X-PEEM/NEXAFS and AFM of polypyrrole and copper micro-patterns on insulating fluoropolymer substrates

Micro-patterns (80 μm and 10 μm) of copper and semi-conducting polypyrrole on insulating fluorinated ethylene propylene substrates were characterized using synchrotron-based X-ray Photoemission Electron Microscopy (X-PEEM), Near Edge X-ray Absorption Fine Structure (NEXAFS), and Atomic Force Microscopy (AFM). Electronic states in the polypyrrole are verified using the NEXAFS data, and sample degradation upon irradiation is addressed. X-PEEM images show homogeneous distributions of the corresponding elements in the patterns. They do not exhibit dichroic effects and give information about the growth of copper and polypyrrole (i.e. nucleation of Cu, overgrowth of PPy, formation of PPy granules). AFM results are used to verify the topography of the patterns and support the findings on pattern growth.     

Comparative study of electroless copper deposition based on the seed layers of Pd, PtPd and AuPd

The article reports on electroless deposition of copper films onto p-silicon (1 0 0) using different seed (co-seed) layers of Pd, PtPd and AuPd. The dependence of the compositions and morphologies of different seed layers on resultant Cu films were comparatively studied in detail by atomic force microscopy (AFM), field emission scanning electron microscope (FE-SEM) and X-ray photoelectron spectroscopy (XPS). The activities of electroless copper deposition on the p-silicon (1 0 0) with different seed (co-seed) layers were evaluated by polarization curve. It is concluded that the bimetallic AuPd seed displayed the highest catalytic activity for electroless copper deposition, and followed by the order of PtPd > Pd.     

The effects of powder properties on in-flight particle velocity and deposition process during low pressure cold spray process

In cold spray process, impacting velocity and critical velocity of particles dominate the deposition process and coating properties for given materials. The impacting velocity and critical velocity of particles depend on the powder properties and cold spray conditions. In the present study, the in-flight particle velocity of copper powder in low pressure cold spraying was measured using an imaging technique. The effects of particle size and particle morphology on in-flight particle velocity and deposition efficiency were investigated. The critical velocity of copper powder was estimated by combining the in-flight particle velocity and deposition efficiency. The effect of annealing of feedstock powder on deposition and critical velocity was also investigated. The results showed that the irregular shape particle presents higher in-flight velocity than the spherical shape particle under the same condition. For irregular shape particles, the in-flight velocity decreased from 390 to 282 m/s as the particle size increases from 20 to 60 μm. Critical velocities of about 425 m/s and more than 550 m/s were estimated for the feedstock copper powder with spherical and irregular shape morphology, respectively. For the irregular shape particles, the critical velocity decreased from more than 550 to 460 m/s after preheating at 390 °C for 1 h. It was also found that the larger size powder presents a lower critical velocity in this study.     

Enhanced diamond nucleation on copper substrates by graphite seeding and CO2 laser irradiation

Diamond nucleation on copper (Cu) substrates was investigated by graphite seeding and CO₂ laser irradiation at initial stages of the combustion-flame deposition. A graphite aerosol spray was used to generate a thin layer of graphite powders (less than 1 μm) on Cu substrates. The graphite-seeded Cu substrates were then heated by a continuous CO₂ laser to about 750 °C within 1 min. It was found that diamond nucleation density after this treatment was more than three times as much as that on the virgin Cu substrates. As a consequence, diamond films up to 4 μm were obtained in 5 min. The enhancement of diamond nucleation on the graphite-seeded Cu substrates was attributed to the formation of defects and edges during the etching of the seeding graphite layers by the OH radicals in the flame. The defects and edges served as nucleation sites for diamond formation. The function of the CO₂ laser was to rapidly heat the deposition areas to create a favorable temperature for diamond nucleation and growth.     

Improvement of copper plating adhesion on silane modified PET film by ultrasonic-assisted electroless deposition

Copper thin film on silane modified poly(ethylene terephthalate) (PET) substrate was fabricated by ultrasonic-assisted electroless deposition. The composition and topography of copper plating PET films were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and atomic force microscopy (AFM), respectively. Peel adhesion strength, as high as 16.7 N/cm, was achieved for the planting copper layer to the modified PET substrate with ultrasonic-assisted deposition; however, a relative low value as 11.9 N/cm was obtained for the sample without ultrasonic vibration by the same measurement. The electrical conductivity of Cu film was changed from 7.9 × 10⁴ to 2.1 × 10⁵ S/cm by using ultrasonic technique. Ultrasonic operation has the significant merits of fast deposition and formation of good membranes for electroless deposition of Cu on PET film.     

Microstructure and properties of manganese dioxide films prepared by electrodeposition

Nanostructured manganese dioxide films were obtained by galvanostatic, pulse and reverse pulse electrodeposition from 0.01 to 0.1 M KMnO₄ solutions. The deposition yield was investigated by in situ monitoring the deposit mass using a quartz crystal microbalance (QCM). Obtained films were studied by electron microscopy, X-ray diffraction analysis, energy dispersive spectroscopy, thermogravimetric and differential thermal analysis. The QCM and electron microscopy data were utilized for the investigation of deposition kinetics and film formation mechanism. It was shown that the deposition rate and film microstructure could be changed by variation of deposition conditions. The method allowed the fabrication of dense or porous films. The thickness of dense films was limited to ∼0.1 μm due to the insulating properties of manganese dioxide and film cracking, attributed to drying shrinkage. Porous and crack-free 1-2 μm films were obtained using galvanostatic or reverse pulse deposition from 0.02 M KMnO₄ solutions. It was shown that film porosity is beneficial for the charge transfer during deposition and crack prevention in thick films. Moreover, porous nanostructured films showed good capacitive behavior for applications in electrochemical supercapacitors. The porous nanostructured films prepared in the reverse pulse regime showed higher specific capacitance (SC) compared to the SC of the galvanostatic films. The highest SC of 279 F/g in a voltage window of 1 V was obtained in 0.1 M Na₂SO₄ solutions at a scan rate of 2 mV/s.     

Study of deposition patterns of plating layers in SiC/Cu composites by electro-brush plating

SiC reinforced copper composite coatings were prepared by electro-brush plating with micron-size silicon carbide (SiC) ranging from 1 to 5 μm on pure copper sheet in this paper. The micro-structural characterizations of SiC/Cu composite coatings were performed by optical microscope and Scanning Electron Microscope (SEM) coupled with spectrometer, to study co-deposition mechanism of SiC/Cu. It was found that there were three different patterns of SiC deposition in plating layers during electro-brush plating process, i.e. the particles could deposit inside copper grains, in grain boundaries, or in holes of the surface. To investigate deposition mechanism of each pattern, size of SiC and copper grains was compared. By comparison of size of copper grains and hard particles, SiC were either wrapped in copper grains or deposited in grain boundaries. Moreover, electro-brush plating layers at different brush velocities and current densities were obtained respectively, to analyze the microstructure evolution of the composite coatings. The hardness of plating layers was measured. The results indicated at the current density of 3 A/dm², the SiC/Cu coating was compact with SiC content at a high level and the hardness reached a maximum.     

Laser-induced site-selective silver seeding on polyimide for electroless copper plating

Ag particles were generated on Ag⁺-doped polyimide film by laser direct writing, followed by selective copper deposition using the metallic silver particles as seeds. Laser irradiation caused in situ reduction and agglomeration of silver on the polyimide film. The copper lines were less uniform and compact with higher scanning velocity and the width of the deposited copper line could reach 25 μm. Equations of the relationship between scanning velocity and connectivity of the deposited copper patterns have been derived. The process was characterised by AFM, XPS, SEM, and semiconductor characterisation system.     

Synthesis of intrinsic fluorescent polypyrrole nanoparticles by atmospheric pressure plasma polymerization

Intrinsic fluorescent polypyrrole (ppy) nanoparticles with different shapes were fabricated by atmospheric pressure plasma polymerization. Gradient electrical field and polarization of active particles in the plasma induce change of shape of nanoparticles from spherical to rod, when the plasma power varied from 5 W to 10 W. Both X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) results suggest that the atmospheric pressure plasma polymerization process (APPP) at the power of 5 W and 10 W can help to preserve the integrity of the structure of monomer due to the predominant role of radical polymerization in APPP at these powers. However, when the plasma power increased to 20 W, the ring structure of some pyrroles was destroyed, owing to existence of higher energy species. The polypyrrole nanoparticles exhibit the peak fluorescence around 415 nm. Fluorescent results show that the fluorescent properties of polypyrrole nanoparticles are related to the particle size of the polymer. The bigger particles would have more enlarged room for exciton diffusion, resulting in lower fluorescence intensity and red shift of the fluorescent peak.     

Evolution of magnetic and microstructural properties of thick sputtered NdFeB films with processing temperature

Ta (100 nm)/NdFeB (5 μm)/Ta (100 nm) films have been deposited onto Si substrates using triode sputtering (deposition rate ∼18 μm/h). A 2-step procedure was used: deposition at temperatures up to 400 °C followed by ex-situ annealing at higher temperatures. Post-deposition annealing temperatures above 650 °C are needed to develop high values of coercivity. The duration of the annealing time is more critical in anisotropic samples deposited onto heated substrates than in isotropic samples deposited at lower temperatures. For a given set of annealing conditions (750 °C/10′), high heating rates (?2000 °C/h) favour high coercivity in both isotropic and anisotropic films. The shape and size of Nd₂Fe₁₄B grains depend strongly on the heating rate.     

Direct writing of carbon nanotube patterns by laser-induced chemical vapor deposition on a transparent substrate

Dot array and line patterns of multi-walled carbon nanotubes (MWCNTs) were successfully grown by laser-induced chemical vapor deposition (LCVD) on a transparent substrate at room temperature. In the proposed technique, a Nd:YVO₄ laser with a wavelength of 532 nm irradiates the backside of multiple catalyst layers (Ni/Al/Cr) through a transparent substrate to induce a local temperature rise, thereby allowing the direct writing of dense dot and line patterns of MWCNTs below 10 μm in size to be produced with uniform density on the controlled positions. In this LCVD method, a multiple-catalyst-layer with a Cr thermal layer is the central component for enabling the growth of dense MWCNTs with good spatial resolution.     

Synthesis process of nanowired Al/CuO thermite

Al/CuO nanothermites were fabricated by thermal oxidation of copper layer at 450 °C for 5 h and by aluminum thermal evaporation: thermal evaporation allows producing thin layer less than 2 μm in size. The copper has been deposited by electroplating or thermal evaporation depending on the required thickness. The obtained diameter of Al/CuO nanowires is 150-250 nm. Al/CuO nanowires composite were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and differential thermal analysis (DTA). Two distinct exothermic reactions occurred at 515 and 667 °C and total energy release of this thermite is 10 kJ/cm³.     

Van der Pauw resistivity measurements on evaporated thin films of cadmium arsenide, Cd3As2

Cadmium arsenide is a II-V semiconductor, exhibiting n-type intrinsic conductivity with high mobility and narrow bandgap. It is deposited by thermal evaporation, and has shown the Schottky and Poole-Frenkel effects at high electric fields, but requires further electrical characterisation. This has now been extended to low-field van der Pauw lateral resistivity measurements on films of thickness up to 1.5 μm. Resistivity was observed to decrease with increasing film thickness up to 0.5 μm from about 3 × 10⁻³ Ω m to 10⁻⁵ Ω m, where the crystalline granular size increases with film thickness. This decrease in resistivity was attributed to a decrease in grain boundary scattering and increased mobility. Substrate temperature during deposition also influenced the resistivity, which decreased from around 10⁻⁴ Ω m to (10⁻⁵ to 10⁻⁶) Ω m for an increase in substrate deposition temperature from 300 K to 423 K. This behaviour appears to result from varying grain sizes and ratios of crystalline to amorphous material. Resistivity decreased with deposition rate, reaching a minimum value at about 1.5 nm s⁻¹, before slowly increasing again at higher rates. It was concluded that this resulted from a dependence of the film stoichiometry on deposition rate. The dependence of resistivity on temperature indicates that intercrystalline barriers dominate the conductivity at higher temperatures, with a hopping conduction process at low temperatures.     

Efficient field emission from coiled carbon nano/microfiber on copper substrate by dc-PECVD

Crystalline coiled carbon nano/micro fibers in thin film form have been synthesized via direct current plasma enhanced chemical vapor deposition (PECVD) on copper substrates with acetylene as a carbon precursor at 10 mbar pressure and 750 °C substrate temperature. The as-prepared samples were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). XRD pattern as well as selected area electron diffraction (SAED) pattern showed that the samples were crystalline in nature. SEM and HRTEM studies showed that as synthesized coiled carbon fibers are having average diameter ∼100 nm and are several micrometers in length. The as-prepared samples showed moderately good electron field emission properties with a turn-on field as low as 1.96 V/μm for an inter-electrode distance 220 μm. The variation of field emission properties with inter-electrode distance has been studied in detail. The field emission properties of the coiled carbon fibrous thin films are compared with that of crystalline multiwalled carbon nanotubes and other carbon nanostructures.     

Characterization of diamond films deposited on Re substrate by magnetic field-assisted hot filament chemical vapor deposition

A periodically magnetic field (PMF) was used in a hot-filament chemical vapor deposited (HFCVD) for diamond growth on the rhenium substrate. The morphology, band structures and crystalline structure of the film were analyzed by the scanning electron microscopy (SEM), Raman spectroscopy and X-ray diffractometer (XRD), respectively. The results show that the thickness of the diamond film is about 2900 nm by 4 h deposition with magnetic field-assisted. There is no interlayer between diamond film and the rhenium substrate. The result shows that the turn on voltage of the sample is enhanced from 3.3 to 2.6 V/μm with the PMF. Also the total emission current density at 6.2 V/μm increased from 6.3 to 21.5 μA/cm².     

Relationship between particle size and deformation in the cold spray process

The flattening of aluminum and copper particles cold sprayed onto ceramic surfaces has been described by an ellipsoidal function. The accuracy of this approximation was verified from particle dissections performed in a focused ion beam/scanning electron microscope (FIB/SEM). Flattening data were collected from SEM measurements. It was shown that aluminum particle deformation was limited below ∼5 μm, and copper deformation below ∼2 μm. Deceleration of the particles through the bow shock, strain rate hardening and thermal conduction were factors that contributed to the differences in deformation behaviour.     

Evolution of magnetic permeability and magneto-impedance effect in composite wires with insulator layer

CuBe/Insulator/NiCoP composite wire was prepared by electroless deposition on an insulated CuBe core with a diameter of 90 μm. The conversion relationship between the magneto-impedance and effective magnetic permeability of the composite wire was derived from an energy conversion model. The evolution of the magnetic permeability and the giant magneto-impedance (GMI) effect were investigated. The results show that a distinct GMI effect can be obtained at relatively low frequency. The largest GMI ratio is 240% at 600 kHz, and the maximal field sensitivity is 34%/Oe.     

Field emission properties of polymer-converted carbon films by heat treatment

Carbon films were prepared on single crystal silicon substrates by heat-treatment of a polymer-poly(phenylcarbyne) at 800 °C in Ar atmosphere. The heat-treatment caused the change of the polymer into carbon film, which exhibited good field emission properties. Low turn-on emission field of 4.3 V/μm (at 0.1 μA/cm²) and high emission current density of 250 μA/cm² (at 10 V/μm) were observed for the polymer-converted carbon films. This behavior was demonstrated to be mainly related to the microstructure of the carbon films, which consisted of fine carbon nanoparticles with high sp² bonding. The carbon films, which can be deposited simply with large areas, are promising for practical applications in field emission display.     

1.54 μm emission mechanism of Er-doped zinc oxide thin films

Zinc oxide (ZnO) and Er-doped zinc oxide (ZnO:Er) thin films were formed by pulsed laser deposition, and characterized by photoluminescence (PL) and X-ray diffraction (XRD) in order to clarify the 1.54 μm emission mechanism in the ZnO:Er films. Er ions were excited indirectly by the 325 nm line of a He-Cd laser, and the comparison of the ultraviolet to infrared PL data of ZnO and ZnO:Er films showed that the 1.54 μm emission of Er³⁺ in ZnO:Er film appears at the expense of the band edge emission and the defect emission of ZnO. The crystallinity of the films was varied with the substrate temperature and post-annealing, and it was found that the intensity of the 1.54 μm emission is strongly related with the crystallinity of the films. There are three processes leading to the 1.54 μm emission; absorption of excitation energy by the ZnO host, energy transfer from ZnO to Er ions, and radiative relaxation inside Er ions, and it is suggested that the crystallinity plays an important role in the first two processes.     

Conducting polymer film-based immunosensors using carbon nanotube/antibodies doped polypyrrole

Carbon nanotube/polypyrrole/antibodies polymer films were synthesized successfully on microelectrodes by electrochemical deposition. Electropolymerization was performed at optimal range between −0.8 and +0.8 V at a scan rate of 50 mV s⁻¹ in an electrochemical mini-cell containing monomer pyrroles, carbon nanotubes, and goat IgGs. The conducting polymer films were characterized by Fourier transform infrared spectrometry, Raman spectra, and Field emission scanning electron microscopy. And then, it was prepared for immunosensor application to determine anti-goat IgGs. The results show that a linear range between 0.05 and 0.7 μg ml⁻¹ for anti-goat IgGs detection was observed for immunosensor, a detection limit as low as 0.05 μg ml⁻¹ and a response time of 1 min. The effect parameters of electropolymerization process on immunosensor response are also studied. It found that the immunosensor well active in 1.5 mg ml⁻¹ CNT concentration, 2.5 mM pyrrole, 10 μg ml⁻¹ goat IgGs.