Transcript Lecture 8
Electrochemistry MAE-212 Dr. Marc Madou, UCI, Winter 2016Class VIII Corrosion Table of Content Definition Why study corrosion? Thermodynamics of Corrosion Corrosion Illustrated Protection Mechanisms Evans Diagram 2 8/7/2016 Definition Corrosion is the deterioration of materials by chemical interaction with their environment. The term corrosion is sometimes also applied to the degradation of plastics, concrete and wood, but generally refers to metals. The most widely used metal is iron (usually as steel) and the following discussion is mainly related to metal corrosion. 3 8/7/2016 Why Study Corrosion? Materials are precious resources Engineering design is incomplete without knowledge of corrosion Corrosion contaminates products such as pharmaceutical, food and dairy 4 products Corrosion products are a threat to the environment Ensuring maximum life of new equipment Preservation of existing equipment Protecting or improving the quality of a product in order to maintain or improve a competitive position. Avoiding costly interruptions of production. Reducing or eliminating losses of valuable products by spillage or leaks. Reducing hazards to life and property that might be associated with corrosion: Explosions of pressure vessels or piping systems release of poisonous or explosive gases or vapors Artificial implants for the human body!!! 8/7/2016 Thermodynamics of Corrosion: Gibbs Free Energy Thermodynamic considerations allow the determination of whether a reaction can occur spontaneously If metal dissolution is unfavorable thermodynamically in a given set of circumstances – the job of the corrosion engineer is done Example: Copper in pure deoxygenated water Free Energy: Driving Force of a Chemical Reaction The larger the value of E for any cell – the higher is the tendency for the overall cell reaction to proceed: G EnF Ecell = Ecathode - Eanode 5 8/7/2016 Thermodynamics of Corrosion: Gibbs Free Energy Spontaneous Spontaneous Not Spontaneous 6 8/7/2016 Thermodynamics of Corrosion: The Nernst Equation General Reaction for a Galvanic Cell lL mM qQ rR Nernst Equation: q r RT aQ .aR ... EE ln l m nF aL .aM ... 0 7 8/7/2016 Thermodynamics of Corrosion: Oxygen Electrodes 8 8/7/2016 Thermodynamics of Corrosion: Oxygen Electrode and Differential Aeration Cell Consider two O2 electrodes: one in contact with O2 at 1 atm other in contact with O2 at 0.2 atm 8/7/2016 9 Thermodynamics of Corrosion: Oxygen Electrode and Differential Aeration Cell The reaction is not thermodynamically possible as written Thus, the electrode 1 is cathode electrode 2 the anode. In a differential aeration cell, the electrode in lower O2 pressure acts as the anode and the one in higher O2 pressure acts as the cathode 10 8/7/2016 Thermodynamics of Corrosion: Galvanic Series Galvanic series is an arrangement of both metals and alloys according to their actual measured potentials in a particular environment. There is a Galvanic series for each environment Metals and alloys showing active-passive behavior are listed in both active and passive states. In the 1910s, before the First World War, people were concerned about how easily gun barrels made of steel would corrode. A scientist called Henry Brearly found that adding about 10% chromium to the steel made an alloy which was very resistant to corrosion. He called this new alloy ‘rustless steel’. 11 8/7/2016 Thermodynamics of Corrosion: Galvanic Scale of Metals in Seawater Stainless steel is used to make cutlery, saucepans, surgical instruments and food transporters. Stainless steel is an alloy of iron which contains around 12% chromium and smaller amounts of nickel and carbon 12 8/7/2016 Thermodynamics of Corrosion: Pourbaix Diagram The Nernst Equation allows us to compute lines for equilibrium reactions of interest … Electrochemical reactions of pure charge transfer are horizontal lines since there is no H+ or OH- dependence; Pure acid-base reactions are vertical lines since no electron transfer occurs, thus there is no dependence on potential; Electrochemical reactions involving charge transfer and H+(OH-) are represented as sloping lines. 13 8/7/2016 Thermodynamics of Corrosion: Pourbaix Diagram Marcel Pourbaix developed potential-pH diagrams to show the thermodynamic state of most metals in dilute aqueous solutions With pH as abscissa and potential as ordinate, these diagrams have curves representing chemical and electrochemical equilibria between metal and aqueous environment These diagrams ultimately show the conditions for immunity, corrosion or passivation. A Pourbaix Diagram is a thermodynamic map of corrosion, passivity and nobility of a particular metal as a function of system pH and potential. Operating environments are then superimposed on the diagram to determine the optimum operating conditions for a particular metal. Pourbaix diagrams may also be used to show regions of different forms of corrosion: General corrosion; Pitting corrosion; Passivation. 14 8/7/2016 Thermodynamics of Corrosion: Simplified Pourbaix Diagram for Iron 15 8/7/2016 Thermodynamics of Corrosion: Simplified Pourbaix Diagram for Iron It may also be observed that the form of corrosion is highly sensitive to the level of dissolved oxygen in the environment: 16 8/7/2016 Thermodynamics of Corrosion: Benefits of Pourbaix Diagram Pourbaix diagrams offer a large volume of thermodynamic information in a very efficient and compact format. The information in the diagrams can be beneficially used to control corrosion of pure metals in the aqueous environment By altering the pH and potential to the regions of immunity and passivation, corrosion can be controlled. For example, on increasing the pH of environment in moving to slightly alkaline regions, the corrosion of iron can be controlled Changing the potential of iron to more negative values eliminate corrosion, this technique is called cathodic protection. Raising the potentials to more positive values reduces the corrosion by formation of stable films of oxides on the surface of transition metals 17 8/7/2016 Corrosion Illustrated: Metal Loss Through Voltaic Cells In moist air, exposed iron can be oxidized to Fe2+ … these areas are referred to as anodic areas Other regions of the iron serve as cathodic areas Electrons from the anodic areas reduce atmospheric oxygen to the OH– ion Iron (II) ions migrate from the anodic areas to the cathodic areas, where they combine with the hydroxide ions and are further oxidized to iron(III) hydroxide by atmospheric oxygen … Fe2O3·xH2O is 18 common rust 8/7/2016 Corrosion Illustrated: : Metal Loss Through Voltaic Cells 19 8/7/2016 Corrosion Protection The simplest line of defense against the corrosion of iron is to paint it to exclude oxygen from the surface Another approach is to coat the iron with a thin layer of a less active metal An entirely different approach is to protect iron with a more active metal, as in the zinc-clad iron known as galvanized iron or in stainless steel. air 20 Stainless Steel: Chromium is more reactive than iron. It reacts quickly with oxygen from the air to form a very thin layer of chromium oxide on the surface of the steel. This protects the iron atoms from reacting with the oxygen in the air and prevents rust forming. If the steel is scratched or cut, more chromium atoms quickly form a new protective layer. protective Cr2O3 layer 8/7/2016 Corrosion Protection Cathodic protection: the iron object to be protected is connected to a chunk of an active metal and the iron serves as the reduction halfcell 21 8/7/2016 Example Pourbaix Diagram: Consider a fairly simple system … aluminum corroding in water: the following species are considered to be predominant in the system: Al (s); Al3+ (aq); Al2O3.H2O (s); AlO2- (aq). We can consider several “equilibrium” reactions describing the thermodynamic stability of these aluminum-containing species … 22 8/7/2016 Example Pourbaix Diagram: Pure charge transfer reactions: 1. Al3+(aq) +3 e- n Al (s) Pure acid/base reactions: Al2O3.H2O + 6 H+ n 2 Al3+ + 4 H2O 3. 2 AlO2- + 2 H+ n Al2O3.H2O 2. Mixed charge transfer and acid/base reactions: 4. 23 Al2O3.H2O + 6 H+ + 6 e- n 2 Al (s) + 4 H2O 8/7/2016 Example Pourbaix Diagram: Lines of pure charge transfer are calculated directly through the Nernst Equation … Al3+ + 3 e « Al (s) (aq) E Al 3+ /Al æa ö 2.303RT o Al ÷ ç = E Al log 3+ /Al ça ÷ nF è Al 3+ ø Eo is calculated through the ∆Grxno or looked up in a table of standard potentials; activity of solid Al = 1 … 24 8/7/2016 Example Pourbaix Diagram: Thus; ( E Al 3+ /Al = -1.662 + 0.0197log aAl 3+ ) We see that the potential is dependent upon the concentration of Al3+ in the system. In general, when constructing Pourbaix diagrams we choose ionic concentrations of … 100, 10-2, 10-4 and 10-6 mol/L (more correctly this is mol/kg but at room temperature they are moreor-less equal) 25 8/7/2016 Example Pourbaix Diagram: Potential (E) vs SHE -1.4 Al3+ -1.6 100 10-2 10-4 10-6 -1.8 Al -2 0 26 2 4 6 8 pH 10 12 14 8/7/2016 Example Pourbaix Diagram: Lines for pure acid/base reactions (no electron transfer) are calculated through the equilibrium constant or reaction quotient … Al 2O3.H 2O + 6 H+ ® 2 Al3+ + 4 H 2O ( ) o -DG rxn = RT ln K eq 2 K eq = aAl 3+ a aAl O .H O aH6 + 2 3 27 4 H 2O 2 8/7/2016 Example Pourbaix Diagram: Accounting for Al2O3.H2O as a solid and that water will have an activity of 1.0 gives: aH6 + = Taking logs … 6logaH + aA2 l 3+ K eq æ a 2 3+ ö = log çç Al ÷÷ è K eq ø ( ) ( ) pH = 0.166log ( K ) - 0.333log (a ) -pH =1/ 3log aAl 3+ -1/ 6log K eq 28 eq Al 3+ 8/7/2016 Example Pourbaix Diagram: Calculating Keq from the Gibbs energies of formation tabulations: Gf ------ Al3+ H20 Al2O3.H2O H+ -485.4 -237.0 -1825.5 0.0 kJ/mol kJ/mol kJ/mol kJ/mol æ -é2(-485.4) + 4(-237)-(-1825.5)ù ´1000 ë û K eq = exp ç ç 8.314 298 è Thus; ( 29 )( ) ( pH = 2.732 - 0.333log aAl 3+ ) ö ÷ = 2.882 ´1016 ÷ ø 8/7/2016 Example Pourbaix Diagram: 30 8/7/2016 Example Pourbaix Diagram: For the other acid/base reaction: 2 AlO-2 + 2 H+ « Al 2O3.H 2O K eq = aAl O .H O 2 3 2 (aAlO - )2 (aH + )2 2 ( ) ( ) pH = 0.5log K eq + log aAlO 31 2 8/7/2016 Example Pourbaix Diagram: Gibbs energies of formation … Gf ------ AlO2Al2O3.H2O H+ -838.968 -1825.5 0.0 kJ/mol kJ/mol kJ/mol Keq = 7.354 x 1025 ( ) pH = 12.93+ log a AlO- 2 32 8/7/2016 Example Pourbaix Diagram: 2.5 10-6 Potential (E) vs SHE 2 10-4 10-2 100 1.5 1 0.5 AlO2- 0 Al2O3.H2O -0.5 -1 -1.5 -2 -2.5 4 6 8 10 12 14 16 pH 33 8/7/2016 Example Pourbaix Diagram: Finally, for mixed reactions involving both charge transfer and acid/base reactions … Al2O3.H2O + 6 H+ + 6 e- → 2 Al (s) + 4 H2O We calculate these directly through the Nernst equation: E Al O /Al 2 3 34 4ö 2 æ ç aAl aH 2O ÷ 2.303RT o = E Al O /Al log ç 2 ÷ 2 3 nF ç aAl O a + ÷ è 23 H ø ( )( ( ) ) 8/7/2016 Example Pourbaix Diagram: Eo is calculated through the Gibbs Free Energy of reaction … Gf ------ H 20 Al2O3.H2O Al H+ ( -237.0 -1825.5 0.0 0.0 ) ( kJ/mol kJ/mol kJ/mol kJ/mol ) ( é4 ´ -237.0 - -1825.5 ù ´ 1000J / kJ o -DG ë û o rxn E = = nF 6 ´ 96485 35 E o = -1.516 Volts ) 8/7/2016 Example Pourbaix Diagram: So … ( ) E Al O /Al = -1.516 + 0.059log aH + 2 3 E Al O /Al = -1.516 - 0.059 pH 2 3 36 8/7/2016 Example Pourbaix Diagram: Potential (E) vs SHE -1.4 Al2O3.H2O -1.6 Al -1.8 -2 0 2 4 6 8 10 12 14 pH 37 8/7/2016 Example Pourbaix Diagram: Putting all our lines together … we get the “Pourbaix” Diagram for Aluminum … 38 8/7/2016 39 8/7/2016 Example Pourbaix Diagram: Note the stability lines (a) & (b) that are indicated on the diagram. These denote the “region of stability” for water based on the following reactions … Line a: 40 2H + + 2e - « H 2 Line b: O2 + 4H + + 4 e - « H 2O or equivalently: O2 + 2H 2O + 4 e - « 4OH 8/7/2016 Example Pourbaix Diagram: Again, from the Nernst equation … E H + /H = - 0.059 pH 2 - 0.0295log p H 2 We usually consider the case where pH2 = 1 atm … Line a: 41 E H + /H = - 0.059 pH 2 8/7/2016 Example Pourbaix Diagram: For line b: EO = E - 0.0148log 2 o O2 aH O 2 pO aH4 + 2 EO2o = 1.230 V (as calculated through Gibbs of formation data), thus: EO =1.230 - 0.0591 pH 2 42 8/7/2016 Evans Diagrams: Butler-Volmer Equation where: I = electrode current, Amps Io= exchange current density, Amp/m2 E = electrode potential, V Eeq= equilibrium potential, V A = electrode active surface area, m2 T = absolute temperature, K n = number of electrons involved in the electrode reaction F = Faraday constant R = universal gas constant α = so-called symmetry factor or charge transfer coefficient dimensionless The equation is named after chemists John Alfred Valentine Butler and Max Volmer 43 8/7/2016 Evans Diagrams: Butler-Volmer Equation – High Field Strength 1 nF a ia ` i0 exp RT at high anodic overpotent ial nF c ic ` i0 exp RT at high cathodic overpotent ial ia and ic are the exhange current densities for the anodic and cathodic reactions These equations can be rearranged to give the Tafel equation which was obtained experimentally 44 8/7/2016 Evans Diagrams: Butler Volmer Equation - Tafel Equation c RT RT ln i0 ln ic c nF c nF c 0.059 0.059 log i0 log ic at 25 0 C cathodic reaction cn cn a 0.059 0.059 log i0 log ia at 25 0 C anodic reaction 1 c n 1 c n The equation is the well known Tafel equation a b log i a 45 0.059 0.059 ln io or a ln io 1 n n 0.059 0.059 b or 1 n n 8/7/2016 Evans Diagrams: Current Voltage Curves for Electrode Reactions Without concentration and therefore mass transport effects to complicate the electrolysis it is possible to establish the effects of voltage on the current flowing. In this situation the quantity E - Ee reflects the activation energy required to force current i to flow. Plotted below are three curves for differing values of io with α = 0.5. 46 8/7/2016 Evans Diagrams: Current Voltage Curves for Single Electrode Reactions The iE curves from the previous slide have been rotated. Voltage Electrochemical reactions of different i0 or degrees of reversibility Current 47 8/7/2016 Evans Diagrams: Single Chemical Reaction Only at appreciable overpotentials does the reverse reaction become negligible At Ee the forward and reverse currents are equal 48 8/7/2016 Electrochemical reaction which has a large exchange current density, i0, This means that a small applied voltage results in an appreciable increase in current. Electrode reactions which have a high exchange current density are not easily polarised. Examples are the hydrogen evolution reaction on Pt and AgCl + e ↔ Ag + ClThe H+/H2(Pt) and Ag/AgCl make good reference electrodes because they are not easily polarised 49 8/7/2016 Electrochemical reaction in which the i0 value is very low. This means that it takes an appreciable over-potential to produce a significant current. This electrode is easily polarisable since a small current would result in a significant change in voltage 50 50 8/7/2016 At low overpotential the Butler Volmer equation is linear (Stern Geary equation) nF i io RT 51 51 8/7/2016 So far we have looked mainly at single electrochemical reactions 52 8/7/2016 KINETICS OF AQUEOUS CORROSION Anodic and cathodic reactions are coupled at a corroding metal surface Schematics of two distinct corrosion processes. (a) The corrosion process M + O Mn+ + R showing the separation of anodic and cathodic sites. (b) The corrosion process involving two cathodic reactions. 8/7/2016 53 Butler Volmer graphs for two electrochemical reactions Wagner Traud Method The cathodic and anodic reactions are drawn together on the same graph to show how the currents are equal at the corrosion potential 54 8/7/2016 Note in the previous diagram that: ia = ic = icorr at the corrosion potential Ecorr Ecorr is a mixed potential which lies between (Ee)c and (Ee)a. In this case it is closer to (Ee)a because the i0 and the kinetics of the anodic reaction is faster. The metal dissolution is driven by the anodic activation overpotential Ecorr - (Ee)a The cathodic reaction is driven by the cathodic activation overpotential Ecorr - (Ee)c ηa = ηc = The thermodynamic driving force ΔE = (Ee)c - (Ee)a ΔE is usually large enough to put Ecorr in the Tafel region for both reactions, i.e. the reverse reaction is negligible. 55 8/7/2016 Evans Diagrams It is convenient to represent the linear plots of i and E as log i/E plots with the negative cathodic current plotted positively, i.e. both the anodic and cathodic current appear in the positive quadrant. The linear region gives us the Tafel slopes The i0 for the individual reactions can be obtained by extrapolating back to (Ee)a and (Ee)c if these values are known. 56 8/7/2016 Evans Diagrams In this case the cathodic reaction with the higher oxidation potential is controlling the reaction 57 8/7/2016 Evans Diagrams In this example because of the faster kinetics. the cathodic reaction taking place at the lower oxidation (+ve) Potential is influencing the corrosion rate more, 58 8/7/2016 Evans Diagrams The situation in the previous example often occurs for a metal corroding in acid, compared with the metal corroding in dissolved oxygen. Despite the thermodynamic driving force, Ee, being greater for oxygen than H2/H+, the acid corrosion is faster. In some cases the oxygen and acid have a synergistic effect. For example in the case of Ni corrosion. The reaction is quite slow in sulphuric acid (0.5 M) and it is also slow in water saturated with air at pH 7. In the latter case a passive protective oxide film is formed. However, in the presence of sulphuric acid and air. The corrosion rate is relatively rapid. The acid dissolves the protective oxide film allowing oxygen to corrode the metal. 59 8/7/2016 Evans Diagrams • The relative corrosion rates of metals depends on the i0 and mass transfer. • With acid corrosion: 2H+ + e → H2 • i0 can vary from 10-3 – 10-12 A cm-2 • The Tafel slope 120 mV/decade • For oxygen corrosion O2 + H2 O + 4e → 4OH• I0 is difficult to difficult to determine because it is very low, but it is of the order of <10-10 A cm-2 • The Tafel slope >120 mV/decade 60 8/7/2016 Exchange Current Densities in 1 Molal H2SO4 61 Electrode Material -log10(A/cm2 Palladium 3.0 Platinum 3.1 Rhodium 3.6 Nickel 5.2 Gold 5.4 Tungsten 5.9 Niobium 6.8 Titantium 8.2 Cadmium 10.8 Manganese 10.9 Lead 12 Mercury 12.3 8/7/2016 α Values for Some Reactions Metal 62 System α Pt Pt Hg Hg Fe3+ Ce4+ Ti4+ 2H+ + e ↔ Fe2+ + e ↔ Ce3+ + e ↔ Ti3+ + 2e ↔ H2 0.58 0.75 0.42 0.50 Ni Ag 2H+ + 2e ↔ H2 Ag+ + e ↔ Ag 0.58 0.55 8/7/2016 Evans Diagrams • The slowest reaction controls the rate of corrosion. • Normally this is the cathodic reaction. • In this example: • A small changes in kinetics of cathode have a large effect on corrosion rate. • A small changes in kinetics of anode have small effect on corrosion 63 8/7/2016 Mass Transfer Control • If the cathodic reagent at the corrosion site (e.g., dissolved O2 in the O2 reduction) is in short supply, mass transfer of the reagent can become rate limiting. • The cathodic charge-transfer reaction at the metal/solution interface is fast enough to reduce the concentration of the reagent at interface (cathodic sites) to a value less than that in the bulk solution. • This sets up a concentration gradient and the reaction becomes diffusion controlled. ic i nFDCb C s c Lim 64 nFDCb icorr max 8/7/2016 Mass Transfer Control • When the corrosion rate is limited by mass transfer it can be increased by: • By altering the bulk concentration • By stirring and reducing the thickness of the Nernst diffusion layer ic i nFDCb C s c Lim 65 nFDCb icorr max Where : ic the cathodic current n the number of electrons F the Faraday constant Cb the bulk concentrat ion C s the surface concentrat ion the Nernst diffusion layer 8/7/2016 Mass Transfer Control Activation Controlled 66 Diffusion or Mass Transfer Controlled 8/7/2016 Mass Transfer Control Increase in corrosion potential, Ecorr, and the corrosion current, icorr, due to an increase in mass transfer caused by stirring. 67 8/7/2016 Mixed Transfer Control The cathodic Tafel plot often shows deviation from ideal Tafel behavior Polarization curve for the cathodic process showing: 1. Activation polarization 2. Joint activationconcentration polarization 3. Mass transportlimited corrosion control 68 8/7/2016 Evans Diagrams Anodic Control Cathodic Control Mixed Control 69 8/7/2016 Galvanic Corrosion – Influence of i0 70 8/7/2016