Evaluation of Nanostructured coating layers formed on Ni balls during mechanical alloying of Cu powder

A novel coating method utilizing mechanical alloying was used to deposit a nickel-copper solid solution on the surface of nickel balls in a planetary ball mill. Mechanically milled copper powders were deposited by cold welding on the activated surface of the nickel balls. The impact of the nickel balls causes surface wear, leading to formation of mixed layered particles of copper-nickel and rewelding. In addition, diffusion takes place through the coating layer to form a Ni-Cu solid solution. The hardness of the coating reached a threefold increase (HV_0.01594) in comparison with the substrate hardness. Microstructural characterization of the coating surface performed using an optical microscope, SEM, and EPMA indicates that, with appropriate processing conditions, a thick, fully dense coating can be metallurgically bonded to the nickel balls. XRD results revealed the presence of a solid solution and nanocrystalline structure.     

Structure and mechanical properties of Ni-P electrodeposited coatings

The coatings with different phosphorus contents were obtained by varying the concentration of H₃PO₃ in the electroplating bath. With the increase of phosphorus content, the structure of the Ni-P electrodeposited coatings transformed from microcrystalline to a mixture of nanocrystalline and amorphous phases, then to amorphous phase. A high hardness value of 710 HV_0.1 of as-deposited Ni-P coating was obtained at 8.3 at.% phosphorus content, and high wear resistance was accordingly achieved. The refined nanocrystalline grains with average size of about 7 nm were found to be responsible for the high hardness and improved wear resistance of the as-deposited Ni-P electrodeposited coating.     

Crystallization of mechanically alloyed amorphous W-Mg alloy under high pressure

Pure metal powder mixtures of W and Mg at the desired composition were milled in conventional high-energy ball mill, and amorphous alloy W₅₀Mg₅₀ was obtained after milling for 20 h. The structure evolution of elemental powder mixtures was studied following milling and subsequent high pressure and high temperature treatment. The amorphous alloy transform into a nanocrystalline material below 1050 °C at 4.0 GPa. On increasing the temperature, it transforms into a mixture of several new crystal phases under high-pressure condition. It also found that both mechanical alloying and high pressure treatment are the two necessary processes to form the nanocrystalline and the new phases.     

Plasticity and ab initio characterizations on Fe4N produced on the surface of nanocrystallized 18Ni-maraging steel plasma nitrided at lower temperature

18Ni-maraging steel has been entirely nanocrystallized by a series of processes including solution treatment, hot-rolling deformation, cold-drawn deformation and direct electric heating. The plasma nitriding of nanocrystallized 18Ni-maraging steel was carried out at 410 °C for 3 h and 6 h in a mixture gas of 20% N₂ + 80% H₂ with a pressure of 400 Pa. The surface phase constructions and nitrogen concentration profile in surface layer were analyzed using an X-ray diffractometer (XRD) and the glow discharge spectrometry (GDS), respectively. The results show that an about 2 μm thick compound layer (mono-phase γ′-Fe₄N) can be produced on the top of the surface layer of nanocrystallized 18Ni-maraging steel plasma nitrided at 410 °C for 6 h. The measured hardness value of the nitrided surface is 11.6 GPa. More importantly, the γ′-Fe₄N phase has better plasticity, i.e., its plastic deformation energy calculated from the load-displacement curve obtained by nano-indentation tester is close to that of nanocrystallized 18Ni-maraging steel. Additionally, the mechanical properties of γ′-Fe₄N phase were also characterized by first-principles calculations. The calculated results indicate that the hardness value and the ratio of bulk to shear modulus (B/G) of the γ′-Fe₄N phase are 10.15 GPa and 3.12 (>1.75), respectively. This demonstrates that the γ′-Fe₄N phase has higher hardness and better ductility.     

Synthesis and characterization of in situ nanocrystalline intermetallic phase reinforced AlTiSi amorphous matrix composite

Composites with partially amorphous matrix were synthesized by mechanical alloying of an Al₅₀Ti₄₀Si₁₀ elemental powder blend in a high energy planetary ball-mill, followed by high pressure (8 GPa) low temperature (350–450°C) sintering. Microstructural studies and compositional micro-analysis were carried out using scanning and transmission electron microscopy, and energy dispersive spectroscopy, respectively. Phase evolution as a function of milling time and isothermal temperature and their thermal stability was determined by X-ray diffraction at room or elevated temperature and differential scanning calorimetry, respectively. The microstructure of composites sintered between room temperature and 450°C showed nano-size (≈50 nm) crystalline precipitates of Al₃Ti dispersed in an amorphous matrix. The composites sintered at 400°C with 8 GPa pressure exhibited the highest density (3.58 Mg/m³), nanoindentation hardness (8.8 GPa), Young's modulus (158 GPa) and compressive strength (1940 MPa). A lower hardness and modulus on sintering at 450°C is attributed to additional amorphous to nanocrystalline phase transformation and partial coarsening of Al₃Ti.     

Microstructure and Mechanical Properties of Multilayer α-AlN/α-BCN Coating as Functions of the Current Density during Sputtering of a B<Subscript>4</Subscript>C Target

Multilayer AlN/BCN coating of nanometer scale have been prepared by magnetron sputtering of Al and B₄C targets in an argon–nitrogen atmosphere during deposition on a Si substrate. These coating have an X-ray amorphous structure and the maximum Knoop hardness of 27 GPa (at the current density 100 mA). The first-principle molecular dynamics calculations show that the B4–BN layer is dynamically unstable; thus, it will not be epitaxial and will be amorphous or have a structure different from the B4–BN structure. The thermal vacuum annealing from 600 to 800°C of samples with multilayer nanosized coating leads to the decrease in the Knoop hardness to 18 GPa; however, the coating structure is retained X-ray amorphous.     

Effects of surface mechanical attrition treatment (SMAT) on a rough surface of AISI 316L stainless steel

Surface mechanical attrition treatment (SMAT) improves mechanical properties of metallic materials through the formation of nanocrystallites at their surface layer. It also modifies the morphology and roughness of the work surface. Surface roughening by the SMAT has been reported previously in a smooth specimen, however in this study the starting point was a rough surface and a smoothening phenomenon is observed. In this paper, the mechanisms involved in the surface smoothening of AISI 316L stainless steel during the SMAT are elucidated. The SMAT was conducted on a specimen with a roughness of R_a = 3.98 μm for 0–20 min. The size of milling balls used in the SMAT was varied from 3.18 mm to 6.35 mm. The modification of subsurface microhardness, surface morphology, roughness and mass reduction of the specimen due to the SMAT were studied. The result shows the increasing microhardness of the surface and subsurface of the steel due to the SMAT. The impacts of milling balls deform the surface and produce a flat-like structure at this layer. Surface roughness decreases until its saturation is achieved in the SMAT. The mass reduction of the specimens is also detected and may indicate material removal or surface erosion by the SMAT. The size of milling ball is found to be the important feature determining the pattern of roughness evolution and material removal during the SMAT. From this study, two principal mechanisms in the evolution of surface morphology and roughness during the SMAT are proposed, i.e. indentation and surface erosion by the multiple impacts of milling balls. A comparative study with the results of the previous experiment indicates that the initial surface roughness has no influence in the work hardening by the SMAT but it does slightly on the saturated roughness value obtained by this treatment.     

Stress analysis at the interface between Ni-P coating and SiCp/Al substrate of space mirror

This paper investigates the mechanical properties at the interface of the coating-substrate system, which comprises the electroless nickel-phosphorus (Ni-P) coating and the aluminum matrix composite substrate reinforced by the silicon carbide particles (SiC_p/Al), and is used for the space mirror. To estimate the adhesion of Ni-P coating on SiC_p/Al substrate, the scratch adhesion testing has been performed by drawing a spherically tipped diamond indenter with a radius of 200 μm over the coated surface. The influence of the coating thickness on the interfacial stress induced by the inertial accelerations, temperature gradients and thermal soaks has been evaluated by simulation analysis based on the finite element method. The results of the scratch testing indicate that the adhesion strength of Ni-P coating to SiC_p/Al composite is more than 3.0 GPa. Compared the maximum value of the interfacial stress obtained by simulation analysis with results of the scratch testing, it is can be seen that the mirror has enough safety margin. Furthermore, the most significant conclusion that can be drawn from this work is that the coating thickness should not exceed 45 μm in order to ensure the performance and reliability of Ni-P coating and SiC_p/Al substrate system for space applications.     

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.     

Low-phosporous nickel-coated carbon microcoils: Controlling microstructure through an electroless plating process

Carbon microcoils (CMCs) have been coated with a nickel-phosphorus (Ni-P) film using an electroless plating process, with sodium hypophosphite as a reducing agent in an alkaline bath. CMC composites have potential applications as microwave absorption materials. The morphology, elemental composition and phases in the coating layer of the CMCs and Ni-coated CMCs were investigated by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD), respectively. The effects of process parameters such as pH, temperature and coating time of the plating bath on the phosphorus content and deposition rate of the electroless Ni-P coating were studied. The results revealed that a continuous, uniform and low-phosphorous nickel coating was deposited on the surface of the CMCs for 20 min at pH 9.0, plating bath temperature 70 °C. The as-deposited coatings with approximately 4.5 wt.% phosphorus were found to consist of a mix of nano- and microcrystalline phases. The mean particle size of Ni-P nanoparticles on the outer surface of the CMCs was around 11.9 nm. The deposition rate was found to moderately increase with increasing pH, whereas, the phosphorous content of the deposit exhibited a significant decrease. Moreover, the material of the coating underwent a phase transition between an amorphous and a crystalline structure. The thickness of the deposit and the deposition rate may be controlled through careful variation of the coating time and plating bath temperature.     

High coercivity nanocrystalline YCo5 powders produced by mechanical milling

High coercivity nanostructured YCo₅ powders were successfully prepared by mechanical milling of as-cast alloys and subsequent vacuum annealing. Almost single phase YCo₅ alloys, obtained by arc melting, were processed by high energy mechanical milling using a SPEX 8000 mill. After 4 h of milling, powders become nearly amorphous. DSC scans revealed the existence of an irreversible broad exothermic transition with a maximum at 516 °C associated with the crystallization process. Annealing in high vacuum at 800 °C during 2.5 min led to the formation of YCo₅ nanoparticles with an average particle size of 12 nm. A high intrinsic coercivity of 7.23 kOe together with a σ_r/σ_s ratio of 0.75 were obtained.     

Laser shock wave consolidation of nanodiamond powders on aluminum 319

A novel coating approach, based on laser shock wave generation, was employed to induce compressive pressures up to 5 GPa and compact nanodiamond (ND) powders (4-8 nm) on aluminum 319 substrate. Raman scattering indicated that the coating consisted of amorphous carbon and nanocrystalline graphite with peaks at 1360 cm⁻¹ and 1600 cm⁻¹ respectively. Scanning electron microscopy revealed a wavy, non-uniform coating with an average thickness of 40 μm and absence of thermal effect on the surrounding material. The phase transition from nanodiamond to other phases of carbon is responsible for the increased coating thickness. Vicker's microhardness test showed hardness in excess of 1000 kg_f/mm² (10 GPa) while nanoindentation test indicated much lower hardness in the range of 20 MPa to 2 GPa. Optical surface profilometry traces displayed slightly uneven surfaces compared to the bare aluminum with an average surface roughness (R_a) in the range of 1.5-4 μm depending on the shock wave pressure and type of confining medium. Ball-on-disc tribometer tests showed that the coefficient of friction and wear rate were substantially lower than the smoother, bare aluminum sample. Laser shock wave process has thus aided in the generation of a strong, wear resistant, durable carbon composite coating on aluminum 319 substrate.     

Investigation on microstructure and properties of CrAlN/AlON nanomultilayers

Artificially modulated CrAlN/AlON nanomultilayers were synthesized by direct current reactive magnetron sputtering. The microstructure and mechanical properties were evaluated by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and nano-indentation techniques. The crystallization of AlON layer and its influence on the mechanical property of the nanomultilayers were studied. The results revealed that, under the template effect of NaCl structural CrAlN layer, amorphous AlON was forced to crystallize and grew epitaxially with CrAlN layer when AlON layer thickness was below 0.9 nm, leading to an increase of hardness up to 32.8 GPa. With the further increase of the AlON layer thickness, AlON layer gradually transformed into amorphous structure and blocked epitaxial growth of the multilayers, resulting in the decrease of hardness. The effect of CrAlN layer thickness on hardness of CrAlN/AlON nanomultilayers was also investigated. With the decrease of CrAlN layer thickness, the hardness increased gradually. The maximum hardness was 34.7 GPa when CrAlN layer thickness of was 3.0 nm. The strengthen mechanism of CrAlN/AlON nanomultilayers was finally discussed.     

Amorphization of the intermetallic phase CoZr by mechanical grinding

The intermetallic phase CoZr was milled in a planetary ball mill. X-ray diffraction shows that the crystalline Bragg reflexes vanish totally with increasing milling period while simultaneously a broad maximum appears, attributed to a developing amorphous phase. To amorphize the intermetallic phase completely it takes a relatively long milling period (100 h), whereas a powder mixture of the elements of 50 at% Co and 50 at% Zr is already completely amorphized after 8 h of mechanical alloying. Both amorphous powders produced by different starting materials show identical properties by means of X-ray diffraction, measurement of the released crystallization enthalpy, the absolute specific heat capacity, and Mößbauer spectroscopy. TEM analysis of the intermetallic phase confirms the simultaneous presence of amorphous and remaining crystalline grains after short milling periods and the complete amorphization after long milling periods. A possible explanation for the amorphization process of the compound may be the accumulation of internal strain in the crystalline grains during the milling process. Another possible explanation may be the addition of iron impurities to the stoichiometric compound due to the wear debris of the milling balls and the milling vials of stainless steel.Dedicated to Professor Dr. phil., Dr. h.c. mult. Friedrich Hund on the occasion of his 95^th birthday     

Comparative Study by MS and XRD of Fe50Al50 Alloys Produced by Mechanical Alloying, Using Different Ball Mills

In this work we report a comparative study of the magnetic and structural properties of Fe₅₀Al₅₀ alloys produced by mechanical alloying using two different planetary ball mills with the same ball mass to powder mass relation. The Fe₅₀Al₅₀ sample milled during 48 h using the Fritsch planetary ball mill pulverisette 5 and balls of 20 mm, presents only a bcc alloy phase with a majority of paramagnetic sites, whereas that sample milled during the same time using the Fritsch planetary ball mill pulverisette 7 with balls of 15 mm, presents a bcc alloy phase with paramagnetic site (doublet) and a majority of ferromagnetic sites which include pure Fe. However for 72 h of milling this sample presents a bcc paramagnetic phase, very similar to that prepared with the first system during 48 h. These results show that the conditions used in the first ball mill equipment make more efficient the milling process.     

反应溅射VN/SiO2纳米多层膜的微结构与力学性能

采用V和SiO₂靶通过反应溅射方法制备了一系列具有不同SiO₂和VN调制层厚的VN/SiO₂纳米多层膜. 利用X射线衍射、X射线能量色散谱、高分辨电子显微镜和微力学探针表征了多层膜的微结构和力学性能. 结果表明：在Ar，N₂混和气体中，射频反应溅射的SiO₂薄膜不会渗氮. 单层膜时以非晶态存在的SiO₂，当其厚度小于1nm时，在多层膜中因VN晶体层的模板效应被强制晶化，并与VN层形成共格外延生长. 相应地，多层膜的硬度得到明显提高，最高硬度达34GPa. 随SiO₂层厚度的进一步增加，SiO₂层逐渐转变为非晶态，破坏了与VN层的共格外延生长结构，多层膜硬度也随之降低. VN调制层的改变对多层膜的生长结构和力学性能也有影响，但并不明显. 关键词： 2纳米多层膜')" href="#">VN/SiO₂纳米多层膜 共格外延生长 非晶晶化 超硬效应     

Influence of silicon on the microstructure and mechanical properties of Zr-Si-N composite films

A series of Zr-Si-N composite films with different Si contents were synthesized in an Ar and N₂ mixture atmosphere by the bi-target reactive magnetron sputtering method. These films’ composition, microstructure and mechanical properties were characterized by energy dispersive spectroscopy, X-ray diffraction, scanning electron microscopy, atomic force microscopy and nanoindentation. Experimental results revealed that after the addition of silicon, Si₃N₄ interfacial phase formed on the surface of ZrN grains and prevented them from growing up. Zr-Si-N composite films were strengthened at low Si content with the hardness and elastic modulus reaching their maximum values of 29.8 and 352 GPa at 6.2 at% Si, respectively. With a further increase of Si content, the crystalline Zr-Si-N films gradually transformed into amorphous, accompanied with a remarkable fall of films’ mechanical properties. This limited enhancement of mechanical properties in the Zr-Si-N films may be due to the low wettability of Si₃N₄ on the surface of ZrN grains.     

TiN/Al2O3纳米多层膜的共格外延生长及超硬效应

采用多靶磁控溅射法制备了一系列具有不同Al₂O₃调制层厚度的TiN/Al₂O₃纳米多层膜. 利用X射线能量色散谱、X射线衍射、扫描电子显微镜、高分辨透射电子显微镜和微力学探针表征了多层膜的成分、微结构和力学性能. 研究结果表明，在TiN/Al₂O₃纳米多层膜中，单层膜时以非晶态存在的Al₂O₃层在厚度小于1.5 nm时因TiN晶体层的模板效应而晶化，并与TiN层形成共格外延生长，相应地，多层膜产生硬度明显升高的超硬效应，最高硬度可达37.9 GPa. 进一步增加多层膜中Al₂O₃调制层的层厚度，Al₂O₃层逐渐形成非晶结构并破坏了多层膜的共格外延生长，使得多层膜的硬度逐步降低. 关键词： 2O₃纳米多层膜')" href="#">TiN/Al₂O₃纳米多层膜 外延生长 非晶晶化 超硬效应     

Structure and properties of (TiVCrZrY)N coatings prepared by energetic bombardment sputtering with different nitrogen flow ratios

(TiVCrZrY)N coatings were deposited onto Si substrate by the radio-frequency (RF) magnetron sputtering of a TiVCrZrY alloy target in an N₂/Ar atmosphere. The crystal, microstructural, mechanical, and electrical properties at different N₂-to-total (N₂+Ar) flow-rate ratio (R _N) values were investigated. The coating produced in pure Ar had an equiaxed structure with a hexagonal-close-packed phase. With increased R _N, the crystallinity and grain size markedly decreased. The microstructure of (TiVCrZrY)N coatings transformed from V-shaped columnar with a rough-domed surface into fine fibrous with a smooth surface. The amorphous transition layer above the substrate was also significantly thickened. The hardness of (TiVCrZrY)N decreased from 20.9 GPa to 18.9 GPa, and the electrical resistivity increased from 398.2 μΩ?cm to 21870 μΩ?cm.     

Electroless Ni-P/Ni-B duplex coatings for improving the hardness and the corrosion resistance of AZ91D magnesium alloy

The Ni-P/Ni-B duplex coatings were deposited on AZ91D magnesium alloy by electroless plating process and their structure, morphology, microhardness and corrosion resistance were evaluated. The duplex coatings were prepared using dual baths (acidic hypophosphite- and alkaline borohydride-reduced electroless nickel baths) with Ni-P as the inner layer. The coatings were amorphous in as-plated condition and crystallized and produced nickel borides upon heat-treatment. SEM observations showed that the duplex interface on the magnesium alloy was uniform and the compatibility between the layers was good. The Ni-P/Ni-B coatings microhardness and corrosion resistance of having Ni-B coating as the outer layer was higher than Ni-P coatings. The Ni-P/Ni-B duplex coatings on AZ91D magnesium alloy with high hardness and good corrosion resistance properties would expand their scope of applications.