Chitosan nanoparticles with controlled size and zeta potential

Optimization of chitosan nanoparticles (ChNs) production process employing a 2^(5–2) fractional factorial design was performed to analyze the influence of viscosity average molecular weight (40–120 kDa), the initial concentration of chitosan (2–5 g/L), the initial tripolyphosphate (TPP) concentration (0.8–1.2 g/L), the ratio chitosan/TPP (4/1–10/1) (V/V), and the stirring speed (300–700 rpm), on final nanoparticles size and zeta potential. The measured responses of average particle size and surface charge were determined on Zetasizer Nano ZS. ChNs were prepared using ionotropic cross-linking of chitosan and TPP and were characterized by Fourier-transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), and differential scanning calorimetry (DSC). The experiments showed that the size of synthesized nanoparticles depended on initial concentration and molecular weight of chitosan, TPP concentration and stirring speed within the chosen levels. However, the zeta potential was significantly influenced by chitosan molecular weight, chitosan concentration and stirring speed. The FTIR analysis confirmed the interaction between negative charge of TPP with positive charge of chitosan through the appearance of new peaks at 1222 and 895 cm⁻¹ in produced ChNs. XRD and DSC analysis were used to evaluate the effect of crosslinking of chitosan on crystal structure of ChNs.     

类金刚石薄膜在人工关节摩擦副表面改性进展

类金刚石（DLC）薄膜由于其优异的减摩耐磨性以及良好的生物相容性被引入到人工关节材质中。该文综述了DLC薄膜在人工关节摩擦副表面改性的研究现状,包括DLC薄膜的分类和制备方法。尽管该薄膜已被研究数十年,但在人体复杂的生理力学环境中高负荷摩擦腐蚀等综合作用下,仍存在高内应力导致结合力不足,从而限制其在人工关节领域的应用。该文介绍了降低DLC薄膜内应力提高膜基结合力的方法和DLC薄膜生物相容性的研究进展。最后,对不同DLC薄膜人工关节摩擦副的研究进展进行了阐述。根据该综述,提出厚的无氢DLC涂层（高sp3含量）,且在两个滑动表面上均有DLC薄膜的人工关节副具有优异的耐磨性,对于承重植入体应用至关重要。     

Diamond-like carbon thin films by microwave surface-wave plasma CVD aimed for the application of photovoltaic solar cells

The nitrogen doped diamond-like carbon (DLC) thin films were deposited on quartz and silicon substrates by a newly developed microwave surface-wave plasma chemical vapor deposition, aiming the application of the films for photovoltaic solar cells. For film deposition, we used argon as carrier gas, nitrogen as dopant and hydrocarbon source gases, such as camphor (C₁₀H₁₆O) dissolved with ethyl alcohol (C₂H₅OH), methane (CH₄), ethylene (C₂H₄) and acetylene (C₂H₂). The optical and electrical properties of the films were studied using X-ray photoelectron spectroscopy, Nanopics 2100/NPX200 surface profiler, UV/VIS/NIR spectroscopy, atomic force microscope, electrical conductivity and solar simulator measurements. The optical band gap of the films has been lowered from 3.1 to 2.4 eV by nitrogen doping, and from 2.65 to 1.9 eV by experimenting with different hydrocarbon source gases. The nitrogen doped (flow rate: 5 sccm; atomic fraction: 5.16%) film shows semiconducting properties in dark (i.e. 8.1 × 10^{− 4} Ω^{− 1} cm^{− 1}) and under the light illumination (i.e. 9.9 × 10^{− 4} Ω^{− 1} cm^{− 1}). The surface morphology of the both undoped and nitrogen doped films are found to be very smooth (RMS roughness ≤ 0.5 nm). The preliminary investigation on photovoltaic properties of DLC (nitrogen doped)/p-Si structure show that open-circuit voltage of 223 mV and short-circuit current density of 8.3 × 10^{− 3} mA/cm². The power conversion efficiency and fill factor of this structure were found to be 3.6 × 10^{− 4}% and 17.9%, respectively. The use of DLC in photovoltaic solar cells is still in its infancy due to the complicated microstructure of carbon bondings, high defect density, low photoconductivity and difficulties in controlling conduction type. Our research work is in progress to realize cheap, reasonably high efficiency and environmental friendly DLC-based photovoltaic solar cells in the future.     

Diamond-like carbon coating of alternative metal alloys for medical and surgical applications

The effectiveness of a plasma-deposited, diamond-like carbon (DLC) coating on aluminium alloy based surgical instruments is investigated. Surgical instruments must satisfy a number of important criteria including biocompatibility, functional performance, sterility and cleanability, structural integrity, and fatigue resistance. The integrity of the DLC layer and the diffusion barrier properties are of paramount importance due to biocompatibility considerations of the underlying aluminium metal. We investigate the optimisation of the coating with incorporation of silicon and variation in negative self bias, and highlight the design and manufacture of a lightweight laparoscopic assist instrument from aluminium alloy coated with diamond-like carbon, which has been used successfully in the clinical environment to improve operations such as cholecystectomy (gall bladder removal) and exploratory techniques for the diagnosis of cancer.     

Fabrication of polyamide thin film nanocomposite reverse osmosis membrane incorporated with a novel graphite-based carbon material for desalination

The properties of polyamide (PA) thin film composite (TFC) membranes are affected by many variables, especially the additives in the process of interfacial polymerization that play an important role in the properties of membranes. In this study, a new type graphite carbon was added into organic phase containing trimesoyl chloride for interfacial polymerization with aqueous phase containing m-phenylenediamine to prepare modified polyamide thin film nanocomposite (TFN) membranes for reverse osmosis (RO) adhibition. Polysulfone ultrafiltration membranes were used as the carrier of the interfacial polymerization. The concentration of graphite carbon was selected from 0.002 to 0.01 wt%. The polyamide nanocomposite membrane prepared with the concentration of 0.004 wt% graphite carbon showed the best RO desalination performance, which the water flux of this TFN membrane is over 2.3 times as much as pristine TFC membrane, and the salt rejection is over 99%. This article provides a well-performing polyamide thin film nanocomposite membrane modified by a new-type carbon nanoparticles consequently.     

Diamond-like carbon thin films prepared by ECR argon plasma assisted pulsed laser deposition

Diamond-like carbon films were prepared by pulsed laser ablation of graphite target in argon plasma produced from electron cyclotron resonance (ECR) microwave discharge and analyzed by Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy. The analysis shows that the films prepared with argon plasma assistance have different chemical structure compared with the films prepared in vacuum without plasma assistance. The structure of the films prepared with plasma assistance depends strongly on the bias voltages applied on the substrate. Surface morphology observation shows that the films prepared with argon plasma assistance have a smoother surface than the films prepared without plasma assistance. The re-sputtering of the growing film due to the bombardment of the plasma stream results in reduction of the deposition rate. The ablation plumes during film preparation with and without plasma assistance were examined through optical emission spectroscopy. In vacuum, emission lines from mono-atomic carbons and carbon ions dominate the plume emission. In argon plasma, the plume emission exhibits different behavior in its temporal and spatial evolution. It is initially dominated by strong lines from mono-atomic carbons and carbon ions and then evolves to consist mainly of emissions from C₂ molecules superposed on a featureless continuum. It is also found that the emission intensity of the C₂ molecules as well as the continuum varies with the bias voltages.     

Particle size and zeta potential of carbon black in liquid media

Zeta potential is a parameter that can be used for studying and predicting colloid stability and surface morphology. Even though zeta potential measurements have been applied to both aqueous and non-aqueous suspensions, theories for colloidal behavior and zeta potential in non-aqueous media are not as well-established as those in aqueous environments. There are few reports on systematic studies of zeta potential of colloids in liquid media. In the present study, zeta potential and particle size measurements of two carbon black powder samples in various media were performed. Combined with particle size characterization, the experimental zeta potential values were used to discuss charge transfer and colloid stability of carbon black in suspension.     

SMA polymer thin film electrodeposition on carbon particles

Electrodeposition of styrene-co-maleic anhydride (SMA) polymer, as thin films on carbon particle substrates, was carried out in a fluidized electrode bed reactor (FEBR). Feeder current, time of deposition, flow rate of anolyte (i.e., bed expansion or bed porosity), concentration of SMA in the anolyte, and pH of the anolyte were the key parameters investigated. The film characteristics were evaluated through SEM and FTIR analyses, the amounts determined by weighing. The effect of these parameters on the electrodeposition process is discussed and optimum conditions for deposition are proposed. Also, a possible mechanism for electrodeposition, particularly for the SMA–carbon system, is discussed. Furthermore, where relevant, the parameters and mechanism are compared with those for our parallel work on the ethylene-co-acrylic acid (EAA)–carbon system.     

Surface grafting of polymer onto carbon thin film

The surface grafting of polymers onto carbon thin film deposited on a glass plate was achieved by two methods: the graft polymerization initiated by initiating groups introduced onto the surface; and the trapping of polymer radicals by surface aromatic rings of the thin film. It was found that the radical and cationic graft polymerization of vinyl monomers are initiated by azo and acylium perchlorate groups introduced onto the surface, respectively, and the corresponding polymers are grafted onto the surface: the surface grafting of polymers were confirmed by the contact angle of the surface with water. In addition, the anionic ring-opening alternating copolymerization of epoxides with cyclic acid anhydrides was found to be initiated by potassium carboxylate groups on the carbon thin film to give the corresponding polyester-grafted carbon thin film. On the other hand, polymer radicals formed by the decomposition of azo polymer, such as poly(polydimethylsiloxane-azobiscyanopentanoate) and poly(polyoxyethylene-azobiscyanopentanoate), were successfully trapped by the surface aromatic rings of carbon thin film and polydimethylsiloxane and polyoxyethylene were grafted onto the surface. © 1995 John Wiley & Sons, Inc.     

Perylene derivative sensitized multi-walled carbon nanotube thin film

Perylene-sensitized multi-walled carbon nanotubes (PV-MWNT) have been prepared by a π-stacking between nanotubes and perylene derivatives, N,N′-diphenyl glyoxaline-3,4,9,10-perylene tetracarboxylic acid diacidamide (PV). The resultant nanocomposites have been characterized by transmission electron microscope (TEM), UV-vis absorption, photoluminescence (PL) and photocurrent spectra. Long range ordering can be observed in the form of PV-MWNT via π-stacking by TEM. Red-shift in the optical spectra consisting of the UV-vis absorption and PL spectra with the attraction of PV on the surface of the MWNTs were observed. The evident quenching in PL spectra of PV-MWNT was ascribed to the absorption and transfer of recombination energy by MWNT. Photosensitivity spectra demonstrated an increasing photocurrent in the ultraviolet region and a broadening photosensitivity in the red spectral region for solar cells based on PV-MWNT.     

Bioactive glass nanoparticles with negative zeta potential

The purpose of this work was to produce and characterize SiO₂–CaO–P₂O₅ bioactive glass nanoparticles with negative zeta potential for possible use in biomedical applications. 63S bioactive glass was obtained using the sol–gel method. X-ray fluorescence (XRF) spectroscopy and dispersive X-ray analysis (EDX) confirmed the preparation of the 63S bioactive glass with 62.17% SiO₂, 28.47% CaO and 9.25% P₂O₅ (in molar percentage). The in vitro apatite forming ability of prepared bioactive glass was evaluated by Fourier transform infrared spectroscopy (FTIR) after immersion in simulated body fluid (SBF). The result showed that high crystalline hydroxyapatite can form on glass particles. By the gas adsorption (BET method), particle specific surface area and theoretical particle size were 223.6 ± 0.5 m²/g and ∼24 nm, respectively. Laser dynamic light scattering (DLS) indicated particles were mostly agglomerated and had an average diameter between 100 and 500 nm. Finally, using laser Doppler electrophoresis (LDE) the zeta potential of bioactive glass nanoparticles suspended in physiological saline was determined. The zeta potential was negative for acidic, neutral and basic pH values and was −16.18 ± 1.8 mV at pH 7.4. In summary, the sol–gel derived nanoparticles revealed in vitro bioactivity in SBF and had a negative zeta potential in physiological saline solution. This negative surface charge is due to the amount and kind of the ions in glass structure and according to the literature, promotes cell attachment and facilitates osteogenesis. The nanometric particle size, bioactivity and negative zeta potential make this material a possible candidate for bone tissue engineering.     

Diamond-like carbon film deposited on nitrided 316L stainless steel substrate: A hardness depth-profile modeling

Adhesion and hardness of Diamond-Like Carbon films are improved by nitriding of the steel substrate prior to PVD deposition. Since the mechanical properties of the nitrided steel layer are not homogeneous, i.e. a significant hardness decrease is observed in the upper nitrided layer close to the surface, an outer surface layer of ~ 15 μm is removed prior to the film deposition. In the present work, a 316L stainless steel substrate is nitrided in a cyanide-cyanate solution at 570 °C during 3 h. The coated system involved the deposition of a hydrogenated, amorphous carbon (a-C:H) solid lubricant of ~ 2 μm including a chromium carbide interlayer. The comparison between the hardness behavior of the DLC/steel and the DLC/nitrided steel systems reveals the existence of a very important hardness gap, which highlights the benefit of the nitriding treatment prior to coating deposition. In addition, the microhardness-depth profile is determined from a load-depth curve, by applying a simple hardness model. The predicted change in hardness is found to be in a very good agreement with the experimental profile, which allows the hardness determination both in the white layer and in the diffusion zone over ~ 30 μm in total depth. However, only the composite hardness modeling allows the accurate determination of the intrinsic hardness of the film.     

Vanadium nitride as a novel thin film anode material for rechargeable lithium batteries

Vanadium mononitride (VN) thin films have been successfully fabricated by magnetron sputtering. Its electrochemical behaviour with lithium was examined by galvanostatic cell cycling and cyclic voltammetry. The capacity of VN was found to be stable above 800 mAh g⁻¹ after 50 cycles. By using ex situ X-ray diffraction, high-resolution transmission electron microscopy and selected area electron diffraction as well as in situ spectroelectrochemical measurements, the electrochemical reaction mechanism of VN with lithium was investigated. The reversible conversion reaction of VN into metal V and Li₃N was revealed. The high reversible capacity and good stable cycle of VN thin film electrode made it a new promising lithium-ion storage material for future rechargeable lithium batteries.     

Nanostructures of pyrolytic carbon from a polyacetylene thin film

Pyrolysis of a polyacetylene thin film has been performed in order to carbonize at temperatures of 500 to 1000 °C in vacuum. A trans-polyacetylene thin film was synthesized using a Ziegler-Natta catalyst. A black char below 20% in weight of the original PA film remained after pyrolysis. Structural properties and morphology of the black chars were investigated using Raman scattering spectrum, X-ray diffraction measurements, and scanning and transmission electron microscopy. Dehydrogenation and carbonization of the PA film were almost finished at a pyrolysis temperature of 800 °C. However, hollow spherical or elliptical nano-particles of tens of nanometers in size, which are composed of graphite structure, were included in the black chars obtained at all pyrolysis temperatures in this work. The formation mechanism of a graphite crystal in nanometer size from a PA crystal was discussed.     

薄膜蒸发器干气密封的研制及应用

针对薄膜蒸发器运行工况,采用"气体阻塞"的干气密封替代传统机械密封,实现了机械密封对除盐水的零使用,通过循环水夹套冷却结构降低机封的运行温度,实现了干气密封的长周期运行。薄膜蒸发器干气密封的研制及应用对PTA装置搅拌器釜用机械密封具有重要的推广意义。     

Diamond-like two-phonon absorption in hydrogenated amorphous carbon modified with copper

Diamond nucleation in hydrogenated amorphous carbon films containing ultradispersed copper was monitored by the measurement of IR absorption at the diamond two-phonon frequencies. Anomalously high two-phonon absorption observed in this experiments allowed us to increase the sensitivity of the method. Mechanisms of the two-phonon absorption enhancement are discussed in terms of electrodynamics of media containing nanosize inclusions of copper-doped graphite fragments. Local fields induced by electromagnetic radiation in nanodiamonds in the vicinity of copper-doped graphite fragments were shown to be responsible for the observed amplification of two-phonon absorption.     

Evolution of a metastable thin film with high-hardness wear resistance for advanced cutting tool application

The structure and elastic properties of rocksalt and wurtzite Ti–Al–N ternary solid solutions were investigated using first principles calculations. We also performed an experimental evaluation using the sputtering method to obtain the reliability. The phase transition of (Ti_1−xAl_x)N solid solutions was occurred at x = 0.5–0.75 for both calculations and experimental results. The bulk modulus of rocksalt and wurtzite solid solutions decreases with increasing Al content. On the other hand, shear moduli and Young's moduli gradually increase with Al content only in rocksalt solid solutions. The theoretical and experimental results indicate that the overall mechanical properties of rocksalt solid solutions are superior to those of wurtzite solid solutions. Therefore, controlling the crystal structure of the Ti–Al–N ternary metastable system was crucial for optimizing the material properties.     

Length dependent performance of single-wall carbon nanotube thin film transistors

The effects of the length of single-wall carbon nanotubes (SWCNTs) on their thin film transistors (TFTs) were investigated by using SWCNTs sorted in length using size exclusion chromatography. Higher device performances were obtained in longer SWCNTs and it was found that the average length of the SWCNTs is an important factor to determine the device performance. Detailed analyses, in which the SWCNT density was normalized using percolation threshold, confirmed that the dependence of on-current on the normalized density approximately follows percolation theory, independently of the SWCNT length. On the other hand, the behaviors of off-current and on/off ratio showed the considerably different dependence among SWCNT lengths.     

Diamond-like carbon overcoat for TFMH using filtered cathodic arc system with Ar-assisted arc discharge

The deposition system described for sub-30 Å and thicker carbon (ta-C) overcoat that includes two RF ion beam guns and Filtered Cathodic Arc (FCA) module mounted on a single vacuum chamber. The system is capable of flattening the Thin Film Magnetic Heads (TFMH) surface by ion beam etching; smoothing scratches, trenches, steps on boundaries of different materials, and enhancing the adhesion by ion assisted ion beam sputtering. It provides the highly controllable deposition of carbon using an FCA module with Ar-assisted arc discharge. Low-level particulates are achieved on the deposited film surface (< 5/cm² ). It was shown that crucial impact on filtering the particles with size < 1 μm has the electrostatic field distribution across the plasma guide that can be controlled by duct bias. Mechanical and electrical properties, optical and Raman spectra of ta-C films were investigated as a function of Ar flow in the arc discharge area. At Ar flow rates 0–12 sccm, stress of the films was varied in a range 2.9–7.5 GPa while hardness and Young's Modulus stayed in ranges of 45–60 GPa, and 230–300 GPa, respectively. Density of the obtained films was greater than 2.8 g/cm³. Optical absorption and electrical conductivity of ta-C films showed a significant rise while stress came down with Ar flow. Raman G-peak was higher for ta-C films with lower stress and shifted to lower energy. The low stress films versus high stress films showed a few orders reduced electrical resistance and anisotropy of specific resistance with respect to substrate plane: ρ_⊥ ≫ ρ_∥. In situ ellipsometric control of growing film thickness was implemented on the system. Run-to-run standard deviation was less than 1 Å for 20–25 Å thick films. High corrosion resistance of FCA coatings was exhibited. The impact of Ar gas–carbon plasma interaction on the deposition conditions and microstructure of ta-C films was discussed.     

Diamond-like carbon films with End-Hall ion source enhanced chemical vapour deposition

A custom-designed End-Hall ion source was used to deposit diamond-like carbon (DLC) films in a plasma enhanced chemical vapour deposition (PECVD) mode. The deposition system was characterised and optimised for infrared transmission enhancement applications and large area deposition onto silicon or germanium substrates. Ion bombardment energy (in eV) on substrate was found to scale about 60% of the discharge voltage. Uniformity was about 2.5% and 5% for substrate diameters of 20 cm and 40 cm respectively. For the infrared enhancement applications the optimised ion bombardment energy was about 54 eV with a high deposition rate approximate 30 nm/min. Coating the DLC onto a single side of double-sided polished silicon wafers resulted in a transmission of 69.5% in the wavelength of about 4 μm, very close to the ideal value. Mechanical and reliability properties of the DLC films on silicon wafers were analysed at different environmental conditions. It was found that the DLC films produced in the ion source PECVD deposition system were satisfied with the requirements for the infrared transmission enhancement applications.