Ulf Helmersson

Growth of single‐crystal TiN/VN strained‐layer superlattices with extremely high mechanical hardness

Single‐crystal TiN/VN strained‐layer superlattices (SLS’s) with layer thicknesses lTiN =lVN =λ/2 (where λ is the period of the superlattice) ranging from 0.75 to 16 nm have been grown on MgO(100 ) substrates by reactive magnetron sputtering. Cross‐sectional transmission electron microscopy (TEM) and x‐ray diffraction examinations showed that the films were single crystals exhibiting coherent interfaces and several orders of superlattice reflections. There was no evidence in either plan‐view or cross‐sectional TEM analyses of misfit interfacial dislocation arrays. The primary defects observed were dislocation loops with a diameter of 8–10 nm extending through several layers and small defects with a diameter of 1–2 nm that were confined within single layers. Microindentation hardness values H, measured as a function of λ in films with a total thickness of 2.5 μm, increased from 2035±280 kg mm−2 for Ti0.5V0.5N alloys (i.e., λ=0) to reach a maximum of 5560±1000 kg mm−2 at λ=5.2 nm and then decreased rapidly t...

High power impulse magnetron sputtering discharge

The high power impulse magnetron sputtering (HiPIMS) discharge is a recent addition to plasma based sputtering technology. In HiPIMS, high power is applied to the magnetron target in unipolar pulse ...

Microstructure modification of TiN by ion bombardment during reactive sputter deposition

Abstract Cross-sectional transmission electron microscopy has been used to investigate the effects of low energy (400 eV or less) ion irradiation during the growth of reactively sputtered TiN at temperatures between 300 and 900 °C. The films were deposited on high speed steel substrates in mixed ArN 2 discharges using an applied negative substrate bias voltage V s to vary the energy of impinging ions. The arrival rate ratio between ions and titanium atoms increased from 0.3 to 0.4 as V s was increased from 40 to 400 V. Films grown with V s ⩽ 200 V exhibited a columnar-like microstructure with a mixed (200)–(220) preferred orientation and the average column size increased with increasing T s . Both the width of the columns and the defect number density within each column were also influenced by ion bombardment. Raising V s above about 200 V resulted in a loss of preferred orientation together with an increasing dissolution of the columnar boundaries due to continuous renucleation during growth. Defect number densities in multilayer films were observed to vary abruptly and reversibly with changes in V s atall growth temperatures.

Optical properties of anatase TiO2 thin films prepared by aqueous sol-gel process at low temperature

TiO2 thin films were spin-coated on Si (100) substrates via an aqueous sol–gel route using Ti(OBun)4 and H2O2 as starting materials, and were annealed in air at different temperatures up to 550 °C for 1 h. X-Ray diffractometry indicates that crystallization into anatase started at 350 °C. The 350 °C-annealed films were further characterized by Auger electron spectroscopy, X-ray photoelectron spectroscopy, and variable angle spectroscopic ellipsometry. The results show that homogeneous, carbon-free TiO2 films with high refractive index (n=2.3 at 550 nm) were successfully obtained under an annealing temperature as low as 350 °C. The indirect and direct optical absorption bandgaps of the anatase film are estimated as 3.23 and 3.80 eV, respectively.

Influence of high power densities on the composition of pulsed magnetron plasmas

The application of high power pulses with peak voltage of -2 kV and peak power density of 3 kWcm-2 to magnetron plasma sources is a new development in sputtering technology. The high power is appli ...

High power pulsed magnetron sputtered CrNx films

Microstructure and macroscopic properties of droplet free CrN films deposited by the recently developed high power pulsed magnetron sputtering (HIPIMS) technique are presented. Magnetron glow discharges with peak power densities reaching 3000 W cm−2 were used to sputter Cr targets in both inert and reactive gas atmospheres. The flux arriving at the substrates consisted of neutrals and ions (approx. 70/30) of the sputtered metal and working gas atoms (Ar) with significantly elevated degree of ionization compared to conventional magnetron sputtering. The high-speed steel and stainless steel substrates were metal ion etched using a bias voltage of −1200 V prior to the deposition of CrN films. The film-to-substrate interfaces, observed by scanning transmission electron microscope cross-sections, were clean and contained no phases besides the film and substrate ones or recrystallized regions. CrN films were grown by reactive HIPIMS at floating potential reaching −160 V. Initial nucleation grains were large compared to conventional magnetron sputtered films, indicating a high adatom mobility in the present case. The films exhibited polycrystalline columnar growth morphology with evidence of renucleation. No intercolumnar voids were observed and the corrosion behavior of the film was superior to arc deposited CrNx. A high density of lattice defects was observed throughout the films due to the high floating potential. A residual compressive stress of 3 GPa and a hardness value of HK0.025=2600 were measured. A low friction coefficient of 0.4 and low wear rates against Al2O3 in these films are explained by the absence of droplets and voids known to contribute to extensive debris generation.

Ionized sputter deposition using an extremely high plasma density pulsed magnetron discharge

Time resolved plasma probe measurements of a novel high power density pulsed plasma discharge are presented. Extreme peak power densities in the pulse (on the order of several kW cm−2) result in a very dense plasma with substrate ionic flux densities of up to 1 A cm−2 at source-to-substrate distances of several cm and at a pressure of 0.13 Pa (1 mTorr). The pulse duration was ∼100 μs with a pulse repetition frequency of 50 Hz. The plasma consists of metallic and inert gas ions, as determined from time resolved Langmuir probe measurements and in situ optical emission spectroscopy data. It was found that the plasma composition at the beginning of the pulse was dominated by Ar ions. As time elapsed metal ions were detected and finally dominated the ion composition. The effect of the process parameters on the temporal development of the ionic fluxes is discussed. The ionized portion of the sputtered metal flux was found to have an average velocity of 2500 m s−1 at 6 cm distance from the source, which conforms...

Ion-assisted physical vapor deposition for enhanced film properties on nonflat surfaces

We have synthesized Ta thin films on Si substrates placed along a wall of a 2-cm-deep and 1-cm-wide trench, using both a mostly neutral Ta flux by conventional dc magnetron sputtering (dcMS) and a mostly ionized Ta flux by high-power pulsed magnetron sputtering (HPPMS). Structure of the grown films was evaluated by scanning electron microscopy, transmission electron microscopy, and atomic force microscopy. The Ta thin film grown by HPPMS has a smooth surface and a dense crystalline structure with grains oriented perpendicular to the substrate surface, whereas the film grown by dcMS exhibits a rough surface, pores between the grains, and an inclined columnar structure. The improved homogeneity achieved by HPPMS is a direct consequence of the high ion fraction of sputtered species.

Ionization of sputtered metals in high power pulsed magnetron sputtering

The ion to neutral ratio of the sputtered material have been studied for high power pulsed magnetron sputtering and compared with a continuous direct current (dc) discharge using the same experimen ...

A spectroscopic ellipsometry study of cerium dioxide thin films grown on sapphire by rf magnetron sputtering

Variable angle spectroscopic ellipsometry (VASE) has been used in the photon energy range 1.25–5.0 eV to study the structure and optical properties of cerium dioxide (CeO2) films. Both amorphous and highly oriented crystalline films were grown on sapphire by rf magnetron sputtering. The crystallinity, chemical structure, and surface morphology of the films were studied by x‐ray diffraction, x‐ray photoelectron spectroscopy, and atomic force microscopy, respectively. The measured VASE spectra on a series of films with different thicknesses were analyzed by using multiple optical models. In this way, the complex refractive index N=n+ik of CeO2, the film thicknesses, and the surface roughness of the different films could be determined. The ellipsometrically deduced refractive index spectrum was observed to be strongly dependent on the film structure. Highly oriented crystalline CeO2 films exhibited a higher refractive index and a higher band gap energy than the amorphous film. The surface roughness of the cr...