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Liaoning Key Laboratory Complex Workpiece Surface Special Treatment, Liaoning University of Science and Technology, Anshan 114051, China
A Quasi‐multinary Composite Coating On A Nickel‐rich Ncm Cathode Material For All‐solid‐state Batteries
Received: October 21, 2021 / Revised: November 25, 2021 / Accepted: November 27, 2021 / Published: December 1, 2021
To have high electrical conductivity and good corrosion resistance, a transition metal nitride coating used to protect electronic interconnects in marine environments is necessary. This study synthesized a new CrN-Pt coating with dense growth texture. Pt addition led to a marked increase in electrical conductivity and corrosion resistance. The resistivity decreased from 0.0149 Ohm·cm in the CrN coating to 0.000472 Ohm·cm in the CrN-Pt coating, while the corrosion current density decreased from 24 nA/cm.
On the CrN-Pt coating. The results of the above studies confirm that Pt doping has significant advantages in improving the electrical conductivity and corrosion resistance of nitride coatings for potential applications in the marine environment.
Electrical bonding metals suffer from severe passivation reaction or galvanic corrosion when exposed to the marine environment. Passivation films or corrosion products formed on their surface significantly reduce the efficiency of signal transmission and therefore result in a significant decrease in the reliability of electronic equipment [1, 2, 3]. The production of advanced functional coatings is a possible strategy to extend the service life of electrical connectors in marine environments; however, such coatings should have low resistivity and excellent corrosion resistance.
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Transition metal nitride coatings have high hardness, good chemical inertness, and high resistance to wear and corrosion. These properties make them promising candidates for resisting severe tribocorrosion in the marine environment [ 4 , 5 , 6 , 7 , 8 , 9 , 10 , 11 , 12 , 13 , 14 , 15 , 16 , 17 , 18 ]. Dual chromium nitride (CrN) coatings are developed to increase wear and corrosion resistance on high-speed rotating parts; however, these coatings have shown insufficient service life in industrial applications [13]. In some harsh working environments, such as seawater, the corrosion resistance of CrN coatings does not meet the requirements of long service life. Triple CrXN coatings, where X = W, Mo, Al, Ti, Si, C, etc. mechanical, tribological and anti-corrosion properties. In contrast, the Pt element has high chemical inertness and good corrosion resistance, and Pt doping is expected to effectively improve the corrosion resistance of CrN coatings. However, so far there is no information on Pt doping in CrN coatings. Moreover, relatively little work has been done on the electrical conductivity of these coatings. Here, a novel CrN-Pt coating was fabricated by plasma enhanced magnetron sputtering (PEMS). The potential effect of Pt doping on the growth structure, electrical conductivity and corrosion property of the CrN coating was studied through detailed characterization.
CrN and CrN-Pt coatings were synthesized using the PEMS technique [21]. High purity chromium (99.6%) and platinum (99.9%) were used as targets. 316 L austenitic steel and silicon wafer were chosen for the substrate. These samples were polished with metallographic sandpaper and then ultrasonically cleaned in pure alcohol for 15 minutes. All samples were mounted on a rotating substrate holder. Before coating preparation, the samples were thoroughly treated with Ar
-ions with a bias voltage of 120 V, an argon flow of 100 sccm, and a sputtering time of 60 min. The Cr metal layer was first deposited on the substrate in an argon gas atmosphere. The bias voltage, argon flow, power, and sputtering time were −100 V, 100 sccm, 5000 W, and 5 min, respectively. Top CrN and CrN-Pt coatings were prepared in a gaseous mixture of Ar (99.99%) and high-purity N.
(99.99%). During coating deposition, additional tungsten filaments acted as electron emission sources to cause ionization of gas and metal atoms. These ionized N ions then reacted with metal ions to form a nitride coating. The deposited coatings were prepared with the following parameters: -100 V bias voltage, 100 sccm argon gas flow, 100 sccm nitrogen gas flow, 5000 W power, and 100 min coating time. The composition of the deposited coatings was determined by energy dispersive X-ray spectroscopy (EDS, Bruker, Karlsruhe, Germany) equipped with scanning electron microscopy (SEM, Zeiss ∑IGMA HD, Carl Zeiss, Jena, Germany). X-ray diffraction (XRD, X’ Pert Powder, PANalytical B.V., Almelo, The Netherlands) was performed to study the crystal structures of all layers within the 2θ range scanned from 20° to 90°. The growth textures of all coatings were observed by scanning electron microscopy (SEM, Zeiss ∑IGMA HD). An atomic force microscope (AFM, Oxford MFP-3DInfinity, Abingdon, UK) was used to evaluate the surface roughness (Ra) of the coating. The resistivity of the layers was obtained using a Hall effect measurement system (Hall 8800, Precision Systems Industrial Limited, Taiwan, China) at a room temperature of 25 °C. Corrosion tests were performed using an electrochemical station (CHI760e, Chenhua Instrument Corp, Shanghai, China). The etching medium was a NaCl solution with a concentration of 3.5 wt %. The reference electrode (RE), counter electrode (CE) and working electrode (WE) were saturated calomel electrode (SCE), Pt plate and coating sample, respectively. The exposed area of the coating sample was 1 cm
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. The length, width, and height of the Pt plate were 10, 10, and 0.5 mm, respectively. All electrodes were placed in a standard cell. The scan was in the range of -0.3 ~ 1 V. The scan rate was 1 mV/s. Statistical potential (E
) was used to evaluate corrosion resistance. According to equation (1), the protective efficiency of the coating can be calculated as follows
In addition, electrochemical impedance spectroscopy (EIS) tests were performed and collected in the frequency range from 100 kHz to 0.01 Hz. Each test was repeated three times under the same conditions to check reproducibility. After the corrosion tests, the surface topographies of all layers were observed by SEM.
Table 1 summarizes the composition of CrN and CrN-Pt coatings. The composition of the CrN coating is 53.48 at.% chromium, 45.16 at.% nitrogen and 1.36 at.% oxygen. In contrast, the composition of the CrN-Pt coating is 45.97 at.% chromium, 39.26 at.% nitrogen, 13.33 at.% platinum, and 1.44 at.% oxygen. Trace amounts of oxygen can probably be attributed to adsorption during exposure to air.
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Figure 1 shows the SEM surface image and the elemental map of the CrN-Pt coating. It can be seen that the deposited CrN-Pt coating has a smooth surface feature. Corresponding element mapping shows that these component elements (e.g. Pt and Cr) show a relatively uniform distribution in the deposited coating. It has been reported that the nitride/Ag composite film has a two-phase structure consisting of metallic Ag and nitride matrix. Ag can be dissolved in the ceramic matrix or exist as an isolated phase [22, 23]. Based on these above results, these Pt atoms are probably dissolved within the CrN matrix or distributed independently at the grain boundaries.
Figure 2 shows the XRD results of CrN and CrN-Pt coatings. The diffraction peaks of the CrN coating are centered at 36.82°, 43.24°, 62.75°, and 75.36°, which are mainly assigned to the (111), (200), (220), and (311) crystal planes of the CrN phases (JCPDS11). ) -0065). These CrN phases are also detected in the CrN-Pt coating, while three distinct characteristic peaks at 39.88°, 46.07°, and 68.24°, attributed to the (111), (200), and (220) planes of this coating, are detected. metallic state Pt (JCPDS 87-0640). A partially enlarged drawing placed in Fig. 2 shows a strong (200) diffraction peak in the CrN-Pt coating.
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