Abstract
The characteristics of (Re+Ir)-rich Re-Ir-Ni alloy films electroplated galvanostatically from citrate aqueous solutions with low pH of 2.0~2.5 were investigated. The effects of electroplating variables and bath chemistry on surface morphology, chemical composition and crystallographic structure of the films were studied. The morphology, composition and phase of the alloy films were characterized by environmental scanning electron microscopy, X-ray energy dispersive spectroscopy and X-ray diffraction, respectively. The results show that a dense and bright Re-Ir alloy file is obtained under the conditions of current density of 60 mA·cm-2 and pH=2.0. Increasing temperature results in good quality of the alloys at pH=2.5, but at pH=2.0 the result is opposite. The films deposited at bath temperatures of 60~70 °C and pH=2.0 consist of amorphous phase. At bath temperature of 80 °C, the films consist of ReO3 phase. At current density of 60 mA·cm-2, the crystallographic structure of the film changes from an amorphous phase to a mixture of crystalline and amorphous phases when pH is increased from 2.0 to 2.5. The phases of crystalline are hcp-Ir0.4Re0.6 and hcp-Ni.
Science Press
Rhenium (Re) has a high melting point, high modulus, superior strength and ductility at elevated temperatures[1-3]. Due to these unique properties, Re and its alloy can be widely used in aerospace, nuclear, electrical, chemical, biomedical, as well as catalysis in petroleum industry[4]. However, like all refractory metals, the oxidation of Re is poor in moist air at high temperatures above 600 °C [2]. In order to protect them against high-temperature oxidation, noble metallic platinum (Pt), iridium (Ir) or rhodium (Rh) can be used as an oxidation-resistant layer or incorporated additives to protect Re from oxidizing at high temperature[5-7]. Ir has a high melting point, low oxygen permeability, excellent chemical stability, good corrosion resistance, and displays a thermal expansion coefficient matched with Re and an extensive mutual solubility with Re and there is no intermetallic compounds in Re-Ir binary phase diagram[8-12]. Noble metallic Ir as an effective diffusion barrier for inward-diffusing oxygen is one of the most promising candidates for protective layer of Re-based components in extreme environments[13-19].
The manufacturing processes of Re and its alloys include powder metallurgy[2], electron beam-physical vapor deposition[4,20], chemical vapor deposition (CVD)[3,21], electro-plating[22,23], double-glow plasma[24] and electroless[25,26]. The electrodeposition of Re and its alloy may become an alternative method, which is widely employed in the deposition of pure, uniform, adherent metals and alloys at low temperatures in aqueous bath. It is found that electroplated Re has a low Faradaic efficiency (FE) and poor quality[22]. Adding one of iron-group metal salts to the plating bath will result in high FE and form Re-Me alloys (Me=Ni, Co or Fe) with high Re-content, so the iron-group metals show a catalytic effect on the electroplating of Re[27-29]. For manufacturing processes of Ir and its alloys, CVD[28], physical vapor deposition[30-33] and electrodeposition[34-39] processes can be applied. The electroplating of Ir from aqueous solution has some disadvantages with respect to the stability of electrolyte and the quality of deposits[40]. In addition, hydrogen evolution might lead to deterioration of the deposits, cracking and low FE. Combined with manufacturing processes for Ir, Re and their alloys, the co-deposition of Re-Ir-based alloy by electrodeposition was investigated in terms of some electroplating variables[36,37]. However, in order to achieve the maximal service temperature of the films, it is necessary to further increase the (Re+Ir)-content in the alloy deposits by the change of bath temperature (T), bath pH, current density (j) or bath chemistry.
It is well known that the morphology and chemical composition of electroplated materials are related to the electroplating variables, such as current density, electrolyte composition, bath pH and bath temperature. Cohen Sagivet M et al[41] investigated the effects of bath chemistry on the FE and composition of Re-Ir-Ni alloy films, and found that Re-Ir-based alloy films with Re-content as high as 73at% and Ir-content as high as 29at% are plated under galvanostatic conditions (j=50 mA·cm–2) at pH=5.0 and T=70 °C. Wu et al[42] further studied the effects of bath pH and temperature on characteristics of Re-Ir-Ni films, and found that the pH can significantly affect the morphology and composition of the films. The (Re+Ir)-rich alloy films with few cracks were obtained when bath pH was 2.0~3.5 and other variables remained unchanged. The variation of bath pH in citrate-containing perrhenates, Ir3+ and Ni2+ electroplating baths result in the formation of different metal-citrate complexes, which are expected to have an impact on the overall electroplating process and the nature of the deposits[43-45]. In addition, the bath chemistry, deposition temperature and current density are other important parameters in electroplating of the alloy films. Therefore, this study just focused on the (Re+Ir)-rich Re-Ir-Ni alloy films electroplated galvanostatically from citrate aqueous solutions with a low pH of 2.0~2.5. Under low pH values of 2.0 and 2.5, the effects of bath temperature, current density and Ni2+ content on the morphology, chemical composition and crystallographic structure of Re-Ir-based alloy films were further studied.
In the experiment, a copper (Cu) disc with an exposed surface area of 1.6 cm2 was welded with Cu wire by a spot welder machine. The Cu disc was used as the working electrode (WE). Prior to deposition, the Cu disc surface was cleaned with surfactant soap water in an ultrasonic bath for 10 min in order to remove major contaminants, and then immersed in nitric acid solutions (volume ratio of nitric acid:deionized water is 1:1) at room temperature for about 1 min, and subsequently rinsed with deionized water by a plastic squeeze bottle, followed by cleaning with acetone in an ultrasonic bath.
A three-electrode cell was used for the deposition of the alloys on the Cu disc surface. The three-electrode consisted of a WE of Cu disc as cathode, two platinum foils as the counter-electrode (CE) placed at ~5 mm away on both sides of the WE, and a saturated Ag/AgCl reference electrode (RE). The bath chemistry and deposition conditions are listed in Table 1. In a typical preparation process, 35 mmol/L ammonium perr-henate, 35 mmol/L iridium(III) chloride hydrate, 35 mmol/L citric acid and 8~35 mmol/L nickel sulfaminate were dissolved in deionized water on a magnetic stirring apparatus with a magnetic stir bar. The bath pH of the solution was examined by pH meter 510 from Eutech Instruments, and adjusted to the desired value by adding 5.0 mol/L sodium hydroxide solution at room temperature under magnetic stirring. The applied current density and the bath temperature were controlled by a Princeton Applied Research model 263A Potentiostat/Galvanostat and a MRC B300 thermostatic bath, respectively. The bath solution was purged with pure N2 for 15 min before turning on the current. A N2 blanket was passed above the solution during deposition. In order to maintain homogeneity of the solution and to reduce pitting, a magnetic stir bar was used to stir the solution.
Table 1 Bath chemistry and deposition conditions
| Parameter | Value |
|---|
|
NH4ReO4/mmol/L |
35 |
|
IrCl3·nH2O/mmol/L |
35 |
|
Ni(NH2SO3)2/mmol/L |
8~35 |
|
C6H8O7/mmol/L |
35 |
|
pH |
(2.0, 2.5)± 0.1 |
|
Temperature, T/°C |
(60~80)±1.0 0.0 |
|
Current density, j/mA·cm-2 |
40~60 |
|
Deposition time/h |
1 |
|
Electrolyte volume/mL |
~10 |
The mass change before and after each deposition was measured by an analytical balance (BA 210 Sartorius, resolution 0.1 mg). The phases and crystallographic structure of the selected (Re+Ir)-rich alloy films were determined by X-ray diffraction (XRD, Scintag, USA) equipped with a Cu-Kα radiation source. The deposited specimens were examined by an environmental scanning electron microscopy (ESEM, Quanta 200 FEG, FEI) operated in the high vacuum mode, equipped with the attached liquid-nitrogen-cooled Oxford Si X-ray energy dispersive spectroscopy (EDS) detector.
2.1 Effect of bath temperature
The current density and Ni2+ concentration were 50 mA·cm-2 and 35 mmol/L, respectively. Fig.1 shows the effect of bath temperature on chemical composition of the alloys. At pH=2.0, a pure Re deposit is obtained at T=80 °C (Fig.1a). The (Re+Ir)-content is about 99at% and 88at% at 60 and 70 °C, respectively. When pH increases to 2.5, the concen-tration of Ir decreases slightly. The concentration of Ni maintains constant with increasing the temperature from 60 to 70 °C, and increases slightly at T=80 °C (Fig.1b). The (Re+Ir)-content is 87at%, 90at% and 75at% at 60, 70 and 80 °C, respectively. The surface morphologies of alloys at different temperatures are shown in Fig.2.
Fig.1 Effect of bath temperature on chemical composition of alloys deposited at pH value of 2.0 (a) and 2.5 (b)
Fig.2 ESEM images of surface of alloys deposited at different temperatures: (a, b) 60 °C, (c, d) 70 °C and (e, f) 80 °C
The effect of bath temperature on the crystallographic structure of the alloys deposited at pH=2.0 is shown in Fig.3. When bath temperatures are 60 and 70 °C, the strong reflections from Cu substrate are apparent (JCPDS file #04-0836), indicating that thin deposits are formed. A broad halo at ~42° indicates that the deposits consist of amorphous phase. The formation of the metastable amorphous phase may be attributed to the high Re-content, and the relatively low deposition temperature, which result in low diffusion and high activation energy for crystallization. With increasing the temperature to 80 °C, some weak reflections form on the XRD pattern. These reflections indicate that there is a new Re oxide (ReO3) phase (JCPDS file #40-1155). In addition, the result of EDS pattern also reveals that the film formed at T=80 °C is composed of Re oxide.
The effect of current density on chemical composition of the alloys is shown in Fig.4. In this system, the bath temperature is 70 °C and Ni2+ concentration is 35 mmol/L. At pH=2.0, the Re-content increases with increasing the current density, but the Ir-content decreases. The highest Ir-content of 39at% is obtained at j=40 mA·cm-2. A Re-Ir alloy is formed, but there is no evidence of Ni deposition at j=60 mA·cm-2 (Fig.4a), as we hoped. When pH increases to 2.5, the highest Re-content and the lowest Ir- and Ni-content appear at j=50 mA·cm-2 (Fig.4b). With increasing the current density, the (Re+Ir)-rich alloys are obtained. In this system, the (Re+Ir)-content in the alloys is higher than 70at%.
Fig.5 shows the ESEM images of the surface of the alloys deposited at different current densities. When pH=2.0, the surface morphologies are shown in Fig.5a and 5c. A black deposit is obtained at j=40 mA·cm-2. The rough surface presents some particles and small grooves (Fig.5a), indicating that the film is very thin. At j=50 mA·cm-2, the surface morphology is shown in Fig.2c. At j=60 mA·cm-2, the surface of the deposit is smooth and has no cracks (Fig.5c). The film thickness is about 3.8 μm. With increasing the current density, the surface structure is evolved from rough to dense and smooth. When pH is 2.5, the surface morphologies are present in Fig.5b and 5d. At j=40 mA·cm-2, the surface is not covered completely with the deposits, and some large grooves are present (Fig.5b). With increasing the current density, the dense and smooth films are obtained (Fig.5d); further, the surface of the coarse-grained film has some micro-cracks (Fig.5d). The thickness is uniform, about 6.2 μm. The fracture surface is composed of fine grains, containing a through-thickness micro-cracking. Therefore, the tolerable current densities for the sound deposits are found to be 60 mA·cm-2 at pH=2.0, and 50 mA·cm-2 at pH=2.5.
Fig.5 ESEM images of the surface of the alloys deposited at pH=2.0 (a, c), pH=2.5 (b, d) and different current densities: (a, b) j= 40 mA·cm-2 and (c, d) j=60 mA·cm-2
Netherton and Holt[46] suggested that the composition of electroplated Re-Ni alloys is not changed with pH or current density. The increase of current density may lead to spongy deposits and almost halved Re-content in Re-Ni deposits[23]. In this study, the increase of current density is available for the electrodeposition of ternary alloys at low pH. The low applied current density results in poor quality of the deposits, which are uncovered completely on the surface of the substrate. In addition, the Re-content of Re-Ir-Ni alloys increases with increasing the current density at pH=2.0, but at pH=2.5 it is complex. Therefore, the electroplating process of Re-Ir-Ni alloys is different from that of Re-Ni alloys.
When the applied current density is 60 mA·cm-2, the effect of pH on the crystallographic structure of the film is shown in Fig.6. The strong reflections from Cu substrate are present, indicating that a thin film is formed. At pH=2.0, a big broad halo at ~42° indicates that the Re92Ir8 film is made of amorphous phase. The atomic radii of Re and Ir are very close. Thus, Ir atoms may occupy substitutional sites of the hexagonal Re host lattice, forming a solid solution of Re-Ir alloy. When pH increases to 2.5, the chemical composition of the deposit is changed. The reflections from the substrate still appear. In addition, new reflections, possibly related to crystalline hcp-Ir0.4Re0.6 and hcp-Ni, appear. The big and weak broad reflection at 39°~45° indicates that the solid solution is formed in the Re62Ir24Ni14 deposit, which consists of a mixture of crystalline (hcp-Ir0.4Re0.6 and hcp-Ni phases) and amorphous phases. In previous work, the Re-Ir-Ni ternary alloys with low Re-content (<40at%) consist of two same phases with nanosized crystallites[41,42]. In this study, Re62Ir24Ni14 alloy with a small amount of amorphous phase may be attributed to the high Re-content. The similar results have been reported by Younes[47] and Zabinski et al[45], that is, it is attributed to an increase of W or Re content in W-Ni or Re-Ni alloy films, respectively. The crystallographic structure of the film is determined by Re content in the alloy films. The bath chemistry, bath temperature, bath pH and the applied current density influence the structure only indirectly, in their effects on the Re-content of the alloy films.
2.3 Effect of Ni ion concentration
Fig.7 shows the effect of Ni2+ concentration on chemical composition of the alloys at T=70 °C and j=50 mA·cm-2. When pH=2.0, the concentration of Ni in the deposits gradually increases with increasing the Ni2+ concentration. When the Ni2+ concentration is 8 mmol/L, Re-Ir alloy is obtained (Fig.7a). When pH=2.5, the Ir-content decreases significantly with increasing the Ni2+ concentration, but the Re-content changes contrarily (Fig.7b). Re-Ir alloy is composed of 6at% Re and 94at% Ir, with low Ni2+ addition concentration of 8 mmol/L. The low (Re+Ir)-content is about 70at% when Ni2+ concentration is 16 mmol/L. Here, oxygen content is excluded from the experimental result. In fact, the chemical composition of the alloy includes oxygen, indicating that the films are oxidized during deposition in this system.
Fig.7 Effect of Ni2+ content on chemical composition of the alloys deposited when T=70 °C and j=50 mA·cm-2: (a) pH=2.0 and (b) pH=2.5
Fig. 8 shows the ESEM images of the top surface of the alloys deposited with different Ni2+ addition concentrations. When pH=2.0, the black deposits are obtained at low Ni2+ concentration of 8~16 mmol/L. The surface is composed of many white particles, and some grooves are present (Fig.8a). With increasing the Ni2+ content and other variables being constant, the surface of the deposit consists of large agglomerate in the form of small white particles with cauliflower-like pattern. The fine nanoparticles are present (Fig.8c). With increasing pH value, these white particles disappear (Fig.8b and 8d). However, the surface is not uniform, some large agglomerates are present (Fig.8d). Although the low Ni2+ concentration can result in high (Re+Ir)-content in the alloys, the poor quality of the films is not likely to be applied in practical engineering.
Fig.8 ESEM images of the top surface of films with different Ni2+ contents: (a, b) 8 mmol/L and (c, d) 16 mmol/L
Fig.9 illustrates the XRD patterns of the films deposited with different Ni2+ concentrations at pH=2.0 and pH=2.5. For pH=2.0, the film is composed of Re oxide when the concentrations of Ni2+ are 8 and 16 mmol/L. Unfortunately, the diffraction peaks corresponding to metallic Ir are not observed when the concentration of Ni2+ is 16 mmol/L at pH=2.5. It can be concluded that the film with Ir-content of 94at% is composed of Ir-C-O complex or Ir3+ from plating solutions. Therefore, there are not metallic alloy layers in this system (Fig.8), containing oxides, Ir-C-O complex or Ir3+ from solutions.
In Fig.7d, the highest Ir-content in an alloy (up to 94 at%) is found, indicating that the deposition of Ir3+ is favored. According to the above results at low bath pH, we can find out that the high Re-content in the deposit is obtained as the deposition parameters, namely bath temperature and current density are varied (Fig.1 and 4). At pH=2.0 and pH=2.5, the main species in solution are H3Cit and H2Cit-, and the relative abundance of H3Cit is larger than that of H2Cit-. Considering the perrhenate-citrate complexes, it is known that ReO4H2Cit2- is formed below as well as above pH=3.0. The rate of dissociation of the ReO4H2Cit2- complex is independent of pH in the range of 3~5.5. However, below pH=3.0, the dissociation rate increases rapidly with decreasing pH, approaching a first-order dependence on H+ at pH=2.0[44]. We thus can hypothesize that this complex that is less stable at pH=2.0 or pH=2.5 allows efficient plating of the alloy, which results in an increase in the Re-content.
Regarding the complexing properties of Ni2+ with species derived from citric acid, nickel can exist in solution either as “free” Ni2+, as NiCit– or as [NiCit2]4–. There can be other complexes, but what really matters is the ratio of the stoichiometric concentrations of citrate to that of Ni. It is well known that the rate of deposition of free Ni ion is faster than that of Ni-citrate ion, and it is almost blocked completely when there is a large excess of the complex with two citrate species. The two predominate complexes of Ni with citrate are Ni (50%) and [NiCi2]4– (50%) when pH is 2.0 and 2.5[23]. Brenner[48] suggested that the citrate ion forms complexes with the iron-group metals, thereby inhibiting the rate of their deposition and consequently favoring the deposition of Re. With the combination of the mechanism for deposition process of electroplating Re-Ir-Ni alloy, the deposition of Ni is blocked due to the complexes of Ni-citrate, and the content of Ir thus increases[41].
1) The Re-Ir-based alloy films can be electroplated from low pH acid citrate solutions. Re-Ir-based alloy films with Re-content as high as 100at% and Ir-content as high as 94at% are obtained, and the (Re+Ir)-content exceeds 70at%.
2) The bath temperature has a significant impact on chemical composition and morphology of the alloys. The Re-Ir-Ni alloys with no cracks are obtained at 60 and 70 °C when pH=2.0. With increasing the temperature up to 80 °C, a ReO3 film is found, but its quality is poor. Increasing the bath temperature results in poor quality of the alloys formed at pH=2.0, but it is opposite when pH=2.5.
3) The high current densities are available for electrodeposition of the alloys, resulting in good quality of the deposits. The tolerable current densities for sound deposits are 60 mA·cm-2 at pH=2.0 and 50 mA·cm-2 at pH=2.5. A bright Re-Ir binary alloy without cracks forms at j=60 mA·cm-2 at pH=2.0.
4) Decreasing the Ni2+ concentration results in high (Re+Ir)-content (>70at%), but there are no metallic alloy layers. These deposits are composed of oxides, Ir-C-O complex or Ir3+ from plating solutions. When Ni2+ contents are 8 and 16 mmol/L, the surface of black deposits at pH=2.0 is composed of agglomerates in the form of small white particles with cauliflower-like pattern. The low Ni2+ concentration results in poor quality of the films, which is not likely to be applied in practical engineering.
5) At pH=2.0, the alloys deposited at 60 and 70 °C consist of amorphous phases. When the applied current density is 60 mA·cm-2, the crystallographic structure of the film is changed from an amorphous phase to a mixture of crystalline (hcp-Ir0.4Re0.6 and hcp-Ni phases) and amorphous phases as the pH is increased from 2.0 to 2.5.
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