Microstructure and tribological performance of self-lubricating diamond/tetrahedral amorphous carbon composite film

In order to smooth the rough surface and further improve the wear-resistance of coarse chemical vapor deposition diamond films, diamond/tetrahedral amorphous carbon composite films were synthesized by a two-step preparation technique including hot-filament chemical vapor deposition for polycrystalline diamond (PCD) and subsequent filtered cathodic vacuum arc growth for tetrahedral amorphous carbon (ta-C). The microstructure and tribological performance of the composite films were investigated by means of various characterization techniques. The results indicated that the composite films consisted of a thick well-grained diamond base layer with a thickness up to 150 μm and a thin covering ta-C layer with a thickness of about 0.3 μm, and sp³-C fraction up to 73.93%. Deposition of a smooth ta-C film on coarse polycrystalline diamond films was proved to be an effective tool to lower the surface roughness of the polycrystalline diamond film. The wear-resistance of the diamond film was also enhanced by the self-lubricating effect of the covering ta-C film due to graphitic phase transformation. Under dry pin-on-disk wear test against Si₃N₄ ball, the friction coefficients of the composite films were much lower than that of the single PCD film. An extremely low friction coefficient (∼0.05) was achieved for the PCD/ta-C composite film. Moreover, the addition of Ti interlayer between the ta-C and the PCD layers can further reduce the surface roughness of the composite film. The main wear mechanism of the composite films was abrasive wear.     

Electromagnetic wave absorption properties of carbonyl iron-ferrite/PMMA composites fabricated by hybridization method

The surface of carbonyl iron powder or a mixture of carbonyl iron and ferrite was coated with polymethylmethacrylate (PMMA) microspheres by a hybridization method to make hybrid powders, and then electromagnetic wave absorption properties of the hybrid composites prepared with these hybrid powders have been investigated. As for the carbonyl iron/PMMA hybrid composite, the reflection loss less than −20 dB could be achieved in a frequency range of 1.7–5.0 GHz when the composite thickness was below 5.00 mm. In the case of the carbonyl iron-ferrite/PMMA hybrid composite, a similar reflection loss was observed in a frequency range of 4.3–13.0 GHz. Thus, the addition of ferrite was found to be useful for achieving a large absorption in a wide frequency range, especially for higher frequency values. Simulated values for the minimum reflection loss are well agreed with actually measured ones, because of homogeneous distribution of carbonyl iron and/or ferrite in these hybrid composites.     

Elimination of surface scratch/texture on the surface of single crystal Si substrate in chemo-mechanical grinding (CMG) process

Si wafers are widely used as a substrate material for fabricating ICs. The quality of ICs depends on the quality of Si wafers. The chemo-mechanical grinding (CMG) with soft abrasive grinding wheels (SAGW) has been recently found to be a great potential process for machining Si wafers to generate superior surface quality at low cost. However, there have been very few studies on observing variation of topography of scratch/texture and understanding basic eliminating process of scratch/texture on the ground Si wafer. Furthermore, few reports on the variation of surface roughness and material removal rate (MRR) during CMG process and relationship between MRR and surface roughness during CMG process are presented. In this paper, a series of CMG experiments have been conducted to study the elimination process of artificial scratches created on etched Si surfaces and residual textures induced by SD1500 diamond wheel in CMG process, and to understand the topography variations of Si surfaces and some basic grinding characteristics during CMG process.     

Nanoporous carbon spheres and their application in dispersing silver nanoparticles

Monodisperse nanoporous carbon spheres (NCS) were synthesized in large quantities via a facile hydrothermal synthesis. It is found that the NCS have rough surfaces with a large quantity of uniformly distributed protruding and concaving zones. Large quantities of nanopores of about 0.3 nm in diameter are distributed uniformly on the whole sphere surfaces. The effects of reaction parameters on the surface roughness, sphere diameter and pore size of NCS were investigated. Taking the NCS as substrates, silver nanoparticles (NPs) were deposited onto their surfaces using a one-step ultrasonic electrodeposition procedure. The deposited silver NP has a uniform distribution, a high particle density and a narrow size range of 12-16 nm in diameter. This study demonstrates an efficient approach to fabricate noble-metal/carbon nanocomposites.     

Roughness and fibre reinforcement effect onto wettability of composite surfaces

Wettability of glass/epoxy and carbon/epoxy composites materials has been determined via sessile drop technique. Good-Van Oss approach has been used to evaluate surface free energy parameters of smooth and rough surfaces. Results obtained point out the influence of fibre reinforcement on surface free energy of composite materials. In addition, the interest of surface treatment to increase surface roughness has been discussed in terms of wettability. To sum up, results obtained clearly demonstrate the necessity of considering properties of a given composite surface not only as a polymer but a fibre/polymer couple. The drawn conclusions are of great interest as it may have numerous consequences in applications such as adhesion.     

AFM investigation on surface evolution of amorphous carbon during ion-beam-assisted deposition

Hydrogen-free amorphous carbons (a-C) have been prepared on mirror-polished Si(1 1 1) wafers through thermally evaporated C₆₀ with simultaneous bombardments of Ne⁺ ions. The time evolution of film surfaces has been characterized by atomic force microscopy (AFM) at two temperatures of 400 and 700 °C, respectively. Based on the topography images and the root-mean-square (rms) roughness analysis, it is found that the a-C surfaces present roughening growth at the initial stage. With increasing growth time, the cooperative nucleation of the islands and pits appears on the surfaces, suggesting three-dimensional growth, and then they continue to evolve to irregular mounds at 400 °C, and elongated mounds at 700 °C. At the steady growth stage, these surfaces further develop to the structures of bamboo joints and ripples corresponding to these two temperatures, respectively. It is believed that besides ion sputtering effect, the chemical bonding configurations in the amorphous carbon films should be taken into considerations for elucidating the surface evolutions.     

Surface and interface investigation of aluminosilicate biomaterial by the “in vivo” experiments

Porous mixtures of aluminosilicate/calcium phosphate have been studied for biomaterials applications. Aluminosilicates formed with an inorganic polymeric constitution present amorphous zeolites because of their 3D network structure and present the ability to link to bone matrix. Amorphous geopolymers of the potassium-poly(sialate)-nanopolymer type were synthesised at low temperature and studied for their use as potential biomaterials. They were mixed with 13% weight of calcium phosphate like biphasic hydroxyapatite and β-tricalcium phosphate. In this study, “in vivo” experiments were monitored to evaluate the biocompatibility, the surface and the interface behaviour of these composites when used as bone implants. Moreover, it has been demonstrated using histological and physicochemical studies that the developed materials exhibited a remarkable bone bonding when implanted in a rabbit's thighbone for a period of 1 month. The easy synthesis conditions (low temperature) of this composite and the fast intimate links with bone constitute an improvement of synthetic bone graft biomaterial.     

Cell adhesive ability of a biological foam ceramic with surface modification

Biological foam ceramic is a promising material for tissue engineering scaffold because of its biocompatibility, biodegradation and adequate pores measured from micrometer to nanometers. The aim of this study was to evaluate the adhesion and proliferation of adipose-derived stromal cells (ADSCs) on the biological foam ceramic coated with fibronectin. ADSCs were harvested from SD rats and passaged three times prior to seeding onto biological foam surface modified with fibronectin (50 μg/ml). Scaffold without surface modification served as control. To characterize cellular attachment, cells were incubated on the scaffold for 1 h and 3 h and then the cells attached onto the scaffold were counted. The difference of proliferation was appraised using MTT assay at day 1, 3, 5 and 7 before the cells reached confluence. After 7 days of culture, scanning electron microscope (SEM) was chosen to assess cell morphology and attachment of ADSCs on the biological foam ceramic. Attachment of ADSCs on the biological foam ceramic surface modified with fibronectin at 1 h or 3 h was substantially greater than that in control. MTT assay revealed that ADSCs proliferation tendency of the experimental group was nearly parallel to that of control. SEM view showed that ADSCs in the experimental groups connected more tightly and excreted more collagen than that in control. The coating of fibronectin could improve the cell adhesive ability of biological foam ceramics without evident effect on proliferation.     

Preparation and characterizations of SiO2/TiO2/γ-glycidoxypropyltrimethoxysilane composite materials for optical waveguides

SiO₂/TiO₂/γ-glycidoxypropyltrimethoxysilane composite materials processed by the sol-gel technique were studied for optical waveguide applications. Waveguide films with thickness more than 1.7 μm were prepared on a silicon substrate by a single-coating process and low-temperature heat treatment from these high-titanium-content composite materials. Scanning electron microscopy (SEM), atomic force microscopy (AFM), thermal gravimetric analysis (TGA), UV-visible spectroscopy (UV-VIS), Fourier-transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS) have been used to characterize the waveguide films. TGA curves showed that organic compounds in the composite materials would decompose in the temperature range from 200 °C to 480 °C. SEM, AFM and UV-VIS results showed that a dense, porous-free, and high transparency in the visible range waveguide film could be obtained at a low heat-treatment temperature. It was also noted that the carbon content in the film with higher titanium content heated at high temperature was evidenced by XPS. The waveguide propagation loss properties of the composite material films were also investigated and showed a dependence on the titanium molar fraction. Received: 13 June 2000 / Accepted: 21 June 2000 / Published online: 20 September 2000     

Dislocation evolution in titanium during surface severe plastic deformation

Surface mechanical attrition treatment (SMAT) is an innovative technique which can produce nanocrystalline (nc) layers of several tens of micrometers thickness on surfaces of metallic materials. In this work, the grade structures of commercially pure titanium (CP Ti) processed by SMAT was studied intensively, and the microstructure observations indicated that the dislocation evolution could be separated into three steps: (1) formation of dislocation tangles; (2) formation of dislocation bands; and (3) dynamic recrystallization of dislocation bands until the formation of nc Ti.     

Influence of surface morphology of cpTi on the adsorption and attachment of collagen/chitosan

The surface microtopography of implant influences distinctly the rate of bone-formation and the ratio of bone-implant contact. However, it is indicated that the surface of titanium implant existed contamination after different surface treatments. Chitosan is one of the most abundant natural polymers for its adsorption property for metal ions. In this study, we report on the pretreatment of the metal surface and aim to compare the efficacy of three treatments for the binding ability of collagen/chitosan (CL/CS). The compound of collagen and chitosan was immobilized on the titanium oxide and the morphology and chemical composition were used to characterize the titanium surfaces by scanning electron microscope (SEM), X-ray photoelectron spectrometry (XPS). The result showed that the surface displayed irregularities after roughness treatments and the rough surface was beneficial to the adsorption and attachment of CL/CS. The combination of CL/CS was related with the titanium surface character.     

Modified titanium surface with gelatin nano gold composite increases osteoblast cell biocompatibility

This study examined the gelatin nano gold (GnG) composite for surface modification of titanium in addition to insure biocompatibility on dental implants or biomaterials. The GnG composite was constructed by gelatin and hydrogen tetrachloroaurate in presence of reducing agent, sodium borohydrate (NabH₄). The GnG composite was confirmed by UV-VIS spectroscopy and transmission electron microscopy (TEM). A dipping method was used to modify the titanium surface by GnG composite. Surface was characterized by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX). The MC-3T3 E1 cell viability was assessed by trypan blue and the expression of proteins to biocompatibility were analyzed by Western blotting. The GnG composite showed well dispersed character, the strong absorption at 530 nm, roughness, regular crystal and clear C, Na, Cl, P, and Au signals onto titanium. Further, this composite allowed MC-3T3 E1 growth and viability compared to gelatin and pure titanium. It induced ERK activation and the expression of cell adherent molecules, FAK and SPARC, and growth factor, VEGF. However, GnG decreased the level of SAPK/JNK. This shows that GnG composite coated titanium surfaces have a good biocompatibility for osteoblast growth and attachment than in intact by simple and versatile dipping method. Furthermore, it offers good communication between cell and implant surfaces by regulating cell signaling and adherent molecules, which are useful to enhance the biocompatibility of titanium surfaces.     

Protein adsorption resistant surface on polymer composite based on 2D- and 3D-controlled grafting of phospholipid moieties

To prepare the biocompatible surface, a phosphorylcholine (PC) group was introduced on this hydroxyl group generated by surface hydrolysis on the polymer composite composed of polyethylene (PE) and poly (vinyl acetate) (PVAc) prepared by supercritical carbon dioxide. Two different procedures such as two-dimensional (2D) modification and three-dimensional (3D) modification were applied to obtain the steady biocompatible surface. 2D modification was that PC groups were directly anchored on the surface of the polymer composite. 3D modification was that phospholipid polymer was grafted from the surface of the polymer composite by surface-initiated atom transfer radical polymerization (SI-ATRP) of 2-methacryloyloxyethyl phosphorylcholine (MPC). The surfaces were characterized by X-ray photoelectron spectroscopy, dynamic water contact angle measurements, and atomic force microscope. The effects of the poly(MPC) chain length on the protein adsorption resistivity were investigated. The protein adsorption on the polymer composite surface with PC groups modified by 2D or 3D modification was significantly reduced as compared with that on the unmodified PE. Further, the amount of protein adsorbed on the 3D modified surface that is poly(MPC)-grafted surface decreased with an increase in the chain length of the poly(MPC). The surface with an arbitrary structure and the characteristic can be constructed by using 2D and 3D modification. We conclude that the polymer composites of PE/PVAc with PC groups on the surface are useful for fabricating biomedical devices due to their good mechanical and surface properties.     

Chitosan magnetic microspheres for technological applications: Preparation and characterization

One of the major applications of chitosan and its many derivatives are based on its ability to bind strongly heavy and toxic metal ions. In this study chitosan magnetic microspheres have been synthesized. Acetic acid (1%w/v) solution was used as solvent for the chitosan polymer solution (2%w/v) where magnetite nanoparticles were suspended in order to obtain a stable ferrofluid. Glutaraldehyde was used as cross-linker. The magnetic characteristic of these materials allows an easy removal after use if is necessary. The morphological characterization of the microspheres shows that they can be produced in the size range 800–1100 μm.The adsorption of Cu(II) onto chitosan–magnetite nanoparticles was studied in batch system. A second-order kinetic model was used to fit the kinetic data, leading to an equilibrium adsorption capacity of 19 mg Cu/g chitosan.     

Copper adsorption on magnetite-loaded chitosan microspheres: A kinetic and equilibrium study

A composite of Fe₃O₄ nanoparticles and the biopolymer chitosan, chemically crosslinked, was prepared as microspheres and used to adsorb copper ions, which were chosen as a model of contaminant metal in water.     

Preparation of magnetic composite microspheres by surfactant free controlled radical polymerization: Preparation and characteristics

Submicron magnetic composite microspheres have been prepared by a new surfactant free controlled radical polymerization. This new approach is based on the use of diphenylethene (DPE) as radical controlling agent and no emulsifier is required. X-ray powder diffraction (XRD), thermogravimetric analysis (TGA) and transmission electron microscopy (TEM), etc. were conducted to characterize the magnetite particles and magnetic composite microspheres. The average size of the magnetic composite microspheres prepared by this new approach is 265 nm and the magnetite content of the composite microspheres is around 20%. Furthermore, the magnetic composite microspheres which surfaces have epoxy groups were also prepared.     

Polishing behavior of PS/CeO2 hybrid microspheres with controlled shell thickness on silicon dioxide CMP

Organic-inorganic composite microspheres with PS as a core and CeO₂ nanoparticles as a shell were synthesized by in situ decomposition reaction of Ce(NO₃)₃ on the surfaces of PS microspheres prepared through soap-free emulsion polymerization. The shell thickness of the composite microspheres could be turned by varying the concentration of Ce(NO₃)₃ in the reaction solution. The whole process required neither surface treatment for PS microspheres nor additional surfactant or stabilizer. The as-synthesized PS/CeO₂ composite microsphere samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Oxide chemical mechanical polishing (CMP) performance of the PS/CeO₂ composite abrasives with different shell thickness was characterized by atomic force microscopy (AFM). The results indicated that the as-prepared core-shell structured composite microspheres (220-260 nm in diameter) possessed thin shell (10-30 nm) composed of CeO₂ nanoparticles (particle diameter of 5-10 nm), and the final CeO₂ contents of the composite microspheres ranged from 10 to 50 wt%. A possible mechanism for the formation of PS/CeO₂ composite microspheres was discussed also. The CMP test results confirmed that the novel core-shell structured composite abrasives are useful to improve oxide CMP performance. In addition, there is an obvious effect of shell thickness of the composite abrasives on oxide CMP performance.     

The morphologies of fractured surfaces and fracture toughness in some As-Se-Sb-S-I glasses

As part of a general physical characterization of amorphous materials in the pseudobinary system (As₂Se₃)_100−x(SbSI)_x type, their indentation fracture toughness was determined. It is a system with the variable ratio of classical amorphous compound As₂Se₃ and the molecule of antimony sulfoiodide, SbSI, which in the monocrystal form is characterized as ferroelectrics. Because of chalcogenides are generally very brittle and under load they crack very easily, these glasses have been studied with the aim of examining the possibility of obtaining some new structures on the basis of the materials with amorphous internal network, the structures that will have a higher quality in respect of mechanical properties. The morphologies of fractured surfaces were investigated by scanning electron microscope.     

Immobilization of silver nanoparticles on silica microspheres

The silver nanoparticles (Ag NPs) have been immobilized onto silica microspheres through the adsorption and subsequent reduction of Ag⁺ ions on the surfaces of the silica microspheres. The neat silica microspheres that acted as the core materials were prepared through sol–gel processing; their surfaces were then functionalized using 3-mercaptopropyltrimethoxysilane (MPTMS). The major aims of this study were to immobilize differently sized Ag particles onto the silica microspheres and to understand the mechanism of formation of the Ag nano-coatings through the self-assembly/adsorption behavior of Ag NPs/Ag⁺ ions on the silica spheres. The obtained Ag NP/silica microsphere conglomerates were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and energy-dispersive spectroscopy (EDS). Their electromagnetic wave shielding effectiveness were also tested and studied. The average particle size of the obtained Ag NPs on the silica microsphere was found that could be controllable (from 2.9 to 51.5 nm) by adjusting the ratio of MPTMS/TEOS and the amount of AgNO₃.