ASTM B343-1992a(2004)e1 Standard Practice for Preparation of Nickel for Electroplating with Nickel《镍电镀用镍制备的标准实施规范》.pdf

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1、Designation: B 343 92a (Reapproved 2004)e1Endorsed by AmericanElectroplaters SocietyEndorsed by NationalAssociation of Metal FinishersStandard Practice forPreparation of Nickel for Electroplating with Nickel1This standard is issued under the fixed designation B 343; the number immediately following

2、the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEWarning note in 4.2 updated

3、 in May 2004.1. Scope1.1 This practice summarizes well-known, generally practi-cal methods for producing adherent electrodeposits of nickelon nickel.1.2 Electrodeposits of nickel on nickel are produced, forexample, to improve the performance of decorative coatings, toreclaim electroplated parts that

4、 are defective, and to resumenickel electroplating after interruptions in processing. Interrup-tions may be deliberate, for example, to machine the electrode-posit at an intermediate stage in the electrodeposition of thicknickel coatings. The interruptions may be unintentional, forexample, resulting

5、 from equipment and power failures.1.3 To ensure good adhesion of nickel to nickel, precautionsshould be taken to avoid biopolar effects during nickel elec-troplating. This is of particular importance in return-typeautomatic plating machines where one rack follows anotherrack closely. Bipolar effect

6、s can be avoided by making theracks cathodic while they are entering or leaving the nickeltank. Separate current control on entry and exit stations isdesirable.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the use

7、r of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Types of Nickel2.1 The types of nickel for which an overplate of nickel maybe desired are dull nickel, semi-bright nickel, bright nickel, andnickel stri

8、ke. Variations in these types may possibly requirespecial handling.2.2 Surface conditions of the nickel may vary as follows:2.2.1 Freshly electroplated surfaces that are still wet withelectroplating solution or rinse water (see 5.1),2.2.2 Freshly electroplated surfaces that have been allowedto dry (

9、see 5.2),2.2.3 Buffed, polished, or machine-ground surfaces (see5.3), and2.2.4 Surfaces that have been given a reverse-current treat-ment in an alkaline solution for cleaning or possibly strippingan overplate of chromium (see 5.4).3. Cleaning3.1 The following cleaning treatments may be used for allc

10、onditions and types of electrodeposited nickel. The choice ofthe procedure will be governed largely by the condition of thesurface.3.1.1 DegreasingDegreasing is used to remove the bulkof grease, oil, and buffing compounds that may be present onthe surface. The cleaning may be effected with vapor deg

11、reas-ing, organic solvents, emulsion cleaners, or soak cleaner.3.1.2 Electrolytic Alkaline CleaningRemoval of finaltraces of dirt, grease, and oil is accomplished best withelectrolytic alkaline cleaning. The solution may be either aproprietary cleaner or a formulated one. Since a nickel surfaceforms

12、 an oxide coating if treated anodically in an alkalinesolution, this condition must be altered in subsequent steps if itcannot be avoided.4. Activating4.1 The procedure used for etching or activating the nickelsurface usually determines the soundness of the adhesion. Thechoice of the procedure may b

13、e governed by the condition ofthe surface and possibly the type of nickel. The milder etchingtreatment should be used in the case of highly finishedsurfaces, but it may result in sacrificing maximum adhesion.The thickness of the nickel may militate against the use ofcertain etching procedures, and t

14、herefore the thickness re-moved is indicated for each procedure described in 4.2 to 4.8.4.2 Anodic Treatment in Concentrated Sulfuric Acid(Nickel removed nil). A 70 mass % sulfuric acid solutioncontaining 661 mL of concentrated, 96 mass % sulfuric acid(density 1.83 mL) diluted to 1 L may be used for

15、 activating thenickel surface provided the temperature of the solution is notover 30C (see Warning). When the initial mixture cools,1This practice is under the jurisdiction of ASTM Committee B08 on Metallicand Inorganic Coatings and is the direct responsibility of Subcommittee B08.02 onPre Treatment

16、.Current edition approved April 1, 2004. Published May 2004. Originallyapproved in 1960. Last previous edition approved in 1998 as B 343 92a (1998).1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.dilute to exact volume. The time of t

17、reatment should be about1 min at a current density of 10 A/dm2. At this current densitythe nickel normally goes passive and a bright surface becomesonly slightly dull. This type of passivity is removed bysubsequent rinsing in water. (WarningSlowly add the sul-furic acid with rapid stirring to the ap

18、proximate amount ofwater required.)4.3 Anodic Etching in Sulfuric Acid(Nickel removedapproximately 1.3 m.) A 25 mass % sulfuric acid solution,containing 166 mL of concentrated, 96 mass % sulfuric acid(density 1.83 g/mL), diluted to 1 L is used for this anodicetching treatment in which the nickel sur

19、face is first etched ata low current density of 2 A/dm2for 10 min and then madepassive at 20 A/dm2for 2 min and finally cathodic for 2 or 3 sat 20 A/dm2. See Warning in 4.2. The temperature of thesolution should be kept below 25C. This treatment results inexcellent adhesion, but the amount of etchin

20、g makes it lessdesirable for a highly finished surface.4.4 Anodic Etching in Watts-Type Bath(Nickel removedapproximately 4 m.) This procedure employs an anodictreatment in a low-pH Watts bath for 3 min at 1 A/dm2(10A/ft2), followed by cathodic treatment for 3 to 6 min at 3A/dm2(30 A/ft2). The compos

21、ition of the solution is 240 to 300g/L nickel sulfate (NiSO47H2O), 40 to 60 g/L nickel chloride(NiCl26H2O), and 25 to 40 g/L boric acid. It is operated at atemperature between 25 and 50C and at a pH between 1.5 and2.0. An additional bath is not required if a means of reversingthe current is availabl

22、e. The amount of etching obtained issufficient to dull a bright surface, and there is danger of bathcontamination from bare areas.4.5 Acid-Nickel Chloride Treatment(Nickel removed ap-proximately 1.3 m.) This procedure employs an anodictreatment followed by a cathodic treatment in a low-pH nickelchlo

23、ride solution. The composition of the solution is 240 g/L ofnickel chloride (NiCl26H2O) and 31 mL of concentrated, 37mass % hydrochloric acid (density 1.16 g/mL). The normalprocedure is to make the work anodic for 2 min at 3 A/dm2andthen cathodic for 6 min at the same current density. Where it isnot

24、 possible to reverse the current in the same tank, the twosteps may be carried out in separate tanks. The latter arrange-ment may be more practical commercially. This treatmentproduces a dull finish on a bright surface, but the etching is notsufficiently drastic to preclude finishing with bright nic

25、keldeposit.NOTE 1Nickel anode materials containing greater than 0.01 mass %sulfur are not recommended for use in acid nickel strike baths operatingat pH 0.5, or lower, to avoid oxidation of sulfides by hydrochloric acid.4.6 Etching by Acid Immersion(Nickel removed approxi-mately 1.3 m.) Adequate etc

26、hing may be obtained on somenickel surfaces by a short dip at room temperature in a solutionof either 500 mL of concentrated 37 mass % hydrochloric acid(density 1.18 g/mL) diluted to 1 L, or 150 mL of concentrated96 mass % sulfuric acid (density 1.83 g/mL) diluted to 1 L. See4.2. The length of the i

27、mmersion required may vary from 10 sto 1 min.4.7 Electropolishing Treatment(Nickel removed approxi-mately 1.3 m.) This procedure is commonly employed onrejects that have been repolished to remove the defective area.The electropolishing solution commonly used consists of amixture of 150 mL of 96 mass

28、 % sulfuric acid (density 1.83g/mL) and 630 mL of 85 mass % phosphoric acid (density 1.69g/mL) diluted to 1 L. See Warning in 4.2. Temperature ofsolution ranges from 45 to 55C. The work is made anodic atcurrent densities from 15 to 20 A/dm2. The electropolishingtreatment is usually applied for 2 to

29、15 min. The cathodes maybe electrolytic nickel strip. Subsequent alkaline cleaning andan acid dip are normally used before electroplating.4.8 Cathodic Treatment(Nickel removed nil.) These pro-cedures are recommended where the nickel surface has notbeen severely passivated. Prior cleaning may be requ

30、ired, suchas alkaline soak cleaning or electrocleaning, or both. Ifelectrocleaning is employed, only cathodic current should beused. In the following formulations, 96 mass % sulfuric acidwith a density of 1.83 g/mL, and 37 mass % hydrochloric acidwith a density of 1.16 g/mL, are used.4.8.1 Cathodic

31、Treatment in Sulfuric Acid:Sulfuric acid 30 to 100 mLWater to 1 LTemperature ambient to 45CCurrent density 1 A/dm2Anodes pure leadTime 30 s to 5 min4.8.2 Cathodic Treatment in Hydrochloric Acid:Hydrochloric acid 100 to 300 mLWater to 1 LTemperature ambientCurrent density 1 A/dm2Anodes electrolytic n

32、ickel strip or nickelbar anodesTime 30 s to 5 minNOTE 2In some instances, the use of 2 g/L of ammonium bifluoride(NH4 HF) has been found to be beneficial in either of the aboveformulations.NOTE 3Proprietary acid salt formulations may be used with thesuppliers recommendations.5. Electroplating Proced

33、ures5.1 Wet Freshly Electroplated SurfacesNickel surfacesthat are still wet with electroplating solution can sometimes beplaced directly in the subsequent nickel electroplating bathwithout any special treatment. If the solutions are not compat-ible, a water rinse may be used between nickel baths. Th

34、isprocedure will normally give good adhesion with Watts-typenickel and certain semi-bright nickels but may give pooradhesion with bright nickels. A mild etch, such as a shortimmersion in a dilute acid solution, may be required for somesemi-bright and bright nickel surfaces.5.2 Dry Freshly Electropla

35、ted SurfacesNickel surfacesthat have been allowed to dry following the rinse from theelectroplating bath may only require an activation treatment.However, if there is a possibility of a trace of oil or grease onthe surface, a cathodic alkaline cleaner should be used first. Ashort immersion in a dilu

36、te acid solution should be adequate toactivate most nickel surfaces, but certain bright nickels mayrequire more drastic activation.B 343 92a (2004)e125.3 Polished, Buffed, or Machine Ground SurfaceThesenickel surfaces can usually be treated alike for nickel electro-plating, although the buffed surfa

37、ce will require more drasticdegreasing treatment and alkaline cleaning. For decorativesurfaces, a mild etch, such as a short immersion in a dilute acidor a short anodic treatment in sulfuric acid, should be adequateto assure good adhesion.5.4 Anodic Alkaline Treated SurfaceThe oxide film on anickel

38、surface from anodic treatment in an alkaline solutionmust be removed by a suitable activation treatment before thenickel surface can be electroplated adherently with nickel. Anacid dip or a mild anodic etch in sulfuric acid is usually notadequate. A heavy anodic etch in sulfuric acid, an electropol-

39、ishing treatment, a low-pH nickel bath, or the acid-nickelchloride treatment will normally be required to provide a sounddeposit. A wipe on a buffing wheel will also serve to removethe oxide film.5.5 Rejects with Chromium ElectroplateOn parts requir-ing the removal of chromium for reprocessing, use

40、of an anodicalkaline chromium strip should preferably be avoided. Acidstripping should be used. If an anodic alkaline strip is used,then an anodic acid etch is absolutely necessary.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item

41、mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical commit

42、tee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a mee

43、ting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive,

44、PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).B 343 92a (2004)e13