Preparation and properties of electroless Ni-P-SiO2 composite coatings

Dispersible SiO₂ nanoparticles were co-deposited with electroless Ni-P coating onto AISI-1045 steel substrates in the absence of any surfactants in plating bath. The resulting Ni-P/nano-SiO₂ composite coatings were heat-treated for 1 h at 200 °C, 400 °C, and 600 °C, respectively. The hardness and wear resistance of the heat-treated composite coatings were measured. Moreover, the structural changes of the composite coatings before and after heat treatment were investigated by means of X-ray diffraction (XRD), while their elemental composition and morphology were analyzed using an energy dispersive spectrometer (EDS) and a scanning electron microscope (SEM). Results show that co-deposited SiO₂ particles contributed to increase the hardness and wear resistance of electroless Ni-P coating, and the composite coating heat-treated at about 400 °C had the maximum hardness and wear resistance.     

Influences of laser remelting on microstructure of nanostructured Al2O3-13 wt.% TiO2 coatings fabricated by plasma spraying

The effects of laser remelting on microstructure of nanostructured Al₂O₃-13 wt.% TiO₂ ceramic coatings prepared by plasma spraying with agglomerated powders were studied. The microstructure of the feedstock, as-sprayed and laser-remelted coatings were investigated by using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffractometry (XRD). The results indicate that the plasma-sprayed ceramic coating consists of both fully melted regions and partially melted regions. The totally ceramic coating, especially the fully melted regions, has a typical plasma-sprayed lamellar-like structure as the conventional coating, and has some pores. According to the difference of microstructures, the partially melted regions can be divided into liquid-phase sintered regions (a three-dimensional net or skeleton-like structure: Al₂O₃-rich submicron particles embedded in the TiO₂-rich matrix) and solid-phase sintered regions (remained nanoparticles). The lamellar defect of the as-sprayed coating is erased, and the compactness of the coating is improved significantly after laser remelting. The laser-remelted region composed of fine equiaxed grains, which are different from the conventional column-like crystals along the direction of the heat current. Due to the rapid solidification of laser remelting process, there are still some nanoparticles in the remelted region because of an insufficient time for grains growth.     

Microstructures and tribological properties of plasma sprayed WC-Co-Cu-BaF2/CaF2 self-lubricating wear resistant coatings

A promising WC-Co-Cu-BaF₂/CaF₂ self-lubricating wear resistant coating was deposited via atmospheric plasma spraying (APS) process by using homemade feedstock powders composed of WC-Co, Cu and BaF₂/CaF₂ eutectic. The as-prepared cermet coatings had better frictional behavior comparing with the WC-Co coating. Moreover, the often-occurred decarburization of WC in APS process was noticeably improved due to the binding of copper and BaF₂/CaF₂ phase, which not only offered effective solid lubrication, but also acted as bind phases to mend the microstructure and protected WC from decomposition. The optimized specimen contained 10 wt.% Cu and 10 wt.% BaF₂/CaF₂ in a WC-Co matrix, which had excellent frictional and wear performance. The wear mechanism of the self-lubricating wear resistant coating was discussed with the microstructures, compositions and mechanical properties of the composite materials in detail.     

Study of the synthesis and Cl2 gas-sensing properties of nanometer HNO3-doped SnO2

We focused on the effects of the inorganic acid HNO₃ on the gas-sensing properties of nanometer SnO₂ and prepared the powders via a dissolution-pyrolysis method. Furthermore, the powders were characterized by means of X-ray diffraction (XRD), scanning electron microscope (SEM), field emission scanning electron microscopy (FESEM) and energy-dispersive X-ray spectra (EDS). Several aspects were surveyed, including the calcining temperature, concentration of nitric acid and the working temperature. The results showed that the gas response of 3 wt% HNO₃-doped SnO₂ powders (calcined at 500 °C) to 10 ppm Cl₂ reached 316.5, at the working temperature 175 °C. Compared with pure SnO₂, appropriate HNO₃ could increase the gas sensitivity to Cl₂ gas more significantly.     

SHS等离子喷涂制备FeAl2O4-Al2O3-Fe纳米复合涂层的研究

利用SHS等离子喷涂技术，将经过机械团聚法制备的Fe₂O₃-Al复合粉体送入等离子焰流，沉积出厚度约为400 μm的复合涂层.利用XRD，SEM 和TEM等检测手段对涂层的成分和组织进行了分析，测定了涂层的显微硬度、断裂韧性以及耐磨性.结果表明涂层为具有纳米结构的FeAl₂O₄-Al₂O₃-Fe纳米复合组织；涂层的显微硬度为HV_100g870；断裂韧性是普通Al₂O₃涂层的2倍；无润滑磨损的耐磨性是普通Al₂O₃涂层的2.5倍. 关键词： SHS等离子喷涂 纳米涂层 断裂韧性     

Laser clad Ni-base alloy added nano- and micron-size CeO2 composites

Micron-size Ni-base alloy (NBA) powders are mixed with both 1.5 wt% (%) micron-CeO₂ (m-CeO₂) and also 1.0–3.0% nano-CeO₂ (n-CeO₂) powders. These mixtures are coated on low carbon steel (Q235) by 2.0 kW CO₂ laser cladding. The effects on microstructures, microhardness and wear resistance of the coating by the addition of m- and n-CeO₂ powders to NBA (m- and n-CeO₂/NBA) have been investigated. Addition to the primary phases of γ-Ni, Cr₂₃C₆ and Ni₃B of NBA coating, CeNi₃ shows up both in m- and n-CeO₂/NBA coatings and CeNi₅ appears only in n-CeO₂/NBA coating. Directional dendrite and coarse equiaxed dendrite are grown in m-CeO₂/NBA coating from interface to central zone, whereas multi-oriented dendrite and fine equiaxed dendrite growth by addition of n-CeO₂. The microhardness and wear resistance of coatings are greatly improved by CeO₂ powder addition, and compared to the addition of 1.0% and 3.0%, 1.5% n-CeO₂/NBA is the best. Hardness and wear resistance of the coating improves with decreasing CeO₂ size from micron to nano.     

电解等离子体法制备Al2O3陶瓷层及其特性研究

利用电弧喷铝并重熔后进行电解等离子体处理(EPP)的方法在Q235钢基体上制备出呈冶金结 合的Al₂O₃陶瓷层.利用XRD，SEM和EDS等手段对陶瓷层的成分和显 微组织进行了分析， 测定了陶瓷层的耐蚀性能和耐磨性能.实验结果表明，陶瓷层主要由α-Al₂O3，γ-Al₂O₃，θ-Al₂O₃以及一 些非晶相组成，组织致密，耐蚀性能和耐磨性能良好. 关键词： 电解等离子体处理 陶瓷层 复合技术 生长机理     

Preparation and properties of composite ceramic coating containing Al2O3–ZrO2–Y2O3 on AZ91D magnesium alloy by plasma electrolytic oxidation

A composite ceramic coating containing Al₂O₃–ZrO₂–Y₂O₃ was successfully prepared on AZ91D magnesium alloy by plasma electrolytic oxidation (PEO) technique in an alkaline aluminate electrolyte. The morphology, elemental and phase composition, corrosion behavior and thermal stability of the uncoated and coated samples were studied by environmental scanning electron microscopy (ESEM), energy dispersive X-ray spectrometer (EDS), X-ray diffractometer (XRD), electrochemical corrosion test, high temperature oxidation test and thermal shock test. The results showed that the composite ceramic coating was composed of Al₂O₃, c-ZrO₂, t-ZrO₂, Y₂O₃ and some magnesium compounds, such as MgO, MgF₂ and MgAl₂O₄. After PEO treatment, the corrosion potential of AZ91D alloy was increased and the corrosion current density was significantly reduced. Besides, the coated magnesium alloys also showed excellent high temperature oxidation resistance and thermal shock resistance at 500 °C environment.     

Distribution of oxygen vacancies and gadolinium dopants in ZrO2–CeO2 multi-layer films grown on α-Al2O3

Gdolinia doped ZrO₂ and CeO₂ multi-layer films were deposited on α-Al₂O₃ (0001) using oxygen-plasma-assisted molecular-beam epitaxy. Oxygen vacancies and Gd dopant distributions were investigated in these multi-layer films using X-ray diffraction (XRD), conventional and high-resolution transmission electron microscopy (HRTEM), annular dark-field imaging in scanning transmission electron microscopy (STEM), X-ray energy dispersive spectroscopy (EDS) elemental mapping and X-ray photoelectron spectroscopy (XPS) depth profiling. EDS and XPS depth profiling reveal that the Gd concentration in the ZrO₂ layer is lower than that in the CeO₂ layer. As a result, a higher oxygen vacancy concentration exists in the CeO₂ layers compared to that in the ZrO₂ layers. In addition, Gd is found to segregate only at the interfaces formed during the deposition of CeO₂ layers on ZrO₂ layers. On the other hand, the interfaces formed during the deposition of ZrO₂ layers on CeO₂ layers did not show any Gd segregation. The Gd segregation behavior at every other interface is believed to be associated with the low solubility of Gd in ZrO₂.     

Electrodeposition and tribological properties of Ni-SrSO4 composite coatings

Ni-SrSO₄ composite coatings were electrodeposited on superalloy Inconel 718 from a Watts electrolyte containing a SrSO₄ suspension. Ni-SrSO₄ coatings were investigated by scanning electron microscope, microhardness tester, and friction and wear tester in sliding against a bearing steel ball under unlubricated condition. The incorporation of SrSO₄ into Ni matrix increases the microhardness of electrodeposited coatings. Ni-SrSO₄ composite coating exhibits a distinctly low friction coefficient and a small wear rate as contrasted with pure Ni coating and the substrate. The effect of SrSO₄ particles on microstructure and tribological properties of Ni-SrSO₄ composite coatings is discussed.     

Wear resistance of reactive plasma sprayed and laser remelted TiB2-TiC0.3N0.7 based composite coatings against medium carbon steel

Wear resistance of reactive plasma sprayed TiB₂-TiC_0.3N_0.7 based composite coatings and the as-sprayed coating with laser surface treatment was investigated using plate-on-plate tests. Wear tests were performed at different normal loads and sliding speeds under dry sliding conditions in air. The surface morphologies of counterparts against as-sprayed and laser remelted coatings were investigated. The microstructure and chemical composition of wear debris and coatings were studied using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS), respectively. The results show that the wear resistance of the laser remelted coating is improved significantly due to their increased microhardness and reduced flaws. The primary wear mechanism of the remelted coating is oxidation wear and its minor wear mechanisms are grain abrasion and fatigue failure during the course of wear test. In contrast, the primary wear mechanism of the as-sprayed coating is grain abrasion at the low sliding speed (370 rpm) and fatigue failure at the high sliding speed (549 rpm). The oxidation wear mechanism is a minor contributor for the as-sprayed coating.     

Synthesis and characterization of thermoluminescent glass-ceramics Li2O-Al2O3-SiO2:CeO2

Vitroceramic powders of Li₂O-Al₂O₃-SiO₂ systems (LAS), doped with 1% (LAS:1Ce) and 10% (LAS:10Ce) molar of cerianite (CeO₂) were synthesized by means of the gelification technique of metal formates of aluminum and lithium, in the presence of tetraethoxy silane and CeO₂. The gels obtained were dried (120 °C, 2.5 h), calcined (480 °C, 5 h) and sinterized (1250 °C, 30 min). The sinterized samples were characterized by X-ray difraction (XRD), scanning electron microscopy (SEM) and microchemical analysis (EDS). There is evidence for a mixture of two phases of 64% β-spodumene (Li₂O-Al₂O₃-4SiO₂) and 36% β-eucryptite (Li₂O-Al₂O₃-2SiO₂). The LAS:1Ce system was enriched in aluminum, the LAS:10Ce system showed areas of heterogeneous composition; some regions with a shortage of CeO₂, while others zones with cerium cumulus. From the microscopy images it was found that CeO₂ acts as a densificant agent in LAS system, favoring the sintering in the host. The chemical route and the sintering processes utilized allow the production of samples exhibiting an acceptable linear correlation between total thermoluminescent emission intensity and the irradiation dose when the CeO₂ concentration is low (less than 1%), opening the possibility of using this kind of glass-ceramic in dosimetry.     

Influences of CO2 laser annealing on mechanical and laser-induced damage properties of ZrO2 thin films

Zirconium dioxide (ZrO₂) thin films were deposited on BK7 glass substrates by the electron beam evaporation method. A continuous wave CO₂ laser was used to anneal the ZrO₂ thin films to investigate whether beneficial changes could be produced. After annealing at different laser scanning speeds by CO₂ laser, weak absorption of the coatings was measured by the surface thermal lensing (STL) technique, and then laser-induced damage threshold (LIDT) was also determined. It was found that the weak absorption decreased first, while the laser scanning speed is below some value, then increased. The LIDT of the ZrO₂ coatings decreased greatly when the laser scanning speeds were below some value. A Nomarski microscope was employed to map the damage morphology, and it was found that the damage behavior was defect-initiated both for annealed and as-deposited samples. The influences of post-deposition CO₂ laser annealing on the structural and mechanical properties of the films have also been investigated by X-ray diffraction and ZYGO interferometer. It was found that the microstructure of the ZrO₂ films did not change. The residual stress in ZrO₂ films showed a tendency from tensile to compressive after CO₂ laser annealing, and the variation quantity of the residual stress increased with decreasing laser scanning speed. The residual stress may be mitigated to some extent at proper treatment parameters.     

Influences of Bi2O3 on microstructure and magnetic properties of MnZn ferrite

MnZn ferrites were prepared by conventional oxide ceramic process. The effects of Bi₂O₃ on microstructure and magnetic properties of MnZn ferrites were investigated by means of characterizing the fracture surface micrograph, composition of grain boundary, magnetic properties and density by scanning electron microscope (SEM), energy dispersive X-ray spectroscope (EDS), B-H analyzer and Archimedes method, respectively. The results indicate that Bi₂O₃ mainly segregates and concentrates in the grain boundary regions, promotes solid-state reaction and grain growth, reduces porosity and enhances density. Optimum addition of Bi₂O₃ increases the permeability and saturation magnetic induction, meanwhile ensures the well frequency stability of permeability.     

XPS investigation of diffusion of two-layer ZrO2/SiO2 and SiO2/ZrO2 sol–gel films

Two-layer ZrO₂/SiO₂ and SiO₂/ZrO₂ films were deposited on K9 glass substrates by sol–gel dip coating method. X-ray photoelectron spectroscopy (XPS) technique was used to investigate the diffusion of ZrO₂/SiO₂ and SiO₂/ZrO₂ films. To explain the difference of diffusion between ZrO₂/SiO₂ and SiO₂/ZrO₂ films, porous ratio and surface morphology of monolayer SiO₂ and ZrO₂ films were analyzed by using ellipsometry and atomic force microscopy (AFM). We found that for the ZrO₂/SiO₂ films there was a diffusion layer with a certain thickness and the atomic concentrations of Si and Zr changed rapidly; for the SiO₂/ZrO₂ films, the atomic concentrations of Si and Zr changed relatively slowly, and the ZrO₂ layer had diffused through the entire SiO₂ layer. The difference of diffusion between ZrO₂/SiO₂ and SiO₂/ZrO₂ films was influenced by the microstructure of SiO₂ and ZrO₂.     

Single-calcination synthesis of pyrochlore-free Pb(Ni1/3Nb2/3)O3-PbTiO3 using a coating method

Pyrochlore-free 0.64Pb(Ni_1/3Nb_2/3)O₃-0.36PbTiO₃ (0.64PNN-0.36PT) powder has been successfully synthesized by only one calcination step using a coating method. The formation of pyrochlore phase is prevented by coating NiCO₃·2Ni(OH)₂·2H₂O on Nb₂O₅ particles. NiCO₃·2Ni(OH)₂·2H₂O-coated Nb₂O₅ powder is prepared by heterogeneous precipitation method. The coating structure is confirmed by transmission electron microscope (TEM) with energy dispersive spectroscope (EDS). Single calcination treatment of the coating powder mixed with appropriate amounts of Pb₃O₄ and TiO₂ powders at 900 °C for 2 h produces the pure-perovskite 0.64PNN-0.36PT powder. The elimination of the pyrochlore phase can be explained in terms of the separating of Pb₃O₄ and Nb₂O₅ by the NiCO₃·2Ni(OH)₂·2H₂O coating layer.     

Microstructure and wear behavior of γ/Al4C3/TiC/CaF2 composite coating on γ-TiAl intermetallic alloy prepared by Nd:YAG laser cladding

As a further step in obtaining high performance elevated temperature self-lubrication anti-wear composite coatings on TiAl alloy, a novel Ni-P electroless plating method was adopted to encapsulate the as-received CaF₂ in the preparation of precursor NiCr-Cr₃C₂-CaF₂ mixed powders with an aim to decrease its mass loss and increase its compatibility with the metal matrix during a Nd:YAG laser cladding. The microstructure of the coating was examined using X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS) and the friction and wear behavior of the composite coatings sliding against the hardened 0.45% C steel ring was evaluated using a block-on-ring wear tester at room temperature. It was found that the coating had a unique microstructure consisting of primary dendrites TiC and block Al₄C₃ carbides reinforcement as well as fine isolated spherical CaF₂ solid lubrication particles uniformly dispersed in the NiCrAlTi (γ) matrix. The good friction-reducing and anti-wear abilities of the laser clad composite coating was suggested to the Ni-P electroless plating and the attendant reduction of mass loss of CaF₂ and the increasing of it's wettability with the NiCrAlTi (γ) matrix during the laser cladding process.     

Laser cladding of in situ TiB2/Fe composite coating on steel

To enhance the wear resistance of mechanical components, laser cladding has been applied to deposit in situ TiB₂/Fe composite coating on steel using ferrotitanium and ferroboron as the coating precursor. The phase constituents and microstructure of the composite coating were investigated using X-ray diffraction (XRD), scanning electron micrograph (SEM) and electron probe microanalysis (EPMA). Microhardness tester and block-on-ring wear tester were employed to measure the microhardness and dry-sliding wear resistance of the composite coating. Results show that defect-free composite coating with metallurgical joint to the steel substrate can be obtained. Phases presented in the coating consist of TiB₂ and α-Fe. TiB₂ particles which are formed in situ via nucleation-growth mechanism are distributed uniformly in the α-Fe matrix with blocky morphology. The microhardness and wear properties of the composite coating improved significantly in comparison to the as-received steel substrate due to the presence of the hard reinforcement TiB₂.     

Preparation and characterization of nickel nano-Al2O3 composite coatings by sediment co-deposition

Ni-Al₂O₃ composite coatings were prepared by using sediment co-deposition (SCD) technique and conventional electroplating (CEP) technique from Watt's type electrolyte without any additives. The microstructure, hardness, and wear resistance of resulting composites were investigated. The results show that the incorporation of nano-Al₂O₃ particles changes the surface morphology of nickel matrix. The preferential orientation is modified from (2 0 0) plane to (1 1 1) plane. The microhardness of Ni-Al₂O₃ composite coatings in the SCD technique are higher than that of the CEP technique and pure Ni coating and increase with the increasing of the nano-Al₂O₃ particles concentration in plating solution. The wear rate of the Ni-Al₂O₃ composite coating fabricated via SCD technique with 10 g/l nano-Al₂O₃ particles in plating bath is approximately one order of magnitude lower than that of pure Ni coating. Wear resistance for SCD obtained composite coatings is superior to that obtained by the CEP technique. The wear mechanism of pure Ni and nickel nano-Al₂O₃ composite coatings are adhesive wear and abrasive wear, respectively.     

Cu2ZnSnSe4 thin films prepared by selenization of co-electroplated Cu-Zn-Sn precursors

A novel technique for growth of high quality Cu₂ZnSnSe₄ (CZTSe) thin films is reported in our work. The CZTSe thin films were fabricated onto Mo layers by co-electroplating Cu-Zn-Sn precursors followed by annealing in the selenium vapors at the substrate temperature of 550 °C. The morphology and structure of CZTSe thin films were characterized using scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), X-ray diffraction (XRD) and Raman scattering spectrum, respectively. The results revealed that the single phase was in the CZTSe thin films, and the other impurities such as ZnSe and Cu₂SnSe₃ were not existed though they were difficult to distinguish both from EDS and XRD.