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ASTM+B+809-1995

Designation:B809–95(Reapproved2003)Standard Test Method forPorosity in Metallic Coatings by Humid Sulfur Vapor (“Flowers-of-Sulfur”)1This standard is issued under theﬁxed designation B809;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.1.Scope1.1This standard covers equipment and test methods for determining the porosity of metallic coatings,where the pores penetrate down to a silver,copper,or copper-alloy substrate.1.2This test method is suitable for coatings consisting of single or combined layers of any coating that does not signiﬁcantly tarnish in a reduced sulfur atmosphere,such as gold,nickel,tin,tin-lead,and palladium,or their alloys.1.3This test method is designed to determine whether the porosity level is less than or greater than some value which by experience is considered by the user to be acceptable for the intended application.1.4Recent reviews of porosity testing and testing methods can be found in the literature.2,3Guide B765is suitable to assist in the selection of porosity tests for electrodeposits and related metallic coatings.Other porosity test standards are Test Methods B735,B741,B798,and B799.1.5The values stated in SI units are to be regarded as the standard.The values given in parentheses are for information only.1.6This 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 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.For speciﬁc hazards statements,see Section8.2.Referenced Documents2.1ASTM Standards:B374Terminology Relating to Electroplating4B542Terminology Relating to Electrical Contacts and Their Use5B735Test Method for Porosity in Gold Coatings on Metal Substrates by Nitric Acid Vapor5B741Test Method for Porosity in Gold Coatings on Metal Substrates by Paper Electrography5B765Guide for Selection of Porosity Tests for Electrode-posits and Related Metallic Coatings4B798Test Method for Porosity in Gold or Palladium Coatings on Metal Substrates by Gel-Bulk Electrography5 B799Test Method for Porosity in Gold and Palladium Coatings by Sulfurous Acid/Sulfur-Dioxide Vapor53.Terminology3.1Deﬁnitions—Many terms used in this test method are deﬁned in Terminologies B374and B542.3.2Deﬁnitions of Terms Speciﬁc to This Standard:3.2.1corrosion products—reaction products of the basis metal or underplate,that protrude from,or are otherwise attached to,the coating surface after the test exposure.3.2.2measurement area—in this test method,that portion or portions of the surface that is examined for the presence of porosity.The measurement area shall be indicated on the drawings of the parts,or by the provision of suitably marked samples.3.2.3metallic coatings—in this test method,include plat-ings,claddings,or other metallic coatings applied to the substrate.The coating can comprise a single metallic layer ora combination of metallic layers.3.2.4porosity—the presence of any discontinuity,crack,or hole in the coating that exposes a different underlying metal (see Guide B765).3.2.5signiﬁcant surface—of a coated part,is that portion (or portions)of the coating surface that is essential to the serviceability or function of the part,or which can be the source of corrosion products or tarnishﬁlms that interfere with the function of the part.For many plated products,the critical surface is identical to the measurement area.3.2.6tarnish—reaction products of copper or silver with oxygen or reduced sulfur(that is,hydrogen sulﬁde(H2S)and elemental sulfur vapor,but not sulfur dioxide(SO2)or other sulfur oxides).They consist of thinﬁlms or spots that do not protrude signiﬁcantly from the surface of the metallic coating (in contrast to corrosion products).1This test method is under the jurisdiction of ASTM Committee B08on Metallicand Inorganic Coatings and is the direct responsibility of Subcommittee B08.10onTest Methods.Current edition approved Feb.10,2003.Published May2003.Originallyapproved st previous edition approved in1995as B809–95.2Clarke,M.,“Porosity and Porosity Tests,”Properties of Electrodeposits,Sard,Leidheiser,and Ogburn,eds.,The Electrochemical Society,1975,p.122.3Krumbein,S.J.,“Porosity Testing of Contact Platings,”Transactions of theConnectors and Interconnection Technology Symposium,Philadelphia,PA,October1987,p.47.4Annual Book of ASTM Standards,V ol02.05.5Annual Book of ASTM Standards,V ol02.04.1Copyright©ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959,United States.3.2.7tarnish creepage—movement of tarnishﬁlms across the surface of the coating,the tarnish having originated either from pores or cracks in the coating or from areas of bare silver, copper,or copper alloy near the measurement area(as in a cut edge).3.2.8underplate(s)—a metallic coating layer(s)between the substrate and the topmost layer or layers.The thickness of an underplate is usually greater than1µm(40µin.).4.Summary of Test Method4.1The test specimens are suspended over“ﬂowers-of-sulfur”(powdered sulfur)in a vented container at controlled elevated relative humidity and temperature.Elemental sulfur vapor,which always exists in equilibrium with sulfur power in a closed system,attacks any exposed silver,copper,or copper alloy,such as at the bottom of pores.Brown or black tarnish spots indicate porosity.4.2Exposure periods may vary,depending on the extent of porosity to be revealed.4.3This test involves tarnish or oxidation(corrosion)reac-tions in which the products delineate defect sites in coatings. Since the chemistry and properties of these products may not resemble those found in natural or service environments,this test is not recommended for prediction of product performance unless correlation isﬁrst established with service experience (but see5.3).5.Signiﬁcance and Use5.1A major use of this test procedure is for determining coating quality.Porosity tests are indications of the complete-ness of protection or coverage offered by the coatings,since the coatings described in1.2are intended to be protective when properly applied.The porosity test results are therefore a measure of the deposition process control.5.2A particular purpose of the humid sulfur vapor test is for determining the quality of underplates of nickel or nickel alloy in thoseﬁnish systems that have thin,1.2µm or less(50µin.or less)top layers above the nickel,since porosity in the under-plate usually continues into such top layers.5.3The humid sulfur vapor test is often used as an envi-ronmental test to simulate many indoor humid atmosphere tarnishing and tarnish creepage effects.However,the chemistry and properties of these tarnishﬁlms may not resemble those found in other service environments.For such product perfor-mance evaluations,the test should only be used in combination with other performance evaluation tests,as speciﬁed in the referencing document for that product.5.4Porosity tests differ from corrosion and aging tests,since the latter are intended to measure the chemical inertness of the coating.In contrast,in a good porosity test procedure the corrosive agent should not attack the coating.It must instead, clean,depolarize,or activate the substrate metal exposed by the pore,or both,and attack it sufficiently to cause reaction products toﬁll the pore to the surface of the coating.5.5The humid sulfur test is highly sensitive,and is capable of detecting virtually all porosity that penetrates down to copper or copper alloys.Since nickel is not attacked by moist sulfur vapor at100°C or less,this test will not detect pores or cracks in the top coating if such pores or cracks do not penetrate through the nickel underplate overlaying the copper.5.6The level of porosity in the coating that may be tolerable depends on the severity of the environment that the product is likely to encounter during service or storage.Also,the location of the pores on the surface is important.If the pores are few in number or away from the signiﬁcant surfaces,their presence can often be tolerated.5.7The present test method can be used on samples of various geometries,such as curved surfaces.It can also be used for selective area coatings,if allowance is made for tarnish creepage from bare copper alloy areas.5.8This test method is destructive in that it reveals the presence of porosity by contaminating the surface with tarnish ﬁlms.Any parts exposed to this test method should not be placed in service.5.9The relationship of porosity levels revealed by this test method to product performance and service life must be made by the user of the test through practical experience or by judgment.Thus,absence of porosity in the coating may be a requirement for some applications,while a few pores on the signiﬁcant surfaces may be acceptable for others.6.Apparatus6.1Test Vessel—May be any convenient-size vessel of glass,acrylic-resin(or of any other material that is not affected by high humidity or sulfur),such as a glass desiccator of9to 10L capacity.It should have a lid or cover capable of being plugged with a stopper.The stopper shall have a1to4mm diameter hole through it to serve as a vent.6.2Sample Fixture or Holders—Supports or hangers shall be made from material such as glass or acrylic plastic that will not be affected by sulfur or high humidity,and shall be arranged so that the samples will be at least75mm away from the humidity controlling solution or sulfur powder(see6.3). The samples shall also be at least25mm from the vessel walls and at least10mm from other samples or other surfaces.Do not use a desiccator plate.Theﬁxture shall not cover more than 20%of the vessel’s cross-sectional area so that air movement within the vessel will not be restricted during the test.6.3Glass Dish—Petri or other shallow dish approximately 15cm in diameter to hold powdered sulfur.Dish may be supported above the constant humidity solution with plastic blocks,orﬂoated on the liquid.6.4Oven,Air-circulating,capable of maintaining test vessel at a temperature of5062°C(12264°F).6.5Temperature and Relative Humidity(RH)Sensor,with a remote sensor probe having a range of approximately76to 95%RH at50°C,which can be kept in the desiccator during test.66.6Microscope,Optical,Stereo,103—It is preferred that one eyepiece contain a graduated reticle for measuring the diameter of tarnish spots.The reticle shall be calibrated for the magniﬁcation at which the microscope is to be used.6.7Light Source,incandescent or circularﬂuorescent.6The Hygrodynamics Hygrometer,manufactured by Newport Scientiﬁc,Inc., has been found satisfactory for thispurpose.7.Reagents7.1Potassium Nitrate (KNO 3)—American Chemical Soci-ety analyzed reagent grade,or better.7.2Sulfur,Sublimed (“Flowers-of-Sulfur”),N.F.or labora-tory grade.78.Safety and Health Precautions8.1All of the normal precautions shall be observed in handling the materials required for this test.This shall also include,but not be limited to,procuring and reviewing material Safety Data Sheets (MSDS)that meet the minimum require-ments of the U.S.Occupational Safety and Health Administra-tion (OSHA)Hazard Communication Standard for all chemi-cals used in cleaning and testing,and observing the recommendations given.9.Procedure9.1Equilibration of Test Vessel —For the initial series of tests,the test vessel shall be prepared for equilibration at least a day before the ﬁrst exposure.N OTE 1—For all subsequent tests,the initial 24-h equilibration proce-dures do not have to be repeated (see Note 2and 9.8).9.1.1Place the test vessel in the oven,with sample supports in place.Make a saturated solution of potassium nitrate,prepared by adding approximately 200g of the salt to approximately 200mL of deionized water,with stirring,and place it in the bottom of the vessel.N OTE 2—The saturated solution will contain undissolved potassium nitrate salt.This condition is necessary to achieve a constant humidity atmosphere above the solution.9.1.2Place lid on the vessel (do not seal it with grease),insert the temperature-humidity probe through the opening in the top of the lid (leave the stopper out),and set the oven to 55°C.9.1.3During equilibration,open desiccator occasionally and stir contents.As the temperature in the vessel approaches 50°C (122°F),as indicated by the temperature probe,adjust oven temperature as needed to stabilize the vessel at 50°C.9.1.4Fill the glass dish half-full with sulfur (break up any large lumps),and place the dish on supports above the potassium nitrate solution or ﬂoat the dish directly on the solution (see Fig.1).9.1.5Replace the lid and insert the vented stopper in the lid opening.Monitor the vessel temperature over several hours,and adjust oven temperature as needed to keep the vessel at 5062°C (12264°F).When stability has been attained,and the relative humidity is in the 86to 90%range,the apparatus is ready for insertion of test samples.N OTE 3—The system described in this section may be reused for many subsequent tests without replacing the chemicals,and will remain stable for up to 6months as long as the chemicals do not become contaminated with corrosion products or dirt.If allowed to cool,the potassium nitrate mixture will solidify,but it will liquify again when the vessel is reheated and the solution stirred.Crusts and lumps of hardened potassium nitrate should be broken up and stirred into the slurry.Add a few millilitres of deionized water if necessary to return the solution to its original condition.9.2Preparation of Test Samples :9.2.1Handle samples as little as possible,even prior to cleaning,and only with tweezers,microscope lens tissue,or clean soft cotton gloves.9.2.2Prior to being cleaned,the samples shall be prepared so that the measurement areas may be viewed easily through the microscope.If samples are part of assembled products,they may need to be disassembled to ensure proper access to these areas by the test environment.Since the test is speciﬁc to the planted metallic portions of the product,the latter should be separated from plastic housings,etc.,whenever possible,prior to cleaning.Also,nonmetallic materials,such as paper tags,string,tape,etc.,shall be removed,but take care to maintain sample identity.9.2.3Cleaning :9.2.3.1Inspect the samples under 103magniﬁcation for evidence of particulate matter.If present,such particles should7Fisher catalogue no.S-591or WWR Scientiﬁc catalogue no.JT4088have been found satisfactory for thispurpose.FIG.1Typical Test EquipmentSetupbe removed by“dusting”(that is,blowing them off the sample) with clean,oil-free air.N OTE4—An aerosol-can“duster”or a photographer’s brushblower are convenient tools for this purpose.9.2.3.2Thoroughly clean the particle-free samples with solvents or solutions that do not contain CFCs,chlorinated hydrocarbons,or other known ozone-destroying compounds. The procedure outline in Note5has been found to give satisfactory results for coatings with mild to moderate surface contamination.N OTE5—Suggested cleaning procedure:(1)Keep individual pieces separated if there is a possibil-ity of damage to the measurement areas during the various cleaning steps.(2)Clean samples for5min in an ultrasonic cleaner that contains a hot(65to85°C)2%aqueous solution of a mildly alkaline(pH7.5to10)detergent.(3)After ultrasonic cleaning,rinse samples thoroughly under warm running tap water for at least5s.(4)Rinse samples ultrasonically for2min in fresh deionized water to remove the last detergent residues.(5)Immerse in fresh analytical reagent-grade methanol or isoropanol,and ultrasonically agitate for at least30s in order to remove the water from the samples.(6)Remove and dry samples until the alcohol has com-pletely evaporated.If an air blast is used as an aid to drying,the air shall be oil free,clean,and dry.(7)do not touch the measurement area of the samples with bareﬁngers after cleaning.9.2.3.3Reinspect the samples(under103magniﬁcation) for particulate matter on the surface.If particulates are found, repeat the cleaning step.Surface cleanliness is extremely important.Contaminants,such as plating salts andﬂakes of metal,may give erroneous indications of porosity.9.3Place the clean samples in the test vessel,in as quick a manner as possible,in order to minimize deviations from equilibrium conditions.A clean,unplated copper or copper-alloy panel should also be put into the vessel each time a test is run as an internal control,that is,to show that the test system is operative.The copper should start to darken within a few hours.9.4During theﬁrst1to2h of the test run,leave the desiccator slighlty open,by removing the vented stopper,in order to prevent moisture condensation while the system is coming to test temperature.When the test temperature is reached and the relative humidity is in the86to90%range (which may take1to2h),replace the vented stopper.9.5During theﬁrst2to3h of exposure,check temperature and humidity in the desiccator and record it at suitable intervals in order to ensure the attainment of equilibrium conditions.The same shall be done towards the end of the test.9.6Continue the test for the required time;this shall be24 h,unless otherwise speciﬁed.The test system may be left overnight(or over the weekend for a3-day test),without further monitoring.9.7At the end of the test,remove the samples,replace the vessel lid,and allow the samples to cool to room temperature before examining them.9.8For all subsequent runs,eliminate the procedure de-scribed in9.1.However,make routine checks of the actual temperature and humidity within the vessel;occasional stirring of the potassium nitrate solution may be required before a new run.10.Examination and Evaluation10.1Examine the measurement areas at103magniﬁcation using an incandescent or circularﬂuorescent lamp.The pres-ence of brown or black tarnish spots indicates that theﬁnish is porous at these sites down to the silver or copper-alloy substrate.10.2If the pore sites are to be counted,the following may be useful as an aid to counting:10.2.1Count only tarnish and corrosion products that are brown to black.10.2.2Do not consider loose contamination that can easily be removed by mild air dusting as tarnish or corrosion products.10.2.3Move sample around under the light to vary the angle to verify pore indications.Burnished gold can give the appear-ance of black spots.10.3Measure and count a tarnish or corrosion spot when at least three-quarters of the spot falls within the measurement area.Tarnish creepageﬁlms which initiate outside the mea-surement area but fall within it,shall not be counted(see Fig.2).However,the presence of signiﬁcant tarnish creepage should be recorded and its location given.10.4Pore size shall be deﬁned by the longest diameter of the corrosion product.Unless otherwise speciﬁed,corrosion products smaller than0.05mm(0.002in.)in diameter shall not be counted.A graduated reticle in the microscope eyepiece is useful as an aid to counting and sizing.N OTE6—A useful sizing technique is to tabulate the pores in accor-dance with three size ranges:These are,approximately:(a)0.12mm (0.005in.)diameter or less,(b)between0.12and0.40mm(0.005and 0.015in.)diameter,and(c)greater than0.4mm(0.015in.)diameter. 10.5The acceptable number,size,and location of these tarnish or corrosion spots shall be as speciﬁed in the appropri-ate drawing orspeciﬁcationFIG.2Corrosion Products at Boundaries of MeasurementArea11.Precision and Bias11.1Precision —The precision of this test method is being investigated using gold-plated and nickel-plated coupons.11.2Bias —The porosity of commercially produced metalliccoatings is a property with potentially large sample-to-sample variability.8Since there is no acceptable reference material suitable for determining the bias for porosity testing,no statement on bias is being made.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this ers of this standard are expressly advised that determination of the validity of any such patent rights,and the risk of infringement of such rights,are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every ﬁve years and if not revised,either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,which you may attend.If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards,at the address shown below.This standard is copyrighted by ASTM International,100Barr Harbor Drive,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 above address or at 610-832-9585(phone),610-832-9555(fax),or service@ (e-mail);or through the ASTM website ().8Krumbein,S.J.,and Holden,Jr.,C.A.,“Porosity Testing of Metallic Coatings,”Testing of Metallic and Inorganic Coatings,ASTM STP 947,Harding,W.B.,and DiBari,G.A.,eds.,ASTM,1987,p.193.。

Nanostructured Electrode Materials for Lithium-Ion Batteries

Nanostructured Electrode Materials for Lithium -Ion BatteriesA.Manthiram and T.MuraliganthAbstract Electrochemical energy storage systems are becoming increasingly important with respect to their use in portable electronic devices,medical implant devices,hybrid electric and electric vehicles,and storage of solar and wind ener-gies.Lithium-ion batteries are appealing for these needs because of their high energy density,wide range of operating temperatures,and long shelf and cycle life. However,further breakthroughs in electrode materials or improvements in existing electrode materials are critical to realize the full potential of the lithium-ion tech-nology.Nanostructured materials present an attractive opportunity in this regard as they could offer several advantages such as fast reaction kinetics,high power density,good cycling stability with facile strain relaxation compared to their bulk counterparts.In this chapter,we present an overview of the latest progress on the nanostructured anode and cathode materials for lithium-ion batteries. IntroductionEnergy storage and production is one of the greatest challenges facing human kind in the twenty-ﬁrst century.Based on moderate economic and population growth, the global energy consumption is anticipated to triple by the year2010.The rapid depletion of fossil fuel reserves,increasing fuel costs,increasing greenhouse gas emission,and global climate changes are driving the development of sustainable clean energy technologies like fuel cells,solar cells,high energy density batteries, and supercapacitors.While fuel cells and solar cells are energy conversion devices, batteries and supercapacitors are energy storage devices.Nearly one-third of the total energy consumption in the United States is by the transportation sector,and internal combustion engine based automobiles are a sig-niﬁcant contributor of green house gas emission.Hybrid electric vehicles(HEV) and plug-in hybrid electric vehicles(PHEV)are the most viable near-term option A.Manthiram(B)Materials Science and Engineering Program,The University of Texas,Austin,TX78712,USAe-mail:rmanth@211 A.Korkin et al.(eds.),Nanotechnology for Electronics,Photonics,and RenewableEnergy,Nanostructure Science and Technology,DOI10.1007/978-1-4419-7454-9_8,C Springer Science+Business Media,LLC2010212 A.Manthiram and T.Muraliganth Fig.8.1Comparison of theenergy densities of differentbattery systemsfor transportation.Energy storage is also critical for the efﬁcient utilization of the electricity produced from solar and wind energies.Lithium-ion batteries are appeal-ing for automobiles(HEV and PHEV)and the storage of solar and wind energy as they provide higher energy density compared to other rechargeable battery systems such as lead acid,nickel–cadmium,and nickel metal hydride batteries as seen in Fig.8.1[1].However,cost and safety are the major issues with respect to large-scale applications like automobiles and solar and wind energy storage,and they need to be adequately addressed.Lithium-Ion BatteriesRechargeable lithium batteries involve a reversible insertion/extraction of lithium ions into/from a host electrode material during the charge/discharge process.The lithium insertion/extraction process occurring with aﬂow of ions through the elec-trolyte is accompanied by a reduction/oxidation(redox)reaction of the host matrix assisted with aﬂow of electrons through the external circuit(Fig.8.2).The open-circuit voltage V oc of such a lithium cell is given by the difference in the lithium chemical potential between the cathode(μLi(c))and the anode(μLi(a))asV oc=(μLi(c)−μLi(a))/F,(8.1) where F is the Faraday constant.A schematic energy diagram of a cell at open circuit is given in Fig.8.3.The cell voltage is determined by the energies involved in both the electron transfer and Li+transfer.While the energy involved in electron transfer is related to the work functions of the cathode and the anode,the energy involved in Li+transfer is determined by the crystal structure and the coordination geometry of the site into/from which the Li+ions are inserted/extracted[2].Thermodynamic stability considerations require the redox energies of the cathode(E c)and anode8Nanostructured Electrode Materials for Lithium-Ion Batteries213 Fig.8.2Illustration of thecharge–discharge processinvolved in a lithium-ion cellconsisting of graphite as ananode and layered LiCoO2asa cathodeFig.8.3Schematic energydiagram of a lithium cell atopen circuit.HOMO andLUMO refer,respectively,tothe highest occupiedmolecular orbital and lowestunoccupied molecular orbitalin the electrolyte(E a)to lie within the band gap E g of the electrolyte,as shown in Fig.8.3,so that no unwanted reduction or oxidation of the electrolyte occurs during the charge–discharge process.With this strategy,the anode and cathode insertion hosts should have,respectively,the lowest and highest voltages vs.metallic lithium in order to maximize the cell voltage.The concept of rechargeable lithium batteries wasﬁrst illustrated with a transition metal sulﬁde TiS2as the cathode,metallic lithium as the anode,and a nonaque-ous electrolyte[3].Following the initial demonstration,several other sulﬁdes and chalcogenides were pursued during the1970s and1980s as cathodes[4].However, most of them exhibit a low cell voltage of<2.5V vs.lithium anode.This limita-tion in cell voltage is due to an overlap of the higher valent M n+:d band with the top of the nonmetal:p band—for example,with the top of the S:3p band as shown in Fig.8.4.Such an overlap results in an introduction of holes into(or removal of electrons from)the S2−:3p band and the formation of molecular ions such as S2−2,214 A.Manthiram and T.Muraliganth Fig.8.4Relative energies ofmetal:d(for example,Co:3d)and nonmetal:p in(a)asulﬁde and(b)an oxidewhich in turn leads to an inaccessibility of higher oxidation states for M n+in a sul-ﬁde Li x M y S z.The stabilization of higher oxidation state is essential to maximize the cell voltage.Recognizing this difﬁculty with chalcogenides,Goodenough’s group at the University of Oxford focused on oxide cathodes during the1980s[5–7].The location of the top of the O2−:2p band much below the top of the S2−:3p band and a larger raising of the M n+:d energies in an oxide compared to that in a sulﬁde due to a larger Madelung energy(Fig.8.4)make the higher valent states accessible in oxides. For example,while Co3+can be readily stabilized in an oxide,it is difﬁcult to sta-bilize Co3+in a sulﬁde since the Co2+/3+redox couple lies within the S2−:3p band as seen in Fig.8.4.Accordingly,several transition metal oxide hosts crystallizing in a variety of structures(two-dimensional layered and three-dimensional framework structures)have been pursued during the past two decades.Among them LiCoO2, LiNiO2,and LiMn2O4oxides having a high electrode potential of4V vs.metallic lithium have become attractive cathodes for lithium-ion cells.On the other hand, graphite with a low electrode potential of<0.3V vs.metallic lithium has become an attractive anode.Although the initial efforts in rechargeable lithium batteries employed lithium metal as the anode,the strategy failed to attain commercial success due to safety limitations[8,9].The inherent instability of lithium metal and the dendrite for-mation during charge–discharge cycling eventually forced the use of intercalation compounds as anodes.This led to the commercialization of the lithium-ion battery technology by Sony in1990with LiCoO2as the cathode and graphite as the anode. However,the cost and safety issues and the performance limitations associated with the LiCoO2cathode and carbon anode have prompted the search for new electrode materials as well as improvements in existing electrode materials.Nanostructured materials have attracted a lot of interest in the past two decades because of their unusual electrical,mechanical,and optical properties compared to their bulk counterparts[10–15].Recently,nanostructured materials are also gaining increasing popularity for energy storage applications[16–21].This chapter focuses on providing an overview of some of the recent advances in nanostructured anode and cathode materials for lithium-ion batteries.8Nanostructured Electrode Materials for Lithium-Ion Batteries215 Nanostructured Electrode Materials for Lithium-Ion Batteries Nanomaterials offer advantages and disadvantages as electrode materials for lithium-ion batteries.Some of the advantages are given below:•The smaller particle size increases the rate of lithium insertion/extraction because of the short diffusion length for lithium-ion transport within the particle,resulting in enhanced rate capability.•The smaller particle size enhances the electron transport in the electrode, resulting in enhanced rate capability.•The high surface area leads to enhanced utilization of the active materials, resulting in higher capacity.•The smaller particle size aids a better accommodation of the strain during lithium insertion/extraction,resulting in improved cycle life.•The smaller particle size enables reactions that could not otherwise occur with micrometer-sized particles,resulting in new lithium insertion/extraction mechanisms and improved electrochemical properties and performances.Some of the disadvantages are given below:•Complexities involved in the synthesis methods employed could increase the processing cost,resulting in higher manufacturing cost.•The high surface area may lead to enhanced side reactions with the electrolyte, resulting in high irreversible capacity loss and capacity fade during cycling.•The smaller particle size and high surface-to-volume ratio could lead to low packing density,resulting in low volumetric energy density.Nanostructured CathodesNanostructured Layered Oxide CathodesOxides with the general formula LiMO2(M=V,Cr,Co,and Ni)crystallize in a layered structure in which Li+and M3+ions occupy the alternate(111)planes of the rock salt structure to give a layered sequence of-O-Li-O-M-O-along the c axis.The Li+and M3+ions occupy the octahedral interstitial sites of the cubic close-packed oxygen array as shown in Fig.8.5.The structure with strongly(cova-lently)bonded MO2layers allows a reversible extraction/insertion of lithium ions from/into the lithium planes.The lithium-ion movement between MO2layers pro-vides fast two-dimensional lithium-ion diffusion[22],and the edge-shared MO6 octahedral arrangement with a direct M–M interaction provides good electronic conductivity.LiCoO2is the most commonly used transition metal oxide cathode in commercial lithium-ion batteries.It has been used because of its high operating voltage(4V),ease of synthesis,and good cycle life.However,only50%(~140mAh g−1)of the theoretical capacity of LiCoO2can be utilized in practical lithium-ion216 A.Manthiram and T.Muraliganth Fig.8.5Crystal structure oflayered LiCoO2cells due to structural and chemical instabilities at deep charge with(1−x)<0.5in Li1−x CoO2as well as safety concerns[23,24].Moreover the element cobalt is toxic and expensive.In this regard,LiNiO2provides an important advantage compared to LiCoO2since Ni is less expensive and less toxic than Co.However,it suffers from a few problems:(i)difﬁculty to synthesize LiNiO2with all Ni3+and as a perfectly ordered phase without a mixing of Li+and Ni3+ions in the lithium plane[25–27], (ii)Jahn–Teller distortion(tetragonal structural distortion)associated with the low-spin Ni3+:d7(t62g e1g)ion[28,29],and(iii)exothermic release of oxygen at elevated temperatures and safety concerns in the charged state[30,31].As a result,LiNiO2 is not a promising material for lithium-ion cells.However,some of these difﬁculties have been overcome by a partial substitution of Co for Ni forming LiNi1−y Co y O2 [32].For example LiNi0.85Co0.15O2has been found to deliver a high capacity of ~180mAh g−1with good cyclability.In general,LiCoO2and LiNi1−y Co y O2are prepared by solid-state reactions at high temperatures(800–900◦C)[33].The high-temperature method usually results in larger particles and often in irregular morphology and a broad particle size distribution.A number of synthetic routes such as sol–gel,co-precipitation,and emulsion methods have been pursued over the years to synthesize nanostructured layered oxides[34–38].Decreasing the particle size to nanometer range signiﬁ-cantly shortens the lithium-ion diffusion distance and improves the rate performance of the layered oxide cathodes.However,the large surface area of the nanoparticles incurs undesirable side reactions with the electrolyte,especially at higher operating voltages.This effect could be minimized by having nano-sized primary particles agglomerating into micron-sized secondary particles.In this regard,template-assisted methods with the use of porous anodic aluminum oxide have been used to prepare LiCoO2nanotubes with lengths up to several8Nanostructured Electrode Materials for Lithium-Ion Batteries217 Fig.8.6Firstcharge–discharge proﬁles ofsolid solutions betweenlayered Li[Li1/3Mn2/3]O2andLi[Ni1−y−z Mn y Co z]O2micrometers and diameter around200nm[39].Since the rate-determining stepin LiCoO2electrodes is the solid-state lithium-ion diffusion,decreasing the par-ticle size can signiﬁcantly improve the kinetics because of shorter lithium diffusionlength.Accordingly,LiCoO2with a nanotube architecture has been found to exhibitimproved rate performance compared to the conventional LiCoO2[40].Recently,solid solutions between Li[Li1/3Mn2/3]O2(commonly known asLi2MnO3)and LiMO2(M=Mn0.5Ni0.5,Co,Ni,and Cr)have become appeal-ing as they exhibit a high reversible capacity of around250mAh g−1with a lowercost and better safety compared to the LiCoO2cathode[41–45].This capacity isnearly two times higher than that found with the LiCoO2cathode.However,theLi2MnO3−LiMO2solid solutions have a few drawbacks.First,they lose oxygen irreversibly from the lattice duringﬁrst charge as indicated by a voltage plateauat4.5V following an initial sloping region corresponding to the oxidation of thetransition metal ions to4+oxidation state as seen in Fig.8.6.This leads to a largeirreversible capacity loss in theﬁrst cycle.Second,these oxides suffer from poorrate capability,impeding their high-power applications.Decreasing the lithium-ion diffusion distance and having a high surface areananostructure could enhance their rate performance.Especially,one-dimensionalnanowire morphology could be beneﬁcial compared to nanoparticles.Accordingly,Li[Ni0.25Li0.15Mn0.6]O2nanowires with a diameter of around30nm and a highaspect ratio of around100have been synthesized via a template-free hydrother-mal method.Interestingly,the Li[Ni0.25Li0.15Mn0.6]O2sample thus prepared hasbeen found to deliver a stable cycle life and superior rate performance with a highdischarge capacity of around260mAh g−1at7C rate[46].Surface-Modifie(Nanocoating)Layered Oxide CathodesAs pointed out in the earlier section,only50%of the theoretical capacity of layeredLiCoO2cathode could be utilized in practical lithium-ion cells due to the chemi-cal instability in contact with the electrolyte for(1−x)<0.5in Li1−x CoO2[23,24].One way to suppress the chemical reactivity is to coat or modify the surfaceof the cathode with other inert oxides.In fact,surface modiﬁcation of the layered218 A.Manthiram and T.Muraliganth LiCoO2cathode with nanostructured oxides like Al2O3,TiO2,ZrO2,SiO2,MgO, ZnO,and MPO4(M=Al and Fe)has been found to increase the reversible capacity of LiCoO2from~140mAh g−1to about200mAh g−1,which corresponds to a reversible extraction of~0.7lithium per formula of LiCoO2[47–54].The surface modiﬁcation suppresses the reaction of the cathode surface with the electrolyte and thereby decreases the impedance growth of the cathode and improves the capac-ity retention.This clearly demonstrates that the limitation in practical capacity of LiCoO2is primarily due to the chemical instability at deep discharge and not due to the structural(order–disorder)transition at(1−x)=0.5.However,the long-term performance of these nano-oxide-coated cathodes will rely on the robustness of the coating.In addition to the improvement in electrochemical properties,nanocoating of AlPO4on LiCoO2has also been found to improve the thermal stability and safety of LiCoO2cathodes[55].As indicated in the previous section,solid solutions between layered Li2MnO3 and Li[Ni1−y−z Mn y Co z]O2exhibit a huge irreversible loss duringﬁrst cycle.The large irreversible capacity loss is observed to be due to the extraction of lithium as “Li2O”in the plateau region as shown in Fig.8.6and an elimination of the oxygen vacancies formed to give an ideal composition“MO2”at the end of theﬁrst charge, resulting in less number of lithium sites available for lithium insertion/extraction during subsequent cycles[43,56].However,a careful analysis of theﬁrst charge–discharge capacity values in our laboratory with a number of compositions suggests that part of the oxygen vacancies should be retained in the lattice to account for the high discharge capacity values observed in theﬁrst cycle[57].More importantly,it was found that the irreversible capacity loss in theﬁrst cycle can be reduced signiﬁ-cantly by coating these layered oxide solid solutions with nanostructured Al2O3and AlPO4[44,57].Figure8.7shows the TEM images of AlPO4-coated layered oxide, in which the thickness of the AlPO4coating is around5nm.Figure8.8a and b compares theﬁrst charge–discharge proﬁles and the corresponding cyclability data of a series of solid solutions between lay-ered Li[Li1/3Mn2/3]O2and Li[Ni1/3Mn1/3Co1/3]O2before and after surfaceFig.8.7TEM image of4wt.%nano-AIPO4-modiﬁedLi[Li0.2Mn0.54Ni0.13Co0.13]O2cathode8Nanostructured Electrode Materials for Lithium-Ion Batteries219Fig.8.8(a)First charge–discharge proﬁles of the layered(1−x)Li[Li1/3Mn2/3]O2−x Li[Ni1/3Mn1/3Co1/3]O2solid solutions before and after surface modiﬁcation with3wt.% nanostructured Al2O3,followed by heating at400◦C(b)Cyclability of the layered(1−x)Li[Li1/3Mn2/3]O2−x Li[Ni1/3Mn1/3Co1.3]O2solid solutions before and after surface modiﬁ-cation with3wt.%nanostructured Al2O3,followed by heating at400◦Cmodiﬁcation with nanostructured Al2O3[44].The surface-modiﬁed samples exhibit lower irreversible capacity loss and higher discharge capacity values than the pris-tine layered oxide samples.This improvement in surface-modiﬁed samples has been explained on the basis of the retention of more oxygen vacancies in the layered lattice after theﬁrst charge compared to that in the unmodiﬁed samples[57–59]. The bonding of the nano-oxides to the surface of the layered oxide lattice sup-presses the diffusion of oxygen vacancies and their elimination.Remarkably,the surface-modiﬁed(1−x)Li[Li1/3Mn2/3]O2−x Li[Ni1/3Mn1/3Co1/3]O2composition with x=0.4exhibits a high discharge capacity of~280mAh g−1,which is two times higher than that of LiCoO2.Moreover,the surface-modiﬁed cathodes have been found to exhibit higher rate capability than the unmodiﬁed samples despite the electronically insulating nature of the coating materials like Al2O3and AlPO4 [59].This is believed to be due to the suppression of the formation of thick solid-electrolyte interfacial(SEI)layers as the coating material minimizes the direct reaction of the cathode surface with the electrolyte at the high charging voltages.However,these layered oxide solid solutions have to be charged up to about 4.8V,so more stable,compatible electrolytes need to be developed to fully exploit their potential as high energy density cathodes.Moreover,oxygen is lost irreversibly from the lattice duringﬁrst charge,and it may have to be vented appropriately during cell manufacturing.Also,the long-term cyclability of these high-capacity cathodes needs to be fully assessed.220 A.Manthiram and T.Muraliganth Nanostructured Spinel Oxide CathodesOxides with the general formula LiMn2O4(M=Ti,V,and Mn)crystallize in the normal spinel structure(Fig.8.9)in which the Li+and the M3+/4+ions occupy, respectively,the8a tetrahedral and16d octahedral sites of the cubic close-packed oxygen array.A strong edge-shared octahedral[M2]O4array permits reversible extraction of the Li+ions from the tetrahedral sites without collapsing the three-dimensional[M2]O4spinel framework.While an edge-shared MO6octahedral arrangement with direct M–M interaction provides good electrical conductivity,the interconnected interstitial(lithium)sites in the three-dimensional spinel framework provide good lithium-ion conductivity.Fig.8.9Crystal structure ofspinel LiMn2O4As a result,spinel LiMn2O4has become an attractive cathode.Moreover,the element Mn is inexpensive and environmentally benign compared to Co and Ni involved in the layered oxide cathodes.However,LiMn2O4delivers only a limited capacity of around120mAh g−1at an operating voltage of4V.Moreover,LiMn2O4 tends to exhibit capacity fade particularly at elevated temperatures(55◦C).Several factors such as Jahn–Teller distortion occurring on the surface of the particles under conditions of nonequilibrium cycling[60,61],manganese dissolution into the elec-trolyte[62,63],formation of two cubic phases in the4V region,loss of crystallinity [64],and development of micro-strain[65]during cycling have been suggested to be the source of capacity fade.Several strategies have been pursued to overcome the capacity fade of LiMn2O4.The most signiﬁcant of them is cationic substitution to give LiMn2−y M y O4(M=Li,Cr,Co,Ni,and Cu)to suppress the difﬁculties of Jahn–Teller distortion and manganese dissolution[66].Decreasing the particle size to nanometer level can enhance the power perfor-mance of LiMn2O4cathodes further.As a result,a variety of synthetic approaches such as sol–gel[67],solution phase[68],mechanochemical[69],spray pyrolysis [70],and templating methods[71]have been pursued to synthesize nano-sizedLiMn2O4.Recently,single-crystalline LiMn2O4nanorods obtained by usingβ-MnO2nanorods synthesized by hydrothermal reaction have been shown to exhibit high power performance[72].However,the application of nanometer-sized spinel particles for practical lithium-ion batteries is not favorable as the high interfacial contact area between the electrode and the electrolyte will aggravate the dissolution of manganese from the spinel lattice into the electrolyte and increase the capacity fade further. Nano-oxide-Coated Spinel CathodesAs pointed out in the previous section,the major issue with the LiMn2O4spinel cathode is the Mn dissolution from the lattice in contact with the electrolyte. Consequently,coating of the LiMn2O4spinel cathode with nanostructured oxides like Al2O3,TiO2,ZrO2,SiO2,MgO,and ZnO has been found to suppress the Mn dissolution from the spinel lattice in contact with the electrolyte and improve the capacity retention[73–75].Another drawback with the spinel LiMn2O4cathode is the lower energy den-sity compared to the layered oxide cathodes.In this regard,the LiMn1.5Ni0.5O4 spinel cathode is appealing as it offers a discharge capacity of around130mAh g−1at a higher voltage of~4.7V vs.lithium.However,the spinel LiMn1.5Ni0.5O4 encounters the formation of NiO impurity during synthesis and the ordering between Mn4+and Ni2+leads to inferior performance compared to the disordered phase [76].It has been found that the formation of the NiO impurity phase and order-ing can be suppressed by appropriate cation doping as in LiMn1.5Ni0.42Zn0.08O4 and LiMn1.42Ni0.42Co0.16O4[77].One major concern with the spinel LiMn1.5Ni0.5O4cathode is the chemical sta-bility in contact with the electrolyte at the higher operating voltage of4.7V.To overcome this difﬁculty,surface modiﬁcation of LiMn1.42Ni0.42Co0.16O4cathodes with oxides like AlPO4,ZnO,Al2O3,Bi2O3have been carried out(Fig.8.10)[78]. The surface-modiﬁed cathodes exhibit better cyclability and rate capability com-pared to the pristine unmodiﬁed samples as shown in Figs.8.11and8.12.The surface coating not only acts as a protection shell between the active cathode mate-rial surface and the electrolyte,but also offers fast lithium-ion and electron diffusion channels compared to the SEI layer formed by a reaction of the cathode surface with the electrolyte,resulting in enhanced cycle life and rate performance.X-ray photoelectron spectroscopic(XPS)analysis has shown that the surface modiﬁcation indeed suppresses the formation of thick SEI layers and thereby improves the rate capability[78].Moreover,the surface modiﬁcation helps to maintain the high rate capability as the cathodes are cycled compared to the unmodiﬁed cathode,resulting in better rate capability retention during long-term cycling. Nanostructured Polyanion-Containing CathodesA major drawback with cathodes containing highly oxidized redox couples like Co3+/4+and Ni3+/4+is the chemical instability at deep charge and the associatedFig8.10High-resolution TEM images of2wt.%(a)Al2O3-,(b)ZnO-,(c)Bi2O3-,and AlPO4-coated LiMn1.42Ni0.42Co0.16O4Fig.8.11Cycling2wt.%Al2O3-,ZnO-,Bi2O3-,and AlPO4-coatedLiMn1.42Ni0.42Co0.16O4safety problems.Recognizing this,oxides like Fe2(XO4)3that contain the polyanion (XO4)2−(X=S,Mo,and W)and crystallizing in the NASICON-related three-dimensional framework structures were shown in the1980s to exhibitﬂat discharge voltage proﬁles at3.0or3.6V[79,80].In these structures,the FeO6octahedrashare corners with SO4tetrahedra with a Fe-O-S-O-Fe linkage and lithium ionsFig.8.12Comparison of therate capabilities and ratecapability retentions ofLiMn1.42Ni0.42Co0.16O4before and after coating with2wt.%Al2O3,ZnO,Bi2O3,and AlPO4:(a)normalizeddischarge capacity at3rdcycle.(b)normalizeddischarge capacity at50thcyclecould be inserted into the interstitial voids of the framework.Although the lower valent Fe2+/3+couple in a simple oxide like Fe2O3would be expected to offer a lower discharge voltage of<3V,a higher voltage of3.6V is observed with the Fe2+/3+couple in Fe2(SO4)3due to inductive effect caused by the countercation S6+.A stronger S–O covalent bonding weakens the l-bond Fe–O covalence through inductive effect,which results in a lowering of the Fe2+/3+redox couple and an increase in the cell voltage.However,a poor electronic conductivity associated with the Fe-O-X-O-Fe(X=S or P)linkage leads to poor rate capability. Nanostructured Phospho-olivine CathodesFollowing the initial concept of using polyanions[78,79],several phosphates have been investigated in recent years[81–83].Among them,LiFePO4crystallizing inFig.8.13Structure ofolivine LiFePO4the olivine structure(Fig.8.13)with FeO6octahedra and PO4tetrahedra has been shown to be a promising material exhibiting aﬂat discharge voltage of~3.45V, with a theoretical capacity of170mAh g−1.Unlike in the case of layered LiMO2 (M=Co,Ni,or Mn)oxides,the presence of covalently bonded PO4units as well as the operation of Fe2+/3+couple rather than M3+/4+couples leads to good struc-tural and chemical stabilities,resulting in good safety features.Moreover,iron is inexpensive and environmentally benign.However,the initial work was able to extract only<0.7lithium ions from LiFePO4even at very low current densities, which corresponds to a reversible capacity of<120mAh g−1.As the lithium extrac-tion/insertion occurred by a two-phase mechanism with LiFePO4and FePO4as end members without much solid solubility,the limitation in capacity was attributed to the diffusion-limited transfer of lithium across the two-phase interface.Thus, the major drawback with LiFePO4is its poor lithium-ion conductivity resulting from one-dimensional diffusion of Li+ions along the chains(b-axis)formed by edge-shared LiO6octahedra and poor electronic conductivity(~10−9S cm−1).Tremendous efforts have been made in recent years to overcome these prob-lems by cationic doping,decreasing the particle size through various synthesis methods,and coating with electronically conducting agents[84–89].Particularly, nano-sized LiFePO4particles have been shown to exhibit excellent performance with high rate capability due to a shortening of both the electron and lithium-ion diffusion path lengths within the particles.In this regard,dimensionally modulated nanostructures such as nanorods,nanowires,and nanosheets are appealing as they can efﬁciently transport charge carriers while maintaining a large surface-to-volume ratio,enhancing the contact with the electrolyte and the reaction kinetics.Among the various synthesis approaches pursued in the past few years,solution-based methods have been particularly successful for LiFePO4with respect to controlling the chemical composition,tailoring the crystallite size,and particle mor-phologies.However,these methods require either long reaction times(5–24h)or further post-heat treatment processing at temperatures as high as700◦C in reduc-ing atmospheres to achieve phase pure samples and a high degree of crystallinity. In this regard,microwave-assisted synthesis approaches are extremely appealing as they can shorten the reaction time from several hours to a few minutes with enor-mous energy savings and cleanliness.Consequently,our group has demonstrated。

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Lei Zhang,‡ Haitao Zhang,‡* Long Jin, Binbin Zhang, Fangyan Liu, Hai Su, Fengjun Chun, Qinghan Li, Jinfang Peng and Weiqing Yang*
Received 13th February 2016 Accepted 5th May 2016
RSC Advances
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Cite this: RSC Adv., 2016, 6, 50209
Composition controlled nickel cobalt sulﬁde core– shell structures as high capacity and good ratecapability electrodes for hybrid supercapacitors†
Published on 06 May 2016. Downloaded on 25/05/2016 08:28:57.
DOI: 10.1039/c6ra03955c /advt a type of core–shell structured NixCo3ÀxS4 (x ¼ 1, 1.5 and 2) through tuning the ratios of Ni to Co by a simple two-step hydrothermal method. Scanning electron microscopy and transmission electron microscopy images of all the Ni–Co sulﬁdes show high porosity and uniform spherical morphology. Moreover, this study demonstrates that controlling the appropriate ratio of Ni to Co in the core–shell structure is crucial for improving the electrochemical performance in a hybrid supercapacitor. Among them, NiCo2S4 with core–shell structure possesses the highest capacity of 155 mA h gÀ1, whereas as Ni1.5Co1.5S4 shows the excellent rate-capability of up to 80% from 1 to 20 A gÀ1 and cycling stability, which retains 74% after 2000 cycles. Therefore, tuning the metal element contents provides

2014-ACS Appl. Mater. Interfaces-酚变醌

© 2014 American Chemical Society
■
mesoporous carbon,16 graphene,2 and carbon nanoﬁber (CNF),17 have been widely employed as the immobilization materials of enzymes in biosensors, which can be attributed to their large speciﬁc surface area, excellent conductivity, and satisfactory biocompatibility. Among these materials, CNF possesses much larger functionalized surface area compared to that of CNT and is more suitable for immobilization and stability of enzyme. It has been proven that CNF is an outstanding matrix for the development of biosensors, which is far superior to the carbon nanotube.17 Notably, the CNF possesses a history of more than a century; the carbon ﬁlaments discovered in 1889 may be the earliest CNF.18 After more than a century of development, various methods used for CNF preparation have been developed, such as arc-discharge,19 laser ablation,20 chemical vapor deposition (CVD) methods,21 and others. Electrospinning, known as a facile and convenient process technique, produces nanoﬁbers or microﬁbers with diﬀerent diameters using a variety of polymers. Carbonization of electrospun polyacrylonitrile nanoﬁbers can be employed to fabricate CNF.22 In addition, to our best knowledge, CNF from CVD usually contains some impurities, e.g., metal catalyst and graphite particle, which requires a further complicated

(2014)Xianhua Hou, Xiaoli Zou et al. RSC ADV.

RSC Advances
PAPER Surfactant CTAB-assisted synthesis of Li1.13[Ni0.233Mn0.534Co0.233]0.87O2 with festoon-like hierarchical architectures as cathode materials for Li-ion batteries with outstandinguction
The introduction of non-aqueous rechargeable lithium-ion batteries in the 1990s for electric vehicles (EV), plug-in hybrid vehicles (PHEVs) and power portable electronic devices bring about a revolution in battery technology and a remarkable transformation from the relatively low-voltage, low-capacity and water-based systems such as nickel–cadmium1,2 and nickel– metal hydride batteries3,4 because of their relatively high energy density and design exibility. The electrochemical performances of the Li-ion batteries mainly depend on the cathode materials, the anode materials and the electrolyte. While the anode materials have the characteristics of the specic capacity much higher than the cathode material, such as siliconbased,5–7 tin-based,8,9 lithium transition metal oxides10,11 and metal-oxides.12–14 So it has become very important to improve the capability of cathode material, and further to improve the capacity of lithium ion secondary batteries.

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MINERALS METALS & MATERIALS S1047-4838 KONA POWDER PART J KONA Powder and Particle Journal0288-4534 KOREAN J MET MATER Korean Journal of Metals and Materials1738-8228 KOVOVE MATER KOVOVE MATERIALY-METALLIC MATERIALS0023-432X LASER ENG LASERS IN ENGINEERING0898-1507 MACH SCI TECHNOL MACHINING SCIENCE AND TECHNOLOGY1091-0344 MAG CONCRETE RES MAGAZINE OF CONCRETE RESEARCH0024-9831 MAT SCI SEMICON PROC MATERIALS SCIENCE IN SEMICONDUCTOR PROCESSING1369-8001 MATER CONSTRUCC MATERIALES DE CONSTRUCCION0465-2746 MATER CORROS MATERIALS AND CORROSION-WERKSTOFFE UND KORROSION0947-5117 MATER DESIGN MATERIALS & DESIGN0261-3069 MATER HIGH TEMP MATERIALS AT HIGH TEMPERATURES0960-3409 MATER MANUF PROCESS MATERIALS AND MANUFACTURING PROCESSES1042-6914 MATER RES INNOV MATERIALS RESEARCH INNOVATIONS1432-8917 MATER RES-IBERO-AM J Materials Research-Ibero-american Journal of Mat1516-1439 MATER SCI TECH-LOND MATERIALS SCIENCE AND TECHNOLOGY0267-0836 MATER SCI+MATERIALS SCIENCE1068-820X MATER SCI-MEDZG Materials Science-Medziagotyra 1392-1320 MATER SCI-POLAND MATERIALS SCIENCE-POLAND0137-1339 MATER STRUCT MATERIALS AND STRUCTURES1359-5997 MATER TECHNOL MATERIALS TECHNOLOGY1066-7857 MATER TEHNOL Materiali in Tehnologije 1580-2949 MATER TRANS MATERIALS TRANSACTIONS1345-9678 MATER WORLD MATERIALS WORLD0967-8638 MATERIA-BRAZIL Materia-Rio de Janeiro1517-7076 MATERIALWISS WERKST MATERIALWISSENSCHAFT UND WERKSTOFFTECHNIK0933-5137 MATH MECH SOLIDS MATHEMATICS AND MECHANICS OF SOLIDS1081-2865 MET MATER INT METALS AND MATERIALS INTERNATIONAL1598-9623 METALL MATER TRANS B METALLURGICAL AND MATERIALS TRANSACTIONS B-PROCE1073-5615 METALLOFIZ NOV TEKH+METALLOFIZIKA I NOVEISHIE TEKHNOLOGII1024-1809 MICRO NANO LETT Micro & Nano Letters1750-0443 MICROELECTRON INT MICROELECTRONICS INTERNATIONAL1356-5362 MICROSYST TECHNOL MICROSYSTEM TECHNOLOGIES0946-7076MODEL SIMUL MATER SC MODELLING AND SIMULATION IN MATERIALS SCIENCE AN0965-0393 NANO NANO1793-2920 NEW CARBON MATER NEW CARBON MATERIALS1007-8827 OPTOELECTRON ADV MAT Optoelectronics and Advanced Materials-Rapid Com1842-6573 P I MECH ENG L-J MAT PROCEEDINGS OF THE INSTITUTION OF MECHANICAL ENG1464-4207 PARTICUOLOGY Particuology1674-2001 PHILOS MAG PHILOSOPHICAL MAGAZINE1478-6435 PHYS STATUS SOLIDI A PHYSICA STATUS SOLIDI A-APPLICATIONS AND MATERIA1862-6300 PLAST ENG PLASTICS ENGINEERING0091-9578 PROG NAT SCI PROGRESS IN NATURAL SCIENCE1002-0071 RAPID PROTOTYPING J RAPID PROTOTYPING JOURNAL1355-2546 RARE METAL MAT ENG RARE METAL MATERIALS AND ENGINEERING1002-185X RARE METALS RARE METALS1001-0521 RECENT PAT NANOTECH Recent Patents on Nanotechnology1872-2105 REV ADV MATER SCI REVIEWS ON ADVANCED MATERIALS SCIENCE1606-5131 REV ROM MATER Revista Romana de Materiale-Romanian Journal of 1583-3186 ROAD MATER PAVEMENT Road Materials and Pavement Design1468-0629 SAMPE J SAMPE JOURNAL0091-1062 SCI CHINA TECHNOL SC Science China-Technological Sciences1674-7321 SCI MODEL SIMUL Scientific Modeling and Simulations1874-8554 SCI TECHNOL ENERG MA Science and Technology of Energetic Materials 1347-9466 SCI TECHNOL WELD JOI SCIENCE AND TECHNOLOGY OF WELDING AND JOINING1362-1718 SEMICOND SCI TECH SEMICONDUCTOR SCIENCE AND TECHNOLOGY0268-1242 SENSOR MATER SENSORS AND MATERIALS0914-4935 SOLDER SURF MT TECH SOLDERING & SURFACE MOUNT TECHNOLOGY0954-0911 T FAMENA Transactions of FAMENA 1333-1124 VACUUM VACUUM0042-207X ZKG INT ZKG INTERNATIONAL0949-0205 SIAM J IMAGING SCI SIAM Journal on Imaging Sciences1936-4954 IEEE T MED IMAGING IEEE TRANSACTIONS ON MEDICAL IMAGING0278-0062 REMOTE SENS ENVIRON REMOTE SENSING OF ENVIRONMENT0034-4257 INT J REMOTE SENS INTERNATIONAL JOURNAL OF REMOTE SENSING0143-1161 ISPRS J PHOTOGRAMM ISPRS JOURNAL OF PHOTOGRAMMETRY AND REMOTE SENSI0924-2716 PHOTOGRAMM ENG REM S PHOTOGRAMMETRIC ENGINEERING AND REMOTE SENSING0099-1112 PHOTOGRAMM REC PHOTOGRAMMETRIC RECORD0031-868X EURASIP J IMAGE VIDE EURASIP Journal on Image and Video Processing1687-5176 IEEE J-STARS IEEE Journal of Selected Topics in Applied Earth1939-1404 IMAGING SCI J IMAGING SCIENCE JOURNAL1368-2199 INT J IMAG SYST TECH INTERNATIONAL JOURNAL OF IMAGING SYSTEMS AND TEC0899-9457 J APPL REMOTE SENS Journal of Applied Remote Sensing1931-3195 J ELECTRON IMAGING JOURNAL OF ELECTRONIC IMAGING1017-9909 J IMAGING SCI TECHN JOURNAL OF IMAGING SCIENCE AND TECHNOLOGY1062-3701 J REAL-TIME IMAGE PR Journal of Real-Time Image Processing1861-8200 PHOTOGRAMM FERNERKUN Photogrammetrie Fernerkundung Geoinformation1432-8364 RIV ITAL TELERILEVAM Rivista Italiana di Telerilevamento1129-8596 SIGNAL IMAGE VIDEO P Signal Image and Video Processing1863-1703 SMPTE MOTION IMAG J SMPTE MOTION IMAGING JOURNAL0036-1682 ANN FAM MED ANNALS OF FAMILY MEDICINE1544-1709 BRIT J GEN PRACT BRITISH JOURNAL OF GENERAL PRACTICE0960-1643 J AM BOARD FAM MED Journal of the American Board of Family Medicine1557-2625 SCAND J PRIM HEALTH SCANDINAVIAN JOURNAL OF PRIMARY HEALTH CARE0281-3432 AM FAM PHYSICIAN AMERICAN FAMILY PHYSICIAN0002-838X。

ASTM A1059-A1059M - 08

Designation:A1059/A1059M−08Standard Speciﬁcation forZinc Alloy Thermo-Diffusion Coatings(TDC)on Steel Fasteners,Hardware,and Other Products1This standard is issued under theﬁxed designation A1059/A1059M;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(´)indicates an editorial change since the last revision or reapproval.1.Scope1.1This speciﬁcation covers the general requirements for protective zinc coatings(hereinafter referred to as the coatings) to be applied by the thermo-diffusion coating(TDC)method, to various products made of carbon steel,including low and high tensile parts as well as of wrought iron,sintered iron steel-powder and various steel and stainless alloys.TDC is carried out by immersing the parts in a zinc alloy powder at elevated temperature for a period of time,causing a metallur-gical diffusion process of zinc and iron.Further processing may be added,such as,passivation,topcoat application,paint application,etc.1.2This speciﬁcation is applicable to orders in either inch-pound units(as A1059)or in SI units(as A1059M). Inch-pound units and SI units are not necessarily exact equivalents.Within the text of this speciﬁcation and where appropriate,SI units are shown in brackets.Each system shall be used independently of the other without combining values in any way.In the case of orders in SI units,all testing and inspection shall be done using the metric equivalent of the test or inspection method as appropriate.In the case of orders in inch-pound units,such shall be stated to the applicator when the order is placed.1.3This 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 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1ASTM Standards:2A90/A90M Test Method for Weight[Mass]of Coating on Iron and Steel Articles with Zinc or Zinc-Alloy CoatingsA385Practice for Providing High-Quality Zinc Coatings (Hot-Dip)A700Practices for Packaging,Marking,and Loading Meth-ods for Steel Products for ShipmentA902Terminology Relating to Metallic Coated Steel Prod-uctsB487Test Method for Measurement of Metal and Oxide Coating Thickness by Microscopical Examination of Cross SectionD521Test Methods for Chemical Analysis of Zinc Dust (Metallic Zinc Powder)D6386Practice for Preparation of Zinc(Hot-Dip Galva-nized)Coated Iron and Steel Product and Hardware Surfaces for PaintingE376Practice for Measuring Coating Thickness by Magnetic-Field or Eddy-Current(Electromagnetic)Test-ing MethodsF1789Terminology for F16Mechanical FastenersF2329Speciﬁcation for Zinc Coating,Hot-Dip,Require-ments for Application to Carbon and Alloy Steel Bolts, Screws,Washers,Nuts,and Special Threaded Fasteners F2674Speciﬁcation for Zinc Coating,Hot-Dip,Require-ments for Application to Carbon and Alloy Steel Bolts, Screws,Washers,Nuts,and Special Threaded Fasteners [Metric]3.Terminology3.1The following terms and deﬁnitions are speciﬁc to this speciﬁcation.Terminology A902contains other terms and deﬁnitions relating to metallic-coated steel products.Terminol-ogy F1789contains other terms and deﬁnitions relating to mechanical fasteners.3.2Deﬁnitions of Terms Speciﬁc to This Standard:3.2.1thermo-diffusion coating—a process where the steel product is heated in close contact with zinc powder or zinc mixture.3.2.2thermo-diffusion coating—a coating made by thermo-diffusion coating process,consisting of zinc/iron alloys.3.2.3zinc powder—the coating material used to provide corrosion protection to steel.1This speciﬁcation is under the jurisdiction of ASTM Committee A05onMetallic-Coated Iron and Steel Products and is the direct responsibility ofSubcommittee A05.13on Structural Shapes and Hardware Speciﬁcations.Current edition approved Nov.15,2008.Published December2008.DOI:10.1520/A1059_A1059M-08.2For referenced ASTM standards,visit the ASTM website,,orcontact ASTM Customer Service at service@.For Annual Book of ASTMStandards volume information,refer to the standard’s Document Summary page onthe ASTM website.Copyright©ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959.United States3.2.4zinc mixture—a combination of zinc powder and other metallic materials to be used as a coating material in the TDC process.4.Ordering Information4.1Orders for coatings provided under this speciﬁcation shall include the following:4.1.1Quantity(number of pieces to be coated)and total weight.4.1.2Description(type and size of products)and weight.4.1.3ASTM speciﬁcation designation and year of issue.4.1.4Material identiﬁcation(see5.1)and surface condition or contamination.4.1.5Sampling plan,if different from Section8.4.1.6Special test requirements,if different from Section9 (see9.1).4.1.7Special requirements(special stacking,heavier coat-ing weight,etc.).4.1.8Tagging or piece identiﬁcation method.4.2Additional Information—Additional information may be required in certain circumstances.In these cases the purchaser will furnish the applicator with the following additional infor-mation:4.2.1Any likely effects on the metallurgical properties of the base material caused by processing temperatures of up to 1092°F[500°C].4.2.2Determination of areas considered as signiﬁcant sur-faces.This should be done by drawings or by providing samples with suitable markings.4.2.3Any critical thickness tolerances,such as when bolts and nuts are used.This should be done on the product’s drawing or on the purchase order.4.2.4Any special pre-treatment requirements or the exis-tence of other materials,lubricants,stripping materials,pre-existing corrosion,etc.4.2.5Whether quality certiﬁcate is required or not.5.Materials and Manufacture5.1Requirements to design of the products to be coated with zinc are detailed in Practice A385.The following provi-sions are necessary to produce a high quality coating.5.1.1The products to be coated with zinc include parts and assemblies of various sizes:presswork,forged,cast,machined products(nuts,washers,bolts,nails,chains,small round billets,blanks for plumbingﬁxtures,etc.).When coating is applied to long-length parts(pipes,rods),the appropriate production equipment is required.5.1.2The products shall have neither pockets nor closed cavities.All cavities shall be available for applying the coating of diffusion mixture.Should it be impossible to apply the coating to individual portions of surface of the article,the documents shall specify if the coating is allowed to be absent in these cavities.5.1.3The fasteners to be coated with zinc shall meet the requirements of standards in force,for the fasteners,and accompanied with certiﬁcates from manufacturers.5.1.4The products(parts)containing soft solder or resins can not be coated with zinc.5.1.5For Fasteners—The maximum deviations of threads prior to application of the coating shall comply with the standards for threads.An additional gap for the coating for external and internal threads separately or for both threads at the same time,is to be provided,if the coating with increased thickness is to be applied.Requirements for fasteners to be thermal diffusion coated with zinc are found in Speciﬁcations F2329and F2674.5.2Requirements for material and surface of substrate: 5.2.1This is applied to products of standard-quality carbon steel,high-quality structural carbon and low-carbon steel,as well as low-alloyed steel,stainless steels,pig iron and copper.5.2.2The following defects are not allowed on the surfaces of the parts:5.2.2.1Rolled-in scale,burrs;5.2.2.2Separation into layers and cracks including those arising from pickling,polishing and other treatment;5.2.2.3Corrosion damages,pores,and holes.5.2.3The surfaces of cast and forged products shall be free of blow and shrink holes,slag,andﬂux contamination.5.2.4The surfaces of the parts of hot-rolled metal shall be cleaned from scale,pickling sludge,products of corrosion of the base metal,and other contamination.5.2.5After machining,the surfaces of the parts shall be free of visible layer of grease,emulsion,metallic chips,burrs,dust and products of corrosion,and implantation of foreign metal particles.5.2.6Sharp corners and edges of the products except for those required for technological reasons shall be machined to a radius of at least0.001in.[0.3mm].5.2.7After heat treatment,the surfaces of the parts shall be free of blow holes,corrosion centers,separation into layers, and buckling.5.2.8Welds,soldered and brazed joints on the parts shall be scraped bright and continuous over the whole perimeter.5.2.9Prior to applying the coating,the surface of the part shall be degreased(chemically or thermally),cleaned by pickling or abrasive blasting.5.2.10The degree of cleanness of the surface shall be in accordance with Practice D6386.5.2.11The term for storage of the parts with the surface prepared for coating with zinc shall not exceed24hours under conditions excluding the precipitation of a condensate.5.2.12For applying coatings,the zinc powder with humid-ity of not more than1.5%in accordance with Test Methods D521shall be used.6.Chemical Composition6.1The method described results in the formation of iron-zinc compound layers known as Gamma(Solid Zn ions inside Fe substrate),Delta(Fe11Zn40),and Zeta(FeZn7),excluding the external Eta layer of pure free zinc.6.2The zinc mixture used in the thermo-diffusion coating process shall contain a mass fraction not less than94%of metallic zinc and total impurities(other than Zinc oxide)of not more than2%massfraction.6.3It should be noted that there is evidence this coating is subject to premature red staining in atmospheric and acceler-ated test environments;however,this staining has been found not to be associated with corrosion of the substrate steel,but rather superﬁcial oxidation of the zinc/iron ions present on the surface.7.Workmanship,Finish,and Appearance7.1Appearance of the coating:7.1.1The coating shall be ﬂat gray,smooth,and reasonably uniform.Smoothness of surface is a relative term.Minor roughness that does not interfere with the intended use of the part,or roughness that is related to the as-received (un-coated)surface condition of the part,shall not be grounds for rejection.7.1.2The coating shall be free of swellings,blow holes,cuts,ﬂaking,and embedded quartz sand.7.1.3The presence of dark gray spots (variation in the color of the coating without variation in its thickness)not more than 5%of the total surface of the product is allowed on the coating.7.1.4The presence of surface scratches,marks from contact of the part with one another,contact with measuring tools,etc.,without damage to the coating,which would cause exposure of the base metal,is allowed.7.1.5The presence of residual process mixture on the surface of the part is not allowed.7.1.6The thickness of the coating depending on the condi-tions of operations of the product shall be speciﬁed in the standards of speciﬁcation for the product in accordance with Table 1.8.Sampling8.1Test specimens shall be selected randomly from each inspection lot.8.2The method of selection and sample size shall be agreed upon between the applicator and the purchaser.Otherwise,the sample size selected from each lot shall be as follows:Batch Size (Pieces)Sample Size 1to 3All 4to 5003501to 120051201to 320083201to 1000013Above 10000209.Number of Tests and Retests9.1The zinc coating applied shall be tested for appearance and thickness.9.2Each lot of parts coated with zinc shall be presented for testing.A lot shall be considered as a group of articles of the same type and size coated with zinc within the same production cycle.9.3Approximately 10%of articles per lot and each article in case of single-unit production shall be examined for appear-ance.9.4At least three articles per lot shall be tested for thickness of the coating.9.5When using the metallographic (arbitration)method,it is allowed to test the coating thickness on one part per lot.9.6The coating thickness shall be tested prior to the additional treatment of the coating (applying preservation lubricants,etc.).This measurement shall be taken on a non-threaded section of the part.9.7The coating thickness on the threaded portion of a bolt shall not be tested but shall be ensured by the correctness of the coating application technology.When developing the coating process it is recommended to take into account the ISO requirements for threaded fasteners.9.8The checked thickness of the coating shall be accepted as an arithmetical mean of the measured values.9.9Should the results of the measuring of the test control be unsatisfactory,the test shall be repeated on double quantity of parts.10.Specimen Preparation10.1Specimens for testing should not go through any cleaning process and should be tested as is after the ﬁnal coating process (including passivation and or other top coats).11.Test Methods11.1Coating appearance check:The coating appearance shall be checked visually with an unaided eye from the distance of 10in.[25cm]from the surface.The luminance shall be at least 300Lx.11.2Coating thickness testing:TABLE 1Thickness or Weight [Mass]of Zinc Coating for Various Coating ClassesCoating Class Weight [Mass]of Coating,oz/ft 2(g/m 2)of Surface,Minimum Coating Thickness,mils (µm),Minimum 130 3.02(922) 5.14(130)110 2.50(765) 4.33(110)90 2.05(627) 3.54(90)80 1.82(557) 3.15(80)70 1.59(487) 2.76(70)65 1.48(453) 2.56(65)55 1.25(383) 2.17(55)50 1.14(348) 1.97(50)45 1.02(313) 1.77(45)400.91(278) 1.57(40)250.57(174)0.98(25)120.27(84)0.47(12)11.2.1Magnetic Method:11.2.1.1The method is based on the registration of variation in the magnetic resistance depending on the coating thickness in accordance with Practice E376.The magnetic thickness gauges shall be used as measuring instruments.11.2.1.2The arithmetic mean of at least three measured values at edges and center of the surface of one article to be controlled shall be considered as the result of the coating thickness measurement.11.2.2Metallographic Method(Arbitration)—The method is based on the measurement of the coating thickness on the cross-section metallographic specimen using metallographic microscopes of various types in accordance with Test Method B487.The specimen shall be cut from a coated article.The thickness of the zinc coating shall be measured on the specimen at least atﬁve point located at equal distances within a linear area with the length of about0.4in.[1cm].The arithmetic mean of all measured values shall be considered as the result.11.2.3Gravimetric Method—The gravimetric method shall be used for determining the mean thickness of the coating.The method consists of weighing the representative specimens before and after applying the coating and then before and removing the coating in accordance with Test Method A90/ A90M.12.Certiﬁcation12.1When speciﬁed in the purchase order or contract,the purchaser shall be furnished certiﬁcation that samples repre-senting each inspection lot have been either tested or inspected as directed by this speciﬁcation and the requirements have been met.When speciﬁed in the purchase order or contract,a report of the test results shall be furnished.13.Packaging and Package Marking13.1Unless speciﬁed otherwise by the customer in the purchase order,the coated products shall be packaged,trans-ported and stored in accordance with Practices A700.14.Keywords14.1coatings,zinc;fasteners,zinc coated;iron products, zinc coated;steel hardware,zinc coated;steel products,metal-lic coated;zinc coatings,steel productsAPPENDIX(Nonmandatory Information)X1.COATING CHARACTERISTICSX1.1The thermo diffusion zinc coating is anodic in relation to ferrous metals and provides for electrochemical protection of steel against corrosion.X1.2Thermo diffusion results in a hard surface,usually exceeding35Rockwell C,depending on coating parameters.X1.3Thermo diffusion does not create hydrogen embrittle-mentX1.4Due to some porosity on the surface of the coating, thermo diffusion coated parts have excellent bonding charac-teristics with various topcoats and paint system.X1.5The thermo-diffusion zinc coating is obtained by heating the parts in a container with the diffusion mixture consisting of zinc powder and some alloying elements.The working temperatures of applying the coating normally range between710°F to1092°F[320°C to500°C].X1.6Since the coating application process has a sufficiently long duration,the thermo diffusion coating with zinc can be used for parts made of materials that do not change their properties at these temperatures.X1.7The coating obtained shall follow exactly the contours of the article,its thickness shall be very uniform over the whole surface of the part including complex-shaped articles(threaded connections,etc.).X1.8When applying the coating,the part shall be placed in a container.Since the size of the parts is restricted by the size of the container,the appropriate size container must be used. X1.9The coating has strong adhesion to base metal due to mutual diffusion of zinc and iron.Zinc penetrates the base metal to about1⁄3of the coating thickness.X1.10The coating consists mainly of the iron-zinc d1-phase containing4to10%of iron.X1.11Due to the presence of iron in the coating,red stains or brown spots may appear on the surface of the coated article under the inﬂuence of increased humidity or condensate.It is caused by the release of iron ions from the coating.These ions are washed away easily by waterX1.12Should it be impossible to distinguish the corrosion products of the coating and that of base metal,the presence of the coating shall be checked by metallographic method and mass losstesting.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this ers of this standard are expressly advised that determination of the validity of any such patent rights,and the risk of infringement of such rights,are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyﬁve years and if not revised,either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,which you may attend.If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards,at the address shown below.This standard is copyrighted by ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959, United States.Individual reprints(single or multiple copies)of this standard may be obtained by contacting ASTM at the above address or at610-832-9585(phone),610-832-9555(fax),or service@(e-mail);or through the ASTM website ().Permission rights to photocopy the standard may also be secured from the ASTM website(/ COPYRIGHT/).。

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International Journal of Minerals, Metallurgy and Materials Volume 18, Number 3, June 2011, Page 377 DOI: 10.1007/s12613-011-0450-9

Corresponding author: Li-qun Zhu E-mail: zhulq@buaa.edu.cn © University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg 2011

Electrochemical behavior of different shelled microcapsule composite copper coatings

Xiu-qing Xu, Yan-hong Guo, Wei-ping Li, and Li-qun Zhu School of Materials Science and Engineering, Beihang University, Beijing 100191, China (Received: 12 May 2010; revised: 17 June 2010; accepted: 6 July 2010)

Abstract: Copper/liquid microcapsule composite coatings with polyvinyl alcohol (PVA), gelatin or methyl cellulose (MC) as shell materials were prepared by electrodeposition. The influence of shell materials on the corrosion resistance of the composite coatings in 0.1 M H2SO4

was investigated by means of electrochemical techniques, scanning electron microscopy (SEM), and energy dispersion spectrometry (EDS).

The results show that the participation of microcapsules can enhance the corrosion resistance of the composite coatings compared with the traditional copper layer. Based on the analysis of electrochemical test results, the release ways of microcapsules were deduced. Gelatin and MC as the shell materials of microcapsules are easy to release quickly in the composite coating. On the contrary, the releasing speed of PVA microcapsules is relatively slow due to their characteristics.

Keywords: composite coatings; shell materials; copper; microcapsules; electrochemical properties; corrosion resistance; electrodeposition

[This work was financially supported by the National Natural Science Foundation of China (No. 50771010).]

1. Introduction Composite coatings obtained by electrolytic co-deposi-tion have been developed rapidly and play an important role in the research field of material science because of their spe-cial properties about physics, chemistry, biology, and ma-chining, etc. [1-4]. Solid particles that can be incorporated into the composite plating coating are almost unlimited, such as SiC, Al2O3, BC, and ZnO2 [5-8]. Very little informa-tion about the electrolytic co-deposition of metals and microcapsules containing liquid active agents has been pub-lished. The unique advantage of this composite coating is that the release of microcapsules could partially repair and protect the surface of the coating when the surface is locally damaged. Available researches are limited to the preparation process of microcapsules and the performance of the com-posite coating [9-11]. Further research such as the influence of core and shell materials on the performance of composite coatings has been seldom discussed.

In our previous works [12-15], various liquid microcap-sules were prepared using the phase separation in an aque-ous solution method. Also, successful co-deposition of liq-uid microcapsules with nickel and copper were reported, where excellent properties of composite coatings were ex-hibited. It was proved that under appropriate conditions, the core materials can be released [16-17]. The main influenc-ing factors of the release process of microcapsules include the properties of core and shell materials, the size of micro-capsules, and external environment factors, etc. [18-20]. Meanwhile, it also have been found that three main shell materials of microcapsules including polyvinyl alcohol (PVA), gelatin, and methyl cellulose (MC) had different tensile strength, toughness, and permeability, which could affect the release of microcapsules and the properties of the composite coating. In this paper, the influence of shell mate-rials on the release behavior of microcapsules and the corro-sion behavior of composite coatings was discussed. It is beneficial for the application of the composite coating with 378 Int. J. Miner. Metall. Mater., Vol.18, No.3, Jun 2011 functional properties we want. 2. Experimental 2.1. Materials All commercial chemicals were employed without fur-ther pre-treatment in this research. PVA, gelatin, and MC, purchased from Beijing Yili Fine Chemicals Co. Ltd., were used as the shell materials of liquid microcapsules. Hydro-phobic agent was used as the core material of the microcap-sule. Span-80 and anhydrous alcohol were used as the dis-persant and flocculant in the preparation course of micro-capsules, respectively.

2.2. Preparation of liquid microcapsules The liquid microcapsule which is suitable for electro-chemical co-deposition was prepared by means of phase separation in an aqueous solution method. The preparation process is briefly described as follows. The core material (1 mL hydrophobic agent) was added dropwise to a beaker containing 20 mL shell material solution while stirring (1000 r/min) at room temperature. After 5 min, minor Span-80 was added into the emulsion with constant stirring