Influence of sulfidation treatment on the structure and tribological properties of nitrogen-doped diamond-like carbon films

The nitrogen-doped diamond-like carbon (DLC) films were deposited on high speed steel (HSS) substrates in the direct current unbalanced magnetron sputtering system. Sulphurized layer was formed on the surface of DLC films by means of liquid sulfidation in the intermixture of urea and thiourea solution in order to improve the tribological properties of DLC films. The influence of sulfidation treatment on the structure and tribological properties of DLC films was investigated in this work. The structure and wear surface morphology of DLC films were analyzed by Raman spectroscopy, XPS and SEM, respectively. It reveals that the treated films are smooth and uniform; and sulfur atoms are bonded chemically. The treated films have broader distribution of Raman spectra in the range of 1000-1800 cm⁻¹ and higher I_D/I_G ratio than the untreated films as a result of the appearance of the crystalline graphite structure after the sulfidation treatment. It is showed that the sp² relative content increase in the treated films from the XPS measurement. The Raman results are consistent with the XPS results. The tribological properties of DLC films were investigated using a ball-on-disk rotating friction and wear tester under dry friction conditions. It is found that the sulfidation concentration plays an important part in the tribological properties of the treated DLC films. The results showed the treated films with low sulfidation concentration have a lower friction coefficient (0.1) than the treated films with high sulfidation concentration (0.26) and the untreated films (0.27) under the same friction testing conditions, which can be attributed to both the presence of sulfur-containing materials and the forming of the mechanical alloyed layer on the wear surface. Adding the dry nitrogen to the sliding surface in the testing system helps the friction coefficient of the treated films with low sulfidation concentration to decrease to 0.04 further in this work. On the basis of the experimental results, it is indicated that the liquid sulfidation technique, which is low-cost, non-polluting and convenience, would be an appropriate method for the surface treatment of DLC films.     

Characterization and tribological investigation of SiO2 and La2O3 sol–gel films

Thin films of SiO₂ and La₂O₃ were prepared on a glass substrate by a dip-coating process from specially formulated sols. The tribological properties of the resulting thin films sliding against a Si₃N₄ ball were evaluated on a one-way reciprocating friction and wear tester. The morphologies of the unworn and worn surfaces of the films were examined by an atomic force microscope (AFM) and a scanning electron microscope (SEM). La₂O₃ shows the best tribological performance. The coefficient of friction is about 0.1 and the wear life is over 5000 sliding passes both under higher (3 N) and lower load (1 N). The SiO₂ film derived from a specially formulated aqueous solution shows much better performance in resisting wear and reducing friction than the one derived from an ethanol solution. The wear mechanisms of the films are discussed based on SEM observation of the worn surface morphologies. SEM observation of the morphologies of worn surfaces indicates that the worn surface of La₂O₃ is too slight to be observed by SEM. The wear of SiO₂ derived from TEOS solution is the characteristic of delaminating, which is responsible for the abrupt failure of the film. The wear of SiO₂ derived from aqueous solution is the characteristic of fracture. Brittle fracture and severe abrasion dominate the wear of glass substrate.     

Substrate bias effects during diamond like carbon film deposition by microwave ECR plasma CVD

Diamond like carbon (DLC) coatings were deposited on silicon(1 1 1) substrates by microwave electron cyclotron resonance (ECR) plasma CVD process using a plasma of Ar and CH₄ gases under the influence of DC self bias generated on the substrates by application of RF (13.56 MHz) power. DLC coatings were deposited under the varying influence of DC bias (−60 V to −150 V) on the Si substrates. Deposited films were analyzed by different techniques like: X-ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), atomic force microscopy (AFM), Hardness and elastic modulus determination technique, Raman spectroscopy, scanning electron microscopy (SEM) and contact angle measurement. The results indicate that the film grown at −100 V bias has optimised properties like high sp³/sp² ratio of carbon bonding, high refractive index (2.26–2.17) over wide spectral range 400–1200 nm, low roughness of 0.8 nm, high contact angle (80°) compared to the films deposited at other bias voltages (−60 V and −150 V). The results are consistent with each other and find august explanation under the subplantation model for DLC growth.     

Thickness dependence of Ic and Jc of LTG-SmBCO coated-conductor on IBAD-MgO tapes

We have reported SmBa₂Cu₃O_y (SmBCO) films on single crystalline substrates prepared by low-temperature growth (LTG) technique. The LTG-SmBCO films showed high critical current densities in magnetic fields compared with conventional SmBCO films prepared by pulsed laser deposition (PLD) method. In this study, to enhance critical current (I_c) in magnetic field, we fabricated thick LTG-SmBCO films on metal substrates with ion-beam assisted deposition (IBAD)-MgO buffer and estimated the I_c and J_c in magnetic fields.All the SmBCO films showed c-axis orientation and cube-on-cube in-plane texture. T_c of the LTG-SmBCO films were 93.1–93.4 K. J_c and I_c of a 0.5 μm-thick SmBCO film were 3.0 MA/cm² and 150 A/cm-width at 77 K in self-field, respectively. Those of a 2.0 μm-thick film were 1.6 MA/cm² and 284 A/cm-width respectively. Although I_c increased with the film thickness increasing up to 2 μm, the I_c tended to be saturated in 300 A/cm-width. From a cross sectional TEM image of the SmBCO film, we recognized a-axis oriented grains and 45° grains and Cu–O precipitates. Because these undesired grains form dead layers, I_c saturated above a certain thickness. We achieved that I_c in magnetic fields of the LTG-SmBCO films with a thickness of 2.0 μm were 88 A/cm-width at 1 T and 28 A/cm-width at 3 T.     

Tribological behaviors of self-assembled 3-aminopropyltriethoxysilane films on silicon

3-Aminopropyltriethoxysilane (APTES) thin films were prepared on the hydroxylated silicon substrate by a self-assembling process from formulated solution. Chemical compositions of the films were detected by X-ray photoelectron spectrometry (XPS). The thickness of the films was determined with an ellipsometer, while the morphologies of the original and worn surfaces of the samples were analyzed by means of atomic force microscopy (AFM) and scanning electron microscopy (SEM), respectively. The tribological properties of APTES thin films sliding against GCr15 steel ball were evaluated on a UMT-2MT reciprocating friction and wear tester. It was found that the macroscopic friction coefficients for coating times more than 1 h ranged from 0.177 to 0.3 whereas the value for short coating time was as high as 0.8. It was also found that the tribological behaviors of APTES films were sensitive to normal load and sliding velocity. SEM observation of the morphologies of worn surfaces indicates that the wear of silicon is characteristic of brittle fracture and severe abrasion. Differently, abrasion and micro-crack dominate the wear of APTES–SAM. The superior friction reduction and wear resistance of APTES films compared to the silicon substrate are attributed to good adhesion of the films to the substrate.     

Fabrication of Fe:CdSe solar rechargeable (semiconductor–septum) storage cells

The Fe:CdSe thin films have been electrodeposited potentiostatically onto the stainless steel substrates, from non-aqueous bath containing (CH₃COO)₂ · Cd · 2H₂O, SeO₂ and FeCl₃. The solar rechargeable (semiconductor–septum) storage cell is fabricated with the configuration C|1 M polysulphide|n-Fe:CdSe|stainless steel||1 M FeCl₃ or 1 M K₄Fe(CN)₆|C. The charging and discharging modes are studied and discussed. The comparison of FeCl₃ and K₄Fe(CN)₆ based solar rechargeable storage cells, showed that FeCl₃ based storage cell is superior than that of K₄Fe(CN)₆ based electrolyte because relatively charging time is minimum and discharging time is maximum. Thus it is concluded that the storage cell works not only as a generator but also as the storage of electricity.     

Surface engineering of biomedical metallic materials by plasma-based low-energy ion implantation

Plasma-based low-energy ion implantation, including plasma source ion nitriding/carburizing and plasma source low-energy ion enhanced deposition of thin films, for surface engineering of metallic materials was emerged as low-temperature, low-pressure surface modification technique. Plasma source ion nitriding onto AISI 316L austenitic stainless steel produced a high nitrogen face-centered-cubic phase (γ_N) layer about 10 μm thick at the temperature of 380 °C during 4 h with the high microhardness of HK_0.1 N 22.0 GPa. The microhardness of the nitrided surface from the titanium nitride phase [(Ti, Al, V)N] layer on Ti6Al4V alloy at 750 °C during 4 h achieved up to about HK_0.1 N 15.5 GPa. No pitting corrosion in the Ringer’s solution at 37 °C was detected by electrochemical polarization measurement for the nitrided AISI 316L stainless steel and Ti6Al4V alloy, respectively. Plasma source ion nitriding of the metallic materials provided the engineering surfaces with combined improvement in hardness and corrosion resistance.     

AZO/Ag/AZO multilayer films prepared by DC magnetron sputtering for dye-sensitized solar cell application

Ag films were deposited on Al-doped ZnO (AZO) films and coated with AZO to fabricate AZO/Ag/AZO multilayer films by DC magnetron sputtering on glass substrates without heating of glass substrates. The best multilayer films have low sheet resistance of 19.8 Ω/Sq and average transmittance values of 61% in visible region. It was found that the highest figure of merit (F_TC) is 6.9 × 10⁻⁴ Ω⁻¹. For the dye-sensitized solar cell (DSSC) application, the multilayer films were used as transparent conductive electrode (multilayer films/ZnO + Eosin-Y/LiI + I₂/Pt/FTO). The best DSSC based on the multilayer films showed that open circuit voltage (V_oc) of 0.47 V, short circuit current density (J_sc) of 2.24 mA/cm², fill factor (FF) of 0.58 and incident photon-to-current conversion efficiency (η) of 0.61%. It was shown that the AZO/Ag/AZO multilayer films have potential for application in DSSC.     

Effect of the composition on the superconducting properties of IBAD-MgO SmBCO coated conductors with superconducting film directly deposited on epi-MgO layer

Sm_1+xBa_2?xCu_3+yO_7?δ (SmBCO) films were directly deposited on the epi-MgO/IBAD-MgO/Y₂O₃/Al₂O₃/Hastelloy template by co-evaporation using the evaporation using drum in dual chambers (EDDC) system without the buffer layer in order to investigate the effect of the composition ratios on superconducting property, microstructure and texture of SmBCO film. The films with gradient composition ratios of Sm:Ba:Cu were deposited using a shield with an opening which was placed between the substrate and the boats. The highest I_c of 52 A (corresponding to J_c = 1.6 MA/cm² and a thickness of 800 nm) was observed at 77 K in self field at a composition x = 0.01–0.05 and y = ?0.23 to ?0.46. When the composition ratio is outside this range, the I_c value rapidly decreased. The superconducting critical current was highly dependent on the composition ratio. As the composition ratio is farther away from that of the highest I_c, the SmBCO (1 0 3) peak intensity increased and the amount of a-axis oriented parts increased. A dense microstructure with round-shape grains was observed in the region showing the highest I_c. The optimum composition ratio can be found by analyzing films deposited with variable deposition rates of each depositing element.     

Transparent CdO/n-GaN(0001) heterojunction for optoelectronic applications

Undoped CdO films were prepared by sol–gel method. Transparent heterojunction diodes were fabricated by depositing n-type CdO films on the n-type GaN (0001) substrate. Current–voltage (I–V) measurements of the device were evaluated, and the results indicated a non-ideal rectifying characteristic with I_F/I_R value as high as 1.17×10³ at 2 V, low leakage current of 4.88×10⁻⁶ A and a turn-on voltage of about 0.7 V. From the optical data, the optical band gaps for the CdO film and GaN were calculated to be 2.30 eV and 3.309 eV, respectively. It is evaluated that interband transition in the film is provided by the direct allowed transition. The n-GaN (0001)/CdO heterojunction device has an optical transmission of 50–70% from 500 nm to 800 nm wavelength range.     

Oxygen assisted deposition of Sr2FeMoO6 thin films on SrTiO3(1 0 0)

Epitaxial thin films of Sr₂FeMoO₆ (SFMO) were prepared by pulsed laser deposition on SrTiO₃(1 0 0) substrate. Thin films have been grown under different gas environments and they were structurally characterised by XRD. In contrast to previous reports, deposition carried out in the presence of a small amount of O₂ with Ar yields high-quality SFMO films with a saturation magnetic moment of 3.8 μ_B. These SFMO films were strained in such a way that they were elongated along the c-axis and compressed in the ab-axes directions. The large low-field magnetoresistance seen in these films has been attributed to the tunneling across the antisite boundaries.     

Modifications in physical,optical and electrical properties of tin oxide by swift heavy Au8+ ion bombardment

Tin oxide thin films were deposited by a novel technique called as modified-SILAR. The preparative parameters were optimized to obtain good quality thin films. As-deposited films were annealed in O₂ atmosphere for 1 h at 500 °C. The annealed films were irradiated using Au⁸⁺ ions with energy of 100 MeV at different fluencies of 1 × 10¹¹, 1 × 10¹², 5 × 10¹² and 1 × 10¹³ ions/cm² using tandem pelletron accelerator. The irradiation-induced modifications in tin oxide thin films were studied using XRD, AFM, optical band gap, photoluminescence and I–V measurements. XRD studies showed formation of tin oxide with tetragonal structure. AFM revealed uniform deposition of the material with increase in grain size after irradiation. Decrease in band gap from 3.51 eV to 2.82 eV was seen with increases in fluency. A decrease in PL intensity, and an additional peak was observed after irradiation. I–V measurements showed a decrease in resistance with fluency.     

Preparation and properties of ceramic coating on Q235 carbon steel by plasma electrolytic oxidation

Ceramic coating was achieved on Q235 carbon steel by PEO (plasma electrolytic oxidation, PEO) without any pretreatment in sodium aluminate system. The discharge process as well as the accompanied surface morphology evolution was analyzed. The phase and elemental composition of the coatings were also investigated. The corrosion, mechanical and tribological properties of the ceramic coating were primarily studied. It is found that the coating surface was porous and the thickness of the coating was about 120 μm. The coating mainly consisted of FeAl₂O₄, Fe₃O₄ and a little γ-A1₂O₃. The corrosion current of the coated sample was 3.082 × 10⁻⁷ A/cm², which was decreased by two orders of magnitude compared with the uncoated one. The micro hardness of the ceramic coating was 1210 Hv, which was about three times as that of the uncoated sample. The friction coefficient of coated sample was also well improved. Investigations revealed that PEO provided a promising technique for preparation of protective ceramic coatings on steels.     

Homoepitaxial growth of MOD-YBCO thick films on evaporated and MOD templates

We have prepared metal organic deposition (MOD)-YBCO thick films by repeating the coating-pyrolysis-crystallization procedure onto ～100-nm-thick evaporated and MOD templates. Surface morphology of the template was found to strongly affect the homoepitaxial growth of MOD-YBCO layers on the template; namely, the epitaxial growth of MOD-YBCO on the evaporated template was much easier than that on the MOD template. A 220-nm-thick epitaxial MOD-YBCO film was successfully prepared on the 100-nm-thick evaporated-YBCO template to obtain a 320-nm-thick YBCO film, which exhibited J_c = 2.44 MA/cm² and I_c = 78 A/cm. The I_c value has significantly increased from 37 A/cm for the evaporated-template.     

Influence of crystalline diamond nanoparticles on diamond-like carbon friction behavior

Crystalline diamond (CD) particles have been incorporated in diamond-like carbon (DLC) film structure in order to improve DLC electrochemical corrosion resistance. This paper shows the investigation of CD-DLC friction behavior according to the CD average sizes and concentration. The films were growth over 304 stainless steel using plasma enhanced chemical vapor deposition. The response surface methodology was used to develop a mathematical modeling of friction for these films, using the experimental results, in order to identify parameters that control friction and construct tribological maps according to the CD average sizes. The presence of bigger CD particles (250 and 500 nm) increased the film roughness. Films with CD particles of 4 nm presented the most homogeneous friction map, with minor variation in friction coefficient with the increase/decrease of load and sliding speed even when the CD concentration increase. This result suggests that in CD-DLC films containing CD particles of 4 nm average size, the nanoparticles are better incorporated in DLC structure due to its average size (4 nm) that is near than DLC grain size and could occupy the nanospaces between DLC grains.     

Long RE123 coated conductors with high critical current over 500 A/cm by IBAD/PLD technique

We have developed long RE₁Ba₂Cu₃O_7?X (RE123) coated conductors with large current capacity by the ion beam assisted deposition (IBAD) and the pulsed laser deposition using hot wall heating (HW-PLD) technique. As a result, we could fabricate an 8 m-long Gd₁Ba₂Cu₃O_7?X (Gd123) coated wire with the minimum and maximum critical current (I_c) of 951 A/cm-w and 1003 A/cm-w at 77 K, 0 T, respectively, measured in 0.7 m-long sections by the standard 4-probe technique. Furthermore, we succeeded in preparation of over 600 m-long Gd123 coated wire with the uniform I_c distribution over 600 A/cm-w. It had average, maximum and minimum I_c of 665, 698, 609 A/cm-w, respectively. The n-values of the sample showed the maximum I_c and minimum I_c were 40 and 36, respectively. As a result, we set the new world record of I_c × L value as 374535 A m (= 609 A × 615 m). The in-field performance of this long wire was quite high as well; the minimum I_c exceeded 50 A/cm-w at 77 K, 3 T.     

Investigation of properties of Cu containing DLC films produced by PECVD process

Copper containing diamond like carbon (Cu-DLC) thin films were deposited on various substrates at a base pressure of 1×10^?3 Torr using a hybrid system involving DC-sputtering and radio frequency-plasma enhanced chemical vapor deposition (RF-PECVD) techniques. The compressive residual stresses of these films were found to be considerably lower, varying between 0.7 and 0.94 GPa and Cu incorporation in these films improve their conductivity significantly. Their structural properties were studied by Raman spectroscopy, atomic force microscopy, scanning electron microscopy, X-ray photoelectron spectroscopy and X-ray diffraction techniques that clearly revealed the presence of Cu in the DLC structure. Raman analysis yields that Cu incorporation in DLC enhances the graphite-like sp² bonding. However, the sp² bonding was found to continuously reduce with the increasing C₂H₂ gas pressure, this may be due to reduction of Cu nanocrystal at the higher pressure. FTIR results inferred various bonding states of carbon with carbon, hydrogen and oxygen. In addition, hydrogen content and sp³ and sp² fractions in different Cu-DLC films were also estimated by FTIR spectra and were correlated with stress, electrical, optical and nano-mechanical properties of Cu-DLC films. The effect of indentation load (4–10 mN) on nano-mechanical properties of these films was also explored.     

Intense 974 nm emission from ErxYb2−xSi2O7 films through efficient energy transfer up-conversion from Er3+ to Yb3+ for Si solar cell

The optical properties of the Er_xYb_2?xSi₂O₇ thin films were investigated by photoluminescence measurements and the intense 974 nm light emission was observed. The 974 nm emission was mainly from the transition ²F_5/2 to ²F_7/2 level of Yb³⁺ upon exploring energy-transfer via up-conversion at Er^{3+ 4}I_13/2 level. Under 972 nm excitation, the lifetime at Er^{3+ 4}I_13/2 level reaches up to 4 ms for film containing 2 at% Er³⁺, while decreases to about 20 μs as the film is pumped by 488 nm. This confirmed that the energy transfer up-conversion process was the dominant transition at Er^{3+ 4}I_13/2 level. This may be of interest to improve the solar cells′ efficiency by placing this film at the rear of cell, converting the near-infrared photons between 1480 nm and 1580 nm to just above the Si bandgap.     

Excess currents larger than the point contact limit in normal-metal/superconducting junctions

In a point contact NS junction, perfect Andreev reflection occurs over a range of voltages equal to the superconducting energy gap, producing an excess current of I_exc =  (4 / 3)(2 eΔ / h). If the superconductor has a finite width, rather than the infinite width of the point contact, one cannot neglect superfluid flow inside the superconducting contact. The energy range available for perfect Andreev reflections then becomes larger than the superconducting gap, since superfluid flow alters the dispersion relation inside the finite width superconductor. We find a maximum excess current of approximately (7 / 3)(2 eΔ / h) when the width of the superconductor is approximately 7 / 3 times the width of the normal metal.     

Study of well adherent DLC film deposited on piezoelectric LiTaO3 substrate

A well adherent diamond-like carbon (DLC) film was deposited on piezoelectric LiTaO₃ substrate using PECVD by inserting SiO₂ interlayer. DLC film was characterized using Raman spectroscopy and AFM. Physical and mechanical properties were measured using XRR, ellipsometry, scratch test and nano-indentation. The DLC film exhibits the characteristics of hydrogenated amorphous carbon and a very smooth surface with a 0.25 nm RMS. Scratch test shows that critical load (L_c) is 18 N, which is good enough for applying DLC film to SAW device. The measured mass density, refractive index, hardness and Young’s modulus of DLC film deposited on LiTaO₃ are comparable to the reported values for hydrogenated amorphous carbon film, irrespective of substrates on which the films were deposited.