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Article

Fabrication of a Porous TiNi3 Intermetallic Compound to Enhance Anti-Corrosion Performance in 1 M KOH

by
Zhenli He
1,
Yue Qiu
1,
Yuehui He
1,
Qian Zhao
1,
Zhonghe Wang
2 and
Yao Jiang
1,*
1
State Key Laboratory of Powder Metallurgy, Powder Metallurgy Research Institute, Central South University, Changsha 410083, China
2
College of Materials Science and Engineering, Chongqing University, Chongqing 400044, China
*
Author to whom correspondence should be addressed.
Metals 2025, 15(8), 865; https://doi.org/10.3390/met15080865 (registering DOI)
Submission received: 24 June 2025 / Revised: 28 July 2025 / Accepted: 30 July 2025 / Published: 1 August 2025
(This article belongs to the Special Issue Advanced Ti-Based Alloys and Ti-Based Materials)
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Abstract

Porous intermetallic compounds have the properties of porous materials as well as a combination of covalent and metallic bonds, and they exhibit high porosity, structural stability, and corrosion resistance. In this work, a porous TiNi3 intermetallic compound was fabricated through reactive synthesis of elemental powders. Next, detailed studies of its phase composition and pore structure characteristics at different sintering temperatures, as well as its corrosion behavior against an alkaline environment, were carried out. The results show that the as-prepared porous TiNi3 intermetallic compound has abundant pore structures, with an open porosity of 56.5%, which can be attributed to a combination of the bridging effects of initial powder particles and the Kirkendall effect occurring during the sintering process. In 1 M KOH solution, a higher positive corrosion potential (−0.979 VSCE) and a lower corrosion current density (1.18 × 10−4 A∙cm−2) were exhibited by the porous TiNi3 intermetallic compound, compared to the porous Ni, reducing the thermodynamic corrosion tendency and the corrosion rate. The corresponding corrosion process is controlled by the charge transfer process, and the increased charge transfer resistance value (713.9 Ω⋅cm2) of TiNi3 makes it more difficult to charge-transfer than porous Ni (204.5 Ω⋅cm2), thus decreasing the rate of electrode reaction. The formation of a more stable passive film with the incorporation of Ti contributes to this improved corrosion resistance performance.

1. Introduction

Porous materials, due to their high porosity, large surface areas, and good mass transfer ability, are attracting considerable attention in the fields of catalysis [1,2], filtration and separation [3,4], and biomedicine [5,6]. Porous materials can mainly be categorized into porous ceramics, porous metals, and polymer foams [7]. Among them, porous ceramics have excellent corrosion resistance but poor thermal shock resistance and high brittleness, while porous metals show excellent mechanical properties at high temperatures but poor corrosion resistance [8]. Recently, porous intermetallic compounds have attracted increasing attention due to the combination of the advantages of porous ceramics and porous metals. Porous intermetallic compounds, consisting of two or more metallic elements, possess precise stoichiometry, definite atomic configurations, and controlled crystal structure, and exhibit high structural stability and excellent corrosion resistance [9,10,11], making them suitable for work in extremely harsh conditions.
Ti-Ni intermetallic compounds have been widely investigated on account of their low cost, high abundance, hydrogen storage properties, shape memory effect, and hydrogen evolution activity [12,13,14]. According to the environment applied, Ti-based alloys spontaneously form a thermodynamically stable oxide (TiO2) which contributes to high corrosion resistance [15]. Ni-based alloys show outstanding corrosion resistance in aqueous aggressive conditions, which can be ascribed to their capacity to form a stable passive film on the surface [16]. Currently, investigations are most often carried out on the corrosion behavior of NiTi alloy, which suppresses the leaching of nickel ion and enhances corrosion resistance and biocompatibility owing to the formation of a protective TiO2 passive film on its surface [17,18,19]. However, few studies are conducted on the corrosion behavior of TiNi3. In the Ti-Ni system, TiNi3 has the best thermodynamic stability, the strongest alloying ability between Ti and Ni elements, and the highest fracture resistance [20], making it potentially suitable for application in different fields. In alkaline water electrolysis, especially, the high corrosion performance of the electrode itself is crucial in obtaining the good electrochemical stability and corrosion behavior required for long-term operation in practical applications [21]. The Ni element can improve catalytic activity, whereas the Ti element can contribute to passivation. Thus, a combination of Ni and Ti to obtain porous TiNi3 is important for simultaneously achieving good anti-corrosion performance and high activity. In our previous work, we found that porous TiNi3 shows good hydrogen evolution reaction performance in 1 M KOH. Therefore, it is important to investigate the corrosion behavior of porous TiNi3 to meet the demands of practical applications.
The synthesis methods for fabricating intermetallic compounds include reactive synthesis, electrodeposition, and chemical vapor deposition [22,23,24]. Reactive synthesis, with its low cost and short process time, is an extensively utilized method for fabrication of porous intermetallic compounds based on the Kirkendall effect. Reactive synthesis mainly involves powder mixing, pressing, and sintering, which endows intermetallics with good pore formation and pore structure regulation abilities [22,25,26]. Researchers have successfully prepared porous Ni3Al intermetallics [27] and porous Ti-Si-Mo intermetallic compounds with about 40% porosity [28] via reactive synthesis.
In this work, a porous TiNi3 intermetallic compound with good corrosion resistance was prepared using reactive synthesis of elemental powders. The phase composition and pore structure properties of the porous TiNi3 intermetallic compound were investigated in detail during the synthesis process. The corrosion behavior of the porous TiNi3 intermetallic compounds in 1 M KOH solution was assessed via electrochemical measurement. Passive behavior was studied by electrochemical impedance spectroscopy and X-ray photoelectron spectroscopy methods.

2. Materials and Methods

2.1. Materials and Chemicals

Ti powder (~28.7 μm, 99.9%, Beijing Xing Rong Yuan Technology Co., Ltd., Beijing, China), Ni powder (~33.1 μm, 99.9%, Beijing Xing Rong Yuan Technology Co., Ltd., Beijing, China) (Figure 1), and KOH (Sinopharm Chemical Reagent Co., Ltd., Shanghai, China) were utilized as received in this work. Deionized water (18 MΩ∙cm) was provided by an ultrapure purification system.

2.2. Preparation of Materials

To achieve a homogeneous mixture of powders, following our previous work [14], elemental powders of Ti and Ni were thoroughly mixed for 48 h according to an atomic ratio of 1:3 through a V-type mixer. After that, the powder mixture was loaded into a sintering boat (size = 15 × 76 × 11 mm), which was sintered in a vacuum furnace through loose-powder sintering. The vacuum degree was held at 1 × 10−2 Pa or below, and the heating rate was maintained at 5 °C/min. According to the equilibrium Ti-Ni phase diagram [29], the sintering was performed at 750 °C, 900 °C, 1100 °C, and 1300 °C for 2 h, followed by cooling to room temperature.
The porous Ni was also prepared by loose-powder sintering. The sintering was carried out at 750 °C, 900 °C, and 1100 °C for 2 h.

2.3. Characterization Techniques

X-ray diffraction (XRD) was performed on a RigakuD/Max2500 diffractometer (Cu kα, λ = 0.154056 nm, Rigaku Corporation, Tokyo, Japan), and a simple surface treatment was conducted by grinding with sandpaper before XRD testing. A field emission scanning electron microscope (FE-SEM, MIRA 3, Tescan, Brno, Czech Republic) was applied to record the SEM images. The X-ray photoelectron spectra (XPS) were acquired by an ESCALABSB 250 Xi spectrometer (Thermo Fisher Scientific, Waltham, MA, USA) with Al Kα radiation and a 0.05 eV scanning step. Open porosity was tested according to Archimedes’ method using the following equation:
P   =   m 3   −   m 1 m 3   −   m 2   ×   100
where P is the open porosity (%), m1 is the mass of the specimen in atmospheric air, m2 is the mass of the specimen after submergence in water, and m3 is the mass of the specimen after water from the surface is wiped off.

2.4. Electrochemical Measurements

Corrosion behavior in 1 M KOH solution at room temperature was assessed on a CHI660D workstation. Electrochemical tests were carried out using a typical three-electrode system, in which the specimen (exposed area of 1 cm2), the saturated calomel electrode (SCE), and the graphite sheet were used as the working electrode, the reference electrode, and the counter electrode, respectively. Potentiodynamic measurements were acquired at a low scan rate (1 mV/s). Electrochemical impedance spectroscopy (EIS) tests were carried out in a 0.01 Hz–105 Hz frequency range with 5 mV amplitude.

3. Results and Discussion

3.1. Characteristics of Phase and Microstructure

The phase compositions of TiNi3 intermetallic compounds sintered at different temperatures are displayed in Figure 2. At the sintering temperature of 750 °C, the sintered sample is composed of the Ti (PDF#05-0682), TiNi3 (PDF#51-1169), TiNi (PDF#27-0344), and solid solution (Ni) (PDF#01-1258) phases. Among them, the diffraction peaks of the Ti phase are in good agreement with those of the standard card, while all the diffraction peaks of the Ni phase are shifted by a small angle, indicating the formation of a solid solution (Ni). At the sintering temperature of 900 °C, the main phases are solid solution (Ni), TiNi, and TiNi3 phases in the sintered sample. An obvious diffusion reaction at this stage occurred between Ti and (Ni), leading to depletion of the Ti phase and a sharp decrease in the (Ni) phase, as well as the formation of TiNi3 phases and TiNi phases. At 1100 °C, the sintered sample includes TiNi3, solid solution (Ni), and TiNi phases. The decreased peak intensities of (Ni) and TiNi and the increased peak intensity of TiNi3 demonstrate that large numbers of TiNi3 phases were generated by the diffusion reaction between solid solution (Ni) and TiNi. When the sintering temperature is 1300 °C, a single-phase TiNi3 can be formed because of the uniform diffusion.
Figure 3 exhibits backscattered electron (BSE) images of the microstructure of TiNi3 sintered at different temperatures. The phase composition at different sintering temperatures can be determined by combining the results obtained from XRD and energy dispersive X-ray (EDX). At the sintering temperature of 750 °C, the minority of TiNi and TiNi3 phases are formed at the Ti and Ni interface (Figure 3a). At the sintering temperature of 900 °C, large amounts of TiNi and TiNi3 phases are generated and the Ti is depleted due to the more intensive diffusion reaction between Ti and Ni (Figure 3b). At this time, TiNi3 is a major phase, while the TiNi phase is surrounded by a thin layer of TiNi3 phase. At 1100 °C, most of the TiNi phase is replaced by the TiNi3 phase (Figure 3c). When the temperature is increased to 1300 °C, the sintered sample is uniformly diffused, consisting of a single-phase TiNi3 (Figure 3d).
Figure 4 shows the pore structure micromorphology of the sintered TiNi3 intermetallic compound at 1300 °C. The sintered TiNi3 intermetallic compound possesses an abundant open pore structure with a high open porosity of 56.5%. There are two kinds of typical pore structure in the TiNi3 intermetallic compound. One type of pore structure is characterized by huge numbers of large pores which exhibit good connectivity. These large pores are primarily from the gaps between the powder particles because of the bridging effect of the powder particles. Another type of pore structure is characterized by low numbers of fine pores which are generated in the interior of the powder particles, with pore sizes of only a few micrometers. These fine pores are mainly caused by the Kirkendall effect associated with the unequal diffusion rates between Ni and Ti. Therefore, based on these two pore-formation mechanisms, abundant pore structures are formed in the TiNi3 intermetallic compound.

3.2. Corrosion Resistance Behavior

The corrosion behaviors of porous TiNi3 intermetallic compound and porous Ni were investigated in 1 M KOH. Before potentiodynamic polarization measurement, the open circuit potential (OCP) of the specimen was tested to reach a steady state. Figure 5a displays the OCP curve of TiNi3 over 3500 s. It can be seen that the OCP declines within the initial 700 s and then gradually stabilizes. Figure 5b shows the potentiodynamic polarization curves. These curves clearly show that the specimens exhibited typical passive behavior, indicating no fundamental change in the electrochemical feature with Ti addition. The breakdown potential is regarded as the critical potential at the rapid increase in current density, which indicates the capacity of the protective film to restrain local corrosion in corrosive environments [30,31]. It can be seen in Figure 5b that the passivation region of TiNi3 is significantly wider than that of Ni, and the corresponding breakdown potential of TiNi3 shifts toward a more positive value than Ni, indicating that the introduction of Ti significantly improved the passive property and suppressed local corrosion performance. In addition, the current density at which the potentiodynamic polarization curve is located in the relatively flat area, termed the steady-state current density, which can be regarded as a parameter to evaluate overall corrosion resistance [32]. The steady-state current density of TiNi3 is also smaller than that of Ni, indicating the increased protective performance of the passive film.
From the potentiodynamic polarization curves for the samples, the corrosion potential (Ecorr) and corrosion current density (Icorr) were estimated by extrapolation of the anodic and cathodic Tafel curves. The Ecorr of the porous Ni to the TiNi3 intermetallic compounds is obviously shifted from −1.053 VSCE to −0.979 VSCE, indicating a reduction in thermodynamic corrosion tendency through the introduction of Ti. The Icorr is directly related to the corrosion rate of the material, and a larger Icorr value indicates an increased mass loss during the corrosion processes [33]. The Icorr values of the TiNi3 intermetallic compound and porous Ni are 1.18 × 10−4 and 7.56 × 10−4 A∙cm−2, respectively, suggesting a slower corrosion rate for the TiNi3 intermetallic compound. These results indicate that the incorporation of Ti accelerates the formation of a more stable passive film, thus promoting the corrosion resistance of the TiNi3.
Figure 5c presents Nyquist diagrams for the TiNi3 intermetallic compound and porous Ni in 1 M KOH solution. It can be seen that both Nyquist curves exhibit the shape of a single semicircle, indicating that the corrosion process is controlled by the charge transfer process [34]. In general, the semicircle diameter in a Nyquist diagram reflects the strength of the corrosion resistance of the material [35]. A large arc radius indicates a difficult electron transfer process involving a low number of electron transfers per unit time [36]. It can be seen that the capacitive semicircle for the TiNi3 intermetallic compound is larger than that for the porous Ni. This indicates a greater resistance to charge transfer, i.e., better corrosion resistance, through the introduction of Ti.
To further analyze the corrosion property of the TiNi3 intermetallic compound, the Nyquist plots were fitted by the equivalent circuit model (Figure 5d). The fitting results are listed in Table 1. In this model, Rs, Rf, Rct, and CPE represent solution resistance, passive film resistance, charge transfer resistance, and the constant phase element, respectively. The Rf value of the TiNi3 intermetallic compound (2.26 Ω∙cm2) is greater than that of Ni (0.77 Ω∙cm2), indicating a faster rate of formation of a passive film on the surface and, thus, better corrosion protective performance. Meanwhile, the Rct value of the TiNi3 intermetallic compound (713.9 Ω∙cm2) is greater than that of Ni (204.5 Ω∙cm2), making charge transfer more difficult and decreasing the rate of electrode reaction accordingly. This is because the Ti element contributes to formation of the passive film and enhances the surface coverage of the passive film. In addition, polarization resistance is denoted by Rp ( 1 R p   =   1 R ct   +   1 R f ) , with a larger RP value represents a more stable passivation film and lower corrosion activity [37]. According to the calculation results, the RP values of the TiNi3 intermetallic compound and porous Ni are 2.25 and 0.77 Ω∙cm2, respectively, suggesting that the TiNi3 intermetallic compound produces a more stable passivation film, resulting in improvement in corrosion resistance, in agreement with the polarization curves.
The relationship between corrosion resistance and passive film composition in the TiNi3 intermetallic compound before and after corrosion was further studied by XPS. The Ni 2p spectra in Figure 6a show that the peaks at 873.1 and 855.5 eV correspond to Ni2+ 2p1/2 and Ni2+ 2p3/2, respectively, consistent with results obtained before corrosion [38]. As for Ti 2p (Figure 6b), the binding energies at 454.86 and 460.84 eV correspond to Ti 2p3/2 (Ti0) and Ti 2p1/2 (Ti0), and the binding energies at 458.6 and 464.31 eV are assigned to Ti 2p3/2 (Ti4+) and Ti 2p1/2 (Ti4+), respectively [39]. The increased proportion of Ti4+ content after corrosion enhances the thickness of the films. The O 1s peaks include O2− (530.22 eV) and OH− (531.83 eV) (Figure 6c), with OH− being related to the adsorbed H2O or hydrated metal oxides [40]. In the case of the sample after corrosion, the increased OH−/O2− ratio of TiNi3 may be due to the presence of metal hydroxide/oxide (such as Ti) on the surface, which then undergoes further hydrolytic polymerization [41]. Therefore, the film on the surface from XPS analysis includes oxidized Ni and Ti, and the equations for the reaction in the alkaline environment can be stated as follows [42,43]:
Ni + 2OH− → Ni(OH)2 + 2e−
Ni(OH)2 → NiO + H2O
Ti + 2OH− → TiO2 + H2 + 4e−
Ti + 2H2O → TiO2 + 2H2
Figure 7 shows the surface morphology and the pore structure of the TiNi3 intermetallic compound after the potentiodynamic polarization test. It can be seen that the porous TiNi3 intermetallic compound after the polarization test still maintains good pore structure in comparison to the initial specimen. Additionally, there are no corrosion products or pitting observed on the surface, suggesting that TiNi3 exhibits good structural stability in the alkaline environment.

4. Conclusions

A porous TiNi3 intermetallic compound was successfully prepared by elemental powder reactive synthesis and found to possess abundant pore structures and good corrosion resistance in 1 M KOH solution. The polarization curves revealed typical passive behavior, and the smaller steady-state current density of TiNi3 improved the protective performance of the passive film. The EIS results indicated better corrosion resistance due to the introduction of Ti, as evidenced by an increased capacitive semicircle and a higher Rp value. The pore structure after the polarization test remained unchanged, and thus demonstrated good structural stability. The porous TiNi3 intermetallic compound described in this study exhibited good anti-corrosion performance, proving its potential for practical applications in alkaline conditions.

Author Contributions

Z.H.: Validation, writing—original draft, writing—review and editing. Y.Q.: Investigation, methodology, and writing—original draft. Y.H.: Writing—review and editing, validation, and resources. Q.Z.: Investigation, formal analysis, and validation. Z.W.: Investigation, formal analysis, and methodology. Y.J.: Conceptualization, funding acquisition, resources, and writing—review and editing. All authors have read and agreed to the published version of the manuscript.

Funding

This work was supported by the National Natural Science Foundation of China (No. 51971251).

Data Availability Statement

The original contributions presented in this study are included in the article. Further inquiries can be directed to the corresponding author.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Micromorphology of Ti and Ni powders. (a) Ti powders, (b) Ni powders.
Figure 1. Micromorphology of Ti and Ni powders. (a) Ti powders, (b) Ni powders.
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Figure 2. XRD patterns of the mixed Ti−Ni powders at different sintering temperatures during the solid-state sintering process.
Figure 2. XRD patterns of the mixed Ti−Ni powders at different sintering temperatures during the solid-state sintering process.
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Figure 3. Microstructure images and corresponding EDX element mapping images of porous TiNi3 intermetallic compound sintered at different temperatures. (a) 750 °C, (b) 900 °C, (c) 1100 °C, (d) 1300 °C.
Figure 3. Microstructure images and corresponding EDX element mapping images of porous TiNi3 intermetallic compound sintered at different temperatures. (a) 750 °C, (b) 900 °C, (c) 1100 °C, (d) 1300 °C.
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Figure 4. Micromorphology of pore structure of TiNi3 intermetallic compound sintered at 1300 °C. (a–c) BSE images, (d–f) secondary electron (SE) images.
Figure 4. Micromorphology of pore structure of TiNi3 intermetallic compound sintered at 1300 °C. (a–c) BSE images, (d–f) secondary electron (SE) images.
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Figure 5. Corrosion behaviors of porous TiNi3 intermetallic compound sintered at 1300 °C and porous Ni in 1 M KOH solution. (a) Open circuit potential curve of TiNi3, (b) potentiodynamic polarization curves, (c) Nyquist plots, (d) the equivalent circuit model.
Figure 5. Corrosion behaviors of porous TiNi3 intermetallic compound sintered at 1300 °C and porous Ni in 1 M KOH solution. (a) Open circuit potential curve of TiNi3, (b) potentiodynamic polarization curves, (c) Nyquist plots, (d) the equivalent circuit model.
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Figure 6. The XPS spectra of TiNi3 intermetallic compound before and after corrosion. (a) Ni 2p, (b) Ti 2p, (c) O 1s.
Figure 6. The XPS spectra of TiNi3 intermetallic compound before and after corrosion. (a) Ni 2p, (b) Ti 2p, (c) O 1s.
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Figure 7. SEM images of TiNi3 intermetallic compound before and after the test. (a,b) Before the polarization test, (c,d) after the polarization test.
Figure 7. SEM images of TiNi3 intermetallic compound before and after the test. (a,b) Before the polarization test, (c,d) after the polarization test.
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Table 1. Fitting parameters obtained from EIS tests.
Table 1. Fitting parameters obtained from EIS tests.
SamplesRs (Ω cm2)CPE1 (F/cm2)Rf (Ω cm2)CPE2 (F/cm2)Rct (Ω cm2)
TiNi30.626.453 × 10−72.266.998 × 10−3713.9
Ni2.765.621 × 10−50.776.191 × 10−3204.5
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MDPI and ACS Style

He, Z.; Qiu, Y.; He, Y.; Zhao, Q.; Wang, Z.; Jiang, Y. Fabrication of a Porous TiNi3 Intermetallic Compound to Enhance Anti-Corrosion Performance in 1 M KOH. Metals 2025, 15, 865. https://doi.org/10.3390/met15080865

AMA Style

He Z, Qiu Y, He Y, Zhao Q, Wang Z, Jiang Y. Fabrication of a Porous TiNi3 Intermetallic Compound to Enhance Anti-Corrosion Performance in 1 M KOH. Metals. 2025; 15(8):865. https://doi.org/10.3390/met15080865

Chicago/Turabian Style

He, Zhenli, Yue Qiu, Yuehui He, Qian Zhao, Zhonghe Wang, and Yao Jiang. 2025. "Fabrication of a Porous TiNi3 Intermetallic Compound to Enhance Anti-Corrosion Performance in 1 M KOH" Metals 15, no. 8: 865. https://doi.org/10.3390/met15080865

APA Style

He, Z., Qiu, Y., He, Y., Zhao, Q., Wang, Z., & Jiang, Y. (2025). Fabrication of a Porous TiNi3 Intermetallic Compound to Enhance Anti-Corrosion Performance in 1 M KOH. Metals, 15(8), 865. https://doi.org/10.3390/met15080865

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