Modulated pulse power sputtered chromium coatings

Cr coatings were deposited using continuous dc magnetron sputtering (dcMS) and modulated pulse power sputtering (MPP) techniques in a closed field unbalanced magnetron sputtering system at equivalent average target powers. It was found that MPP sputtering exhibited higher deposition rates than in dcMS when the average target power density was above 14 W cm^− 2 for the Cr coating depositions. Plasma diagnostics confirmed a significant increase in the numbers of both target material (Cr) and gas (Ar) ions in the MPP plasma as compared to the dc plasma. The substrate peak current densities measured in the MPP depositions (104-324 mA cm^− 2) have been increased by over a factor of 50 to those in the dcMS conditions (2-5.5 mA cm^− 2). The enhanced ion flux bombardment from the highly ionized MPP plasma led to the formation of denser microstructure and finer grain size in the MPP Cr coatings than in the dcMS Cr coatings. In addition, MPP sputtered Cr coatings exhibited improved hardness and adhesion.     

Magnetron sputtering modes during pulsed deposition process determined by the analysis of power supply parameter

The goal of this paper is to present a new control method of reactive magnetron sputtering. The processes of reactive magnetron sputtering of aluminum target in Ar + O₂ atmosphere in high efficiency deposition and low efficiency deposition mode were studied. The mode of magnetron operation — metallic, transient, reactive (compound) — was determined by the analysis of medium frequency (MF) magnetron voltage and current waveforms and a circulating power (power supply parameter). This parameter enables monitoring of any mismatch between plasma-magnetron impedance and the resonant circuit of power supply. The experiments show that the Al_xO_y layer formation conditions could be determined by use of the power supply parameters. Conclusions were supported by the refractive index and dielectric constant measurements.     

Characteristics of a magnetron cold cathode gauge

The discharge characteristics of a cold-cathode gauge of the non-inverted magnetron type were studied in ultra-high vacuum. The experimental magnetron cell of length 56 mm and diameter 32 mm was made of stainless steel. The cathode with a diameter of 6 mm was placed along the anode axis. The diameter of the anode was 25 mm and the length was 50 mm. Discharge current versus voltage and magnetic field was measured in the pressure range between 1×10⁻⁸ and 1×10⁻⁶ mbar. It was found that the current at first slowly increased with increasing voltage, reached a maximum at a certain voltage, and decreased rapidly with further increase of the voltage. The voltage, at which the current reached the maximum, depended on the magnetic field density and slightly on the pressure. A novel type of a cold cathode gauge with a self-adjusting power supply is suggested.     

Studies of medium frequency high power density magnetron sputtering discharges

Optical emission spectroscopy and Langmuir probe have been used to study the power dependence of medium frequency, 100 kHz, pulsed magnetron sputtering discharge. Copper target was sputtered in the argon atmosphere. The examined power ranged from 0.5 to 4.5 kW which gave an average power density on target surface from 25 to 115 W/cm². Optical spectroscopy did not reveal any significant changes of copper ion contribution to the sputtering process. The electron temperature and plasma potential changed a little with applied power. The electron density depended linearly on the sputtering power.     

High-rate reactive deposition of transparent SiO2 films containing low amount of Zr from molten magnetron target

The paper reports on a reactive deposition of transparent SiO₂ films with a low amount (≤ 3 at.%) of Zr prepared from the molten target using the AC pulsed dual magnetron. It is shown that the deposition rate a_D of the transparent oxide film strongly increases at the critical target power density (W_t)_cr when the solid target starts to melt and the magnetron operates with a molten target. In this case, the evaporation of target material plays a dominant role in the reactive deposition of thin films. This process is called the ionized magnetron evaporation. Oxide films reactively deposited from the molten target are well transparent and highly elastic. The maximum deposition rate of the transparent oxide film achieved in our experiments is 814 nm/min.     

Titanium oxide thin films deposited by high-power impulse magnetron sputtering

Ionized physical vapor deposition processes are of great interest for surface modification because the flexibility of the thin film deposition process can be increased by ionizing the metallic vapor. Recently, high-power impulse magnetron discharges have been implemented to achieve high ionization rates.Thin films of titanium oxide have been deposited on glass and steel substrates using 450 × 150 mm rectangular titanium target in argon-oxygen atmosphere. The average power delivered to the plasma is ranging between 1.5 and 2 kW and peak current and voltage are respectively 200 A and 900 V.Films are characterized using Scanning Electron Microscopy, Grazing Incidence X-ray Diffraction and Optical Transmission Spectroscopy. One of the major findings is the presence of rutile deposited on steel substrate (even for 0 V bias grounded substrate) and the significant increase of the refractive index of the films deposited on glass compared to thin films deposited via conventional direct current bipolar pulsed magnetron sputtering. Films synthesized by high-power impulse magnetron sputtering are denser.     

High conductivity and transparent ZnO:Al films prepared at low temperature by DC and MF magnetron sputtering

Aluminum-doped zinc oxide thin films have been deposited by DC and MF magnetron sputtering from a ceramic oxide target in argon atmosphere without direct heating of the substrates. The samples were prepared at different predetermined conditions of input power or discharge voltage and the influence upon electronic, optical, and microstructural properties has been investigated. The as-deposited layers show low resistivity, such as 9 × 10^− 4 Ω cm minimum for DC excitation and 1.2 × 10^− 3 Ω cm for MF mode, with growth rates up to 130 nm/min, and resulting substrate temperatures always below 200 °C. Low resistivity of the films is combined with high transmission, 85-90% in the visible wavelength range (400-800 nm). A strong (002) texture perpendicular to the substrate has been found, with lower strain for DC than for MF sputtering.     

The ion energy distributions and ion flux composition from a high power impulse magnetron sputtering discharge

The energy distribution of sputtered and ionized metal atoms as well as ions from the sputtering gas is reported for a high power impulse magnetron sputtering (HIPIMS) discharge. High power pulses were applied to a conventional planar circular magnetron Ti target. The peak power on the target surface was 1-2 kW/cm² with a duty factor of about 0.5%. Time resolved, and time averaged ion energy distributions were recorded with an energy resolving quadrupole mass spectrometer. The ion energy distributions recorded for the HIPIMS discharge are broader with maximum detected energy of 100 eV and contain a larger fraction of highly energetic ions (about 50% with E_i > 20 eV) as compared to a conventional direct current magnetron sputtering discharge. The composition of the ion flux was also determined, and reveals a high metal fraction. During the most intense moment of the discharge, the ionic flux consisted of approximately 50% Ti¹⁺, 24% Ti²⁺, 23% Ar¹⁺, and 3% Ar²⁺ ions.     

Transparent conductive ZnO:B films deposited by magnetron sputtering

This paper focuses on the preparation of boron doped ZnO (ZnO:B) films prepared by nonreactive mid-frequency magnetron sputtering from ceramic target with 2 wt.% doping source. Adjusting power density, ZnO:B film with low resistivity (1.54 × 10^− 3 Ω cm) and high transparency (average transparency from 400 to 1100 nm over 85%) was obtained. Different deposition conditions were introduced as substrate fixed in the target center and hydrogen mediation. Hall mobility increased from 11 to above 26 cm²/V·s, while carrier concentration maintained almost the same, leading to low resistivity of 6.45 × 10^− 4 Ω cm. Transmission spectra of ZnO:B films grown at various growth conditions were determined using a UV-visible-NIR spectrophotometer. An obvious blue-shift of absorption edge was obtained while transmittances between 600 nm and 1100 nm remained almost the same. Optical band baps extracted from transmission spectra showed irregular enhancement due to the Burstein-Moss effect and band gap renormalization. Photoluminescence spectra also showed a gradual increase at UV emission peak due to free exciton transition near band gap. We contributed this enhancement in both optical band gap and UV photoluminescence emission to the lattice structure quality melioration.     

Generation processes of super-high-energy atoms and ions in magnetron sputtering plasma

Energy distribution function (EDF) of ion species (Ar⁺, Kr⁺, Xe⁺) in a rare gas magnetron plasma is measured at a substrate position, 0.1 m away from the target surface, by energy-resolved mass spectrometry. The measured ion EDF contains, besides a bulk low-energy part (<10 eV), a tail part of super-high energy on an order of 100 eV, depending on the mass ratio of ion species to target material (tungsten, permalloy (80% Ni, 20% Fe)). A weak electric field in a diffusion region of magnetron plasma cannot accelerate slow bulk ions of ∼0.2 eV to such high energies. Origin of large kinetic energies is attributed to the backscattering process on the target surface where, e.g., Ar⁺ ions impinging on the target are neutralized and reflected as fast Ar atoms of the kinetic energy approximately given by a two-body collision model. Subsequently, a part of fast atoms may be converted to fast ions in three possible collision processes in the diffusion region: (i) electron impact ionization (ii) resonant charge exchange, and (iii) ionization of slow atoms by fast atoms. Among them, the third process is found to be dominant from Monte Carlo simulations where the backscattering process is evaluated by the TRIM code. Furthermore, when the target mass is larger than the bombarding ion mass, the substrate is bombarded by the super-high-energy atoms having a flux 2-4 orders of magnitude larger than the fast-ion flux.     

Magnetically confined high power thermionic line source emitter assembly

A directly heated thermionic high power electron beam source was constructed. The circular cross-section tungsten line cathode of length 140 mm with diameter 0.9 mm was used. Different gun design parameters were investigated and their results are discussed in detail. A uniform external magnetic field of 50 G was employed for focusing of electron beam at 180 ° deflection. The gun delivers uniform emission current density throughout the emission surface. The dimensions of the electron beam at worksite were comparable with the line cathode. The beam power of 57 kW was successfully achieved well below the saturation limit. The spring action mechanism was especially designed to avoid any cathode deformation. The gun design facilitates the reported length and emitting surface temperature of the cathode to be further increased to obtain higher emission values. The important gun features are operational reproducibility and long time stability. The evaporation rates for stainless steel have been achieved up to 1 kg/hr. An area of (280×120 mm²) could be heat treated with the line source electron beam in few milliseconds. The gun is extremely useful for melting, evaporation and heat treatment.     

The electron beam gun with thermionic hairpin-like cathode for welding and surface modifications

An axial thermionic electron beam emitter assembly with a special geometry of the cathode along with particular spacing of the electrodes has been used to produce a stable, sharp and high power density image at an acceleration voltage of 10 kV only. A hairpin-like tungsten wire, with diameter of 0.7 mm having semi-spherical emitting area at the crown with an angle of 45 degree at the vertex was used as a cathode. A direct heating method was used to heat the cathode. The emission current of the gun is in accordance with the Langmuir relation. An electromagnetic coil was used for focusing the beam at the target. A two dimensional programmable movement was applied to control the work site in the x-y direction. Focusing of the beam has been achieved up to 1 mm in diameter at an acceleration voltage of 10 kV.Thermionic efficiency of the gun is 4 mA W⁻¹ and the power density measured is ∼10⁵ W cm⁻².The gun was used for welding and surface modification of different materials including refractory metals.     

Design optimization of a hairpin electron source for electron beam welding

We report the optimization of the design and performance of recently reported hairpin tungsten electron source as a cathode in diode type geometry of the gun. The temperature maximum has been shifted close to the crown of the source. Focusing of the beam has been achieved up to 1 mm in diameter with Gaussian profile of the beam at the target. The perveance and power density measured are 10⁻⁵ A V^−3/2 and 10⁶ W cm⁻², respectively.     

Electrochemical performance of CuO nanocrystal film fabricated by room temperature sputtering

To develop high performance anode materials for thin film batteries, copper oxide (CuO) film is fabricated at room temperature by reactive radio frequency magnetron sputtering. Morphological characterization shows that the CuO film consists of compacted CuO columnar grains of 20 nm in diameter and 200 nm in thickness. The measurement of lithium storage capacity and cyclability of the CuO film show that the first charge capacity of the film is 585 mAh g⁻¹ with an efficiency of 68.3% at a current density of 200 mA g⁻¹. After the 50th cycle, the capacity retention remains as high as 97.4%. The nanostructured CuO film also shows a good rate capability even being cycled at 3000 mA g⁻¹ (5 C), demonstrating that the CuO film can be a promising material as an anode for high performance thin film batteries, especially for thin film battery with amorphous electrolyte.     

Development of a dedicated ion injector for accelerator-based nanoprobe facilities

The paper discusses possible ways of increasing beam brightness in ion injectors. The argon/helium ion injector comprising a newly designed RF ion source and, a Wien filter has been designed for use in accelerator-based nanoprobe facilities. The phase set degradation due to aberrations in the injector ion-optic system was simulated with allowance for multipole and fringing fields. The RF ion sources with different permanent magnet systems were tested. Experiments were performed with argon and helium. A plasma density of up to 3×10¹¹ cm⁻³ and beam brightness of ∼100 A/(m² rad² eV) were obtained. The ion current density inside an extracting electrode in the source was 10 mA/cm² for an emission hole diameter of 0.6 mm. Measurements of the current value and emittance were performed with ion source testing equipment permitting measurements of the ion beam current, emittance, mass composition, and RF power input into the plasma.     

Development of smooth CuInGa precursor films for CuIn1 − xGaxSe2 thin film solar cell applications

CuInGa precursor thin films were deposited using a CuGa (75-25 at.%) and an In 3″ diameter target material simultaneously by RF magnetron sputtering. The precursor films were deposited on Si and glass substrates at − 80 °C and room temperature, and characterized by Rutherford backscattering spectroscopy, Auger electron spectroscopy, scanning electron microscopy, atomic force microscopy and X-ray diffraction. The effects of gun power density and substrate temperatures on resulting precursor film properties were investigated. Precursor films deposited at − 80 °C have a smooth morphology with a 75% reduction in all roughness values and are more dense and homogeneous in structure compared to precursors deposited at room temperature. Therefore these precursors will result in better selenization process reproducibility.     

Study of the inductively coupled plasma assisted DC magnetron sputtering (ICPDMS) during ITO deposition

An inductively coupled plasma (ICP) assisted DC magnetron sputtering (ICPDMS) method for the deposition of indium tin oxide (ITO) thin films was developed to satisfy the challenging requirements of a room temperature process and high temperature durability. The resistivity of ITO thin films deposited by ICPDMS at room temperature was improved to as low as 1.2 × 10^− 2 Ω cm by increasing the RF power of the ICP source to 1200 W. Due to the additional dissociation and ionization by the high density plasma in ICPDMS system, the ITO thin films have a higher portion of Sn and oxygen atoms and a lower initial carrier concentration, ~ 10¹⁸ #/cm³, at room temperature than conventional ITO. However, the carrier concentration could be rapidly increased up to 10²⁰ #/cm³ by post-annealing to temperatures as high as 500 °C for 1 h under high vacuum conditions. Unlike conventional ITO, the electrical properties of ICPDMS-ITO were relatively unchanged after high temperature heat cycles, which is a very attractive property for high performance photovoltaic solar cell applications.     

Hydrogen-free diamond-like carbon films prepared by microwave electron cyclotron resonance plasma-enhanced direct current magnetron sputtering

Hydrogen-free diamond-like carbon (DLC) films were prepared by means of microwave electron cyclotron resonance plasma enhanced direct current magnetron sputtering. To study the influence of enhanced plasma on film fabrication and properties, the structures as well as mechanical and electrical properties of these films were studied as a function of applied microwave power. Results showed that higher microwave power could induce higher plasma density and electron temperature. The hardness increased from 3.5 GPa to 13 GPa with a variation of microwave power from 0 W to 1000 W. The resistivity showed a drastic increase from 4.5 × 10⁴ Ωcm at 0 W to 1.3 × 10¹⁰ Ωcm at 1000 W. The variation of the intensity ratio I(D)/I(G) and the position of the G-peak of the DLC films with respect to changes in microwave power were also investigated by Raman spectroscopy.     

The selective growth of rutile thin films using radio-frequency magnetron sputtering

Using unbalanced radio-frequency (RF) magnetron sputtering crystalline rutile films were synthesised on glass substrates at (combined Ar and O₂) pressures of 0.4 Pa or less, at RF powers of 500 and 600 W with substrate to magnetron distances of 40 mm or longer. Anatase films were deposited at the greater pressure of 1.2 Pa (substrate to magnetron distance of 40 mm) or shorter substrate to magnetron distance of 20 mm (at 0.4 Pa). A mixture of anatase and rutile was formed at 0.5 Pa with all other conditions being as for those required for rutile or the power was reduced along with the substrate to magnetron distance (500 W and 20 mm). The crystallite sizes of rutile obtained were 1 - 3 nm. It is proposed that the greater the energy imparted to the substrate surface by the impinging positive species the greater the activation energy to crystalline phase formation that can be overcome. Hence the formation of rutile over anatase is favoured at greater power, longer magnetron to substrate distances and decreased pressure. Moreover, not only is it possible to control the phase of TiO₂ formed it appears to be possible to control the degree of oxygen non-stoichiometry in the rutile films formed. Smaller O₂ partial pressures, shorter substrate to magnetron distances and greater RF power are believed to produce an environment of reduced reaction of sputtered Ti species with O₂ and to result in the formation of non-stoichiometric rutile structures resulting in increased band gap energies and decreased refractive indices.     

High-current electron sources based on gaseous discharges

We review the operation of a ferroelectric plasma source (FPS) with enhanced plasma density and of high-current hollow cathode (HC) and hollow anode (HA) discharges. Different schemes (arc sources, magnetron and FPS) were used for ignition and sustaining the HC and HA discharges with current amplitude ?4 kA.These discharges are characterized by a positive anode potential with respect to the hollow electrode walls and the plasma density and temperature inside the hollow electrode cavity reach ∼3×10¹⁹m⁻³ and ?12 eV, respectively. It was shown that the incorporation of the FPS in the HA and HC enables one to develop a compact high-current electron source. The characteristics of an electron diode with FPS, HA and HC were studied under an accelerating voltage ?250 kV and ∼400 ns pulse duration. It was shown that these sources allow the generation of an electron beam with a cross-sectional area of 0.01 m² and amplitude up to 1-2 kA.