自催化镍－磷镀层技术要求和试验方法 GB/T 13913－92美国：ASTM B733-97 金属上自催化镍磷镀层标准规范(Standard Specification for Autocatalytic(Electroless) Nickel-Phosphorous Coatings on Metal)ASTMB656-91 工程用金属自催化镍磷沉积标准（Standard Guide for Autocatalytic (Electroless)Nickel-Phosphorus on Metals for Engineering Use）ASTM B656-79 金属上工程用自催化镀镍标准实施办法（该标准于2000年废止）MILC 26074B-军用规范，化学镀镍层的技术要求（Coatings，Electroless Nickel Requirements for Military）AMS 2404A-航空材料规范化学镀镍(Electroless Nickel Plating)AMS 2405-航空材料规范化学镀镍，低磷(Electroless Nickel Plating，Low Phosphrous) NACE T-6A-54 美国腐蚀工程师学会文件化学镀镍层英国：DEE STD 03-5/1 材料的化学镀镍层(Electroless Nickel Coatings of Material)法国：NFA 91-105 化学镀镍层特性和测试方法（Dépôt Chimique s de Nickel-Propciétés Caractéristiques atMéthodes Déssais德国：DIN 50966(1987) 功能化学镀镍层RAL-RG 660(第二部分)（1984）硬铬和化学镀镍层的质量保证苏联标准：ΓOCT 9.305-84奥地利：ÖNOrm c2550(1987) 化学镀镍磷镀层-技术要求和测试日本标准：JISH 8654-89 金属上自催化镍磷镀层H8645-99 ??解ンツケル?りんめフき11.1 国际标准ISO4527该国际标准于1987年发布，论述了含磷2~15wt%的化学镀镍，并阐述了实际的沉积和预处理步骤。
表面处理之化学镀镍规范及制程讲解
Print Date: 11/21/2019
Foxsemicon Integrated Technology Inc.
CONFIDENTIAL
Presenter:
3
ENP處理簡介
Quality Assurance
ENP（無電化鎳）
• 化学镀镍的工业应用
• 由于化学镀镍层具有优秀的均匀性、硬度、耐磨和耐蚀性等综合物理 化学性能，该项技术已经得到广泛应用，目前几乎难以找到一个工业 不采用化学镀镍技术。据报道，化学镀镍在各个工业中应用的比例大 致如下：航空航天工业：9%，汽车工业：5%，电子计算机工业： 15%，食品工业：5%，机械工业：15%，核工业：2%，石油工业： 10%，塑料工业：5%，电力输送工业：3%，印刷工业：3%，泵制 造业：5%，阀门制造业：17%，其他：6%。世界工业化国家的化学 镀镍的应用经历了80年代空前的发展，平均年净增速率高达10%～ 15%；预计化学镀镍的应用将会持续发展，平均年净值速率将降低至 6%左右，而进入发展成熟期。在经济蓬勃发展的东亚和东南地区， 包括中国在内，化学镀应用正在上升阶段，预期仍将保持空前的高速 发展。
ENP溶液濃度主要控制NI和次磷酸鈉的濃度
注:
化鎳藥水的天敵是硝酸根離子,當硝酸根離子達到一定濃度時,它可以 破壞藥水特性,無法鍍鎳,所以要定期用硝酸根離子試紙測試,嚴格控制 硝酸根離子進入溶液
Print Date: 11/21/2019
Foxsemicon Integrated Technology Inc.
Print Date: 11/21/2019
Foxsemicon Integrated Technology Inc.
CONFIDENTIAL
化学镀镍知识概述
化学镀镍知识概述一、化学镀镍溶液的组成与镀液成分设计常识优异的镀液配方对于产生最优质的化学镀镍层是必不可少的。
化学镀镍溶液应包括：镍盐、还原剂、络合剂、缓冲剂、促进剂、稳定剂、光亮剂、润湿剂等。
主盐化学镀镍溶液中的主盐就是镍盐，如硫酸镍、氯化镍、醋酸镍等，由它们提供化学镀反应过程中所需要的镍离子。
早期曾用过氯化镍做主盐，但由于氯离子的存在不仅会降低镀层的耐蚀性，还产生拉应力，所以目前已很少有人使用。
同硫酸镍相比用醋酸镍做主盐对镀层性能是有益的。
但因其价格昂贵而无人使用。
其实最理想的镍离子来源应该是次磷酸镍，使用它不至于在镀浴中积存大量的硫酸根，也不至于在使用中随着补加次磷酸钠而带入大量钠离子，同样因其价格因素而不能被工业化应用。
目前应用最多的就是硫酸镍，由于制造工艺稍有不同而有两种结晶水的硫酸镍。
因为硫酸镍是主盐，用量大，在镀中还要进行不断的补加，所含杂质元素会在镀液的积累，造成镀液镀速下降、寿命缩短，还会影响到镀层性能，尤其是耐蚀性。
所以在采购硫酸镍时应该力求供货方提供可靠的成分化验单，做到每个批量的质量稳定，尤其要注意对镀液有害的杂质尤其是重金属元素的控制。
还原剂用得最多的还原剂是次磷酸钠，原因在于它的价格低、镀液容易控制，而且合金镀层性能良好。
次磷酸钠在水中易于溶解，水溶液的pH值为6。
是白磷溶于NaOH中，加热而得到的产物。
目前国内的次磷酸钠制造水平很高，除了国内需求外还大量出口。
络合剂化学镀镍溶液中除了主盐与还原剂以外，最重要的组成部分就是络合剂。
镀液性能的差异、寿命长短主要取决于络合剂的选用及其搭配关系。
络合剂的第一个作用就是防止镀液析出沉淀，增加镀液稳定性并延长使用寿命。
如果镀液中没有络合剂存在，由于镍的氢氧化物溶解度较小，在酸性镀液中便可析出浅绿色絮状含水氢氧化镍沉淀。
硫酸镍溶于水后形成六水合镍离子，它有水解倾向，水解后呈酸性，这时即析出了氢氧化物沉淀。
如果六水合镍离子中有部分络合剂存在则可以明显提高其抗水解能力，甚至有可能在碱性环境中以镍离子形式存在。
AMS2404D化学镀镍(中文)
化学镀镍1.范围1.1.目的这个规格说明涵盖在不同材料上度化学镍的工艺要求。
1.2．应用这种材料过去常被用作提供统一的构造形状，去提高抵抗防腐蚀性，或改善它的可焊性，但它的作用不仅仅局限在这些应用上，这种材料已被用做服务于1000°F(540℃)尽管它的抗腐蚀作用会随着服务的温度增加而消弱。
1.3.分类这种规格的电镀分类如下：等级一. 除了氢脆化的减除，不进行电镀加热处理。
等级二. 加热处理在450°F（232℃）或者以上，使材料变坚硬。
等级三. 加热处理在375°F（191℃）去核实非热处理合金的粘附性。
等级四. 加热处理在250°F（121℃）去核实热处理合金的粘附性。
1.3.1 除非有细节的规定，一般采用等级一。
1.4.安全或危险材料：当描述和被引用的材料，方法，应用和步骤在这个规格中也许会涉及使用危险材料。
这个规格没有指明在这种使用中会涉及到危险。
这是使用者的责任去确保和熟悉危险材料的安全和正当使用，以及采取必要预防措施确保参与人员的健康和安全。
2.应用文件：下面出版的版本是这个指定范围类规格下的一部分，引用的最新版本在购买订单之日起生效。
2.1.ASTM 出版：ASTM B 117:盐沫测试装置。
ASTM B 487:在横截面下用显微镜测量金属和氧化层厚度。
ASTM B 499:通过磁性法测量膜厚度，无磁性膜在磁性金属上。
ASTM B 568：通过X射线的光谱学去测量膜的厚度。
ASTM B 571：金属膜的粘附性。
ASTM B636：螺旋状镀金属膜的内部压力测试。
ASTM748：通过显微镜扫描横截面测量金属膜的厚度。
ASTM764：对不同镍材料进行逐个表层的厚度测试(STEP测试)。
ASTM384: 材料显微硬度测试。
ASTM519：电镀过程和飞机维修化学中，机械氢脆化测试。
3.技术要求：3.1 预备3.1.1 除非对生产操作有特别的要求，不然组成，运行，热处理，焊接和铜焊在这些配件电镀前完成，除非表面电镀和铜焊相结合。
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化学镀镍相关标准与规范
化学镀镍过程的标准和规范有许多，几乎各国都有自己的标准，这些标准和规范是由许多学科的专业人员共同制定的，为了方便我国技术人员参考，现将其中比较重要的一些标准名称列出：
国际标准：
ISO 4527(1987),ISO/TC107 自催化镍磷镀层-规范和试验方法(Autocatalytic
nickel-phosphorus
coatings-specification and test methods)
中国：
自催化镍－磷镀层技术要求和试验方法 GB/T 13913－92
美国：
ASTM B733-97 金属上自催化镍磷镀层标准规范(Standard Specification for Autocatalytic
(Electroless) Nickel-Phosphorous Coatings on Metal)
ASTMB656-91 工程用金属自催化镍磷沉积标准（Standard Guide for Autocatalytic (Electroless)
Nickel-Phosphorus on Metals for Engineering Use）
ASTM B656-79 金属上工程用自催化镀镍标准实施办法（该标准于2000年废止）
MILC 26074B-军用规范，化学镀镍层的技术要求（Coatings，Electroless Nickel Requirements for Military）
AMS 2404A-航空材料规范化学镀镍(Electroless Nickel Plating)
AMS 2405-航空材料规范化学镀镍，低磷(Electroless Nickel Plating，Low Phosphrous) NACE T-6A-54 美国腐蚀工程师学会文件化学镀镍层
英国：
DEE STD 03-5/1 材料的化学镀镍层(Electroless Nickel Coatings of Material)
法国：
NFA 91-105 化学镀镍层特性和测试方法（Dépôt Chimique s de Nickel-Propciétés Caractéristiques at
Méthodes Déssais
德国：
DIN 50966(1987) 功能化学镀镍层
RAL-RG 660(第二部分)（1984）硬铬和化学镀镍层的质量保证
苏联标准：
ΓOCT 9.305-84
奥地利：
ÖNOrm c2550(1987) 化学镀镍磷镀层-技术要求和测试
日本标准：
JISH 8654-89 金属上自催化镍磷镀层
H8645-99 ??解ンツケル?りんめフき
11.1 国际标准ISO4527
该国际标准于1987年发布，论述了含磷2~15wt%的化学镀镍，并阐述了实际的沉积和预处理步骤。
为了消除钢中的内应力，推荐了热处理的范围，同时也论及了喷砂和喷丸处理。