| 1. |
- Anastasopoulos, M., et al.
(author)
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Multi-Grid detector for neutron spectroscopy : Results obtained on time-of-flight spectrometer CNCS
- 2017
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In: Journal of Instrumentation. - : IOP PUBLISHING LTD. - 1748-0221. ; 12:4
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Journal article (peer-reviewed)abstract
- The Multi-Grid detector technology has evolved from the proof-of-principle and characterisation stages. Here we report on the performance of the Multi-Grid detector, the MG.CNCS prototype, which has been installed and tested at the Cold Neutron Chopper Spectrometer, CNCS at SNS. This has allowed a side-by-side comparison to the performance of 3He detectors on an operational instrument. The demonstrator has an active area of 0.2 m2. It is specifically tailored to the specifications of CNCS. The detector was installed in June 2016 and has operated since then, collecting neutron scattering data in parallel to the He-3 detectors of CNCS. In this paper, we present a comprehensive analysis of this data, in particular on instrument energy resolution, rate capability, background and relative efficiency. Stability, gamma-ray and fast neutron sensitivity have also been investigated. The effect of scattering in the detector components has been measured and provides input to comparison for Monte Carlo simulations. All data is presented in comparison to that measured by the 3He detectors simultaneously, showing that all features recorded by one detector are also recorded by the other. The energy resolution matches closely. We find that the Multi-Grid is able to match the data collected by 3He, and see an indication of a considerable advantage in the count rate capability. Based on these results, we are confident that the Multi-Grid detector will be capable of producing high quality scientific data on chopper spectrometers utilising the unprecedented neutron flux of the ESS.
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| 2. |
- Schmidt, Susann, et al.
(author)
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Boron-10 lined RPCs for sub-millimeter resolution thermal neutron detectors : Feasibility study in a thermal neutron beam
- 2019
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In: Journal of Instrumentation. - : IOP PUBLISHING LTD. - 1748-0221. ; 14:1
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Journal article (peer-reviewed)abstract
- The results of an experimental feasibility study of a position sensitive thermal neutron detector based on a resistive plate chamber (RPC) are presented. The detector prototype features a thin-gap (0.35 mm) hybrid RPC with an aluminium cathode and a float glass anode. The cathode is lined with a 2 mu m thick (B4C)-B-10 neutron converter enriched in B-10. A detection efficiency of 6.2% is measured at the neutron beam (lambda = 2.5 angstrom) for normal incidence. A spatial resolution better than 0.5 mm FWHM is demonstrated.
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| 3. |
- Ahmad, Mohammed Metwally Gomaa, et al.
(author)
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Effect of precursor solutions on the structural and optical properties of sprayed NiO thin films
- 2017
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In: Materials Science in Semiconductor Processing. - : Elsevier BV. - 1369-8001 .- 1873-4081. ; 64, s. 32-38
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Journal article (peer-reviewed)abstract
- Nickel oxide thin films were deposited by a simple and low-cost spray pyrolysis technique using three different precursors: nickel nitrate, nickel chloride, and nickel acetate on corning glass substrates. X-ray diffraction show that the NiO films are polycrystalline and have a cubic crystal structure, although predominantly with a preferred 111-orientation in the growth direction and a random in-plane orientation. The deconvolution of the Ni 2p and O 1s core level X-ray photoelectron-spectra of nickel oxides produced by using different precursors indicates a shift of the binding energies. The sprayed NiO deposited from nickel nitrate has an optical transmittance in the range of 60-65% in the visible region. The optical band gap energies of the sprayed NiO films deposited from nickel nitrate, nickel chloride and nickel acetate are 3.5, 3.2 and 3.43 eV respectively. Also, the extinction coefficient and refractive index of NiO films have been calculated from transmittance and reflectance measurements. The average value of refractive index for sprayed films by nickel nitrate, nickel chloride and nickel acetate are 2.1, 1.6 and 1.85 respectively. It is revealed that the band gap and refractive index of NiO films by using nickel nitrate corresponds to the commonly reported values. We attribute the observed behavior in the optical band gap and optical constants as due to the change of the Ni/O ratio.
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| 4. |
- Bakoglidis, Konstantinos, et al.
(author)
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Comparative study of macro- and microtribological properties of carbon nitride thin films deposited by HiPIMS
- 2017
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In: Wear. - : ELSEVIER SCIENCE SA. - 0043-1648 .- 1873-2577. ; 370
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Journal article (peer-reviewed)abstract
- The macro- and microtribological properties of carbon nitride thin films deposited by high power impulse magnetron sputtering at different substrate bias voltages (V-b) were investigated. V-b of -100, -150, -200, and-300 V were used. A Hysitron Triboindenter TI950 and a reciprocating Tribotechnic tribometer with diamond counterparts were used in order to assess the tribological performance of the films at the micro- and macroscale, respectively. Initial Hertzian contact pressures of 2.5 GPa, 3.3 GPa and 3.9 GPa were chosen for the comparative measurements at both scales. At the macroscale, films with higher initial roughness present an increased wear. Debris creation and asperity deformation takes place causing abrasive wear. At the microscale, compression of the surface material occurs. The run-in friction shows similar trends at both scales; an initial decrease and an increase thereafter. Steady-state friction is not reached at the microscale, attributed to the absence of a graphitic tribolayer in the contact. At the macroscale, all films show abrasive wear and debris creation. Here, the changes in friction coefficients are attributed to the debris loss from the contact during the tribotests. The CN film tested at 2.5 GPa shows a continuous increase of friction, due to the continuous loss of debris from the contact. The other films reach a steady-state friction coefficient, since most of the debris is lost before the end of the tribotests. (C) 2016 Elsevier B.V. All rights reserved.
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| 5. |
- Bakoglidis, Konstantinos D., 1985-
(author)
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Low Friction and Wear Resistant Carbon Nitride Thin Films for Rolling Components Grown by Magnetron Sputtering
- 2015
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Licentiate thesis (other academic/artistic)abstract
- The scope of this licentiate thesis is the investigation of carbon based thin films suitable for rolling components, especially roller bearings. Carbon and carbon nitride are materials with advantageous tribological properties and high resiliency. Such materials are required in order to withstand the demanding conditions of bearing operation, such as high loads and corrosive environments. A fundamental condition for coated bearings is that the deposition temperature must be striktly limited. Thus, carbon nitride (CNx) thin films were synthesized here at low temperature of 150 oC by different reactive magnetron sputtering techniques, which are mid-frequency magnetron sputtering (MFMS), direct current magnetron sputtering (DCMS), and high power impulse magnetron sputtering (HiPIMS). While DCMS is a very well studied technique for carbon based films, MFMS and HiPIMS are relatively new sputtering techniques for carbon, and especially CNx depositions. Using different magnetron sputtering techniques, different ionization conditions prevail in the chamber during each process and influence the obtained film properties at a great extent. It was found that bias duty cycles and the amount of working gas ions are key parameters and affect the morphology and microstructure as well as the mechanical response of the films. Moreover, different bias voltages, from 20 V up to 120 V were applied during the processes in order to investigate the changes that the different ion energies induce in the film structure.The structural, mechanical and tribological properties of CNx films are also presented in this licentiate thesis. The morphology of CNx films strongly depends on both the deposition technique and ion energy. The special configuration of MFMS mode produces highly homogeneous and dense films even from low applied bias voltages, while in HiPIMS mode high bias voltages above 100 V must be applied in order to produce films with similar structural characteristics. DCMS is also proven as a good technique for homogeneous and dense films. Low bias voltages do not favor homogeneous structures, thus at 20 V all techniques produced films with columnar structures with intercolumnar voids. High bias voltages influence the N incorporation in the films, with the appearance of re-sputtering of N-containing species and a promotion of sp2 bonding configurations with increasing ion energy. Nevertheless, the different deposition mode influences the sp2 content in different ways, with only MFMS showing a clear increase of sp2 content with increasing bias voltage and HiPIMS showing relatively constant sp2 content. The morphology and microstructure of the CNx films affects their mechanical response, with higher ion energies producing harder films. A dependency of hardness and elastic modulus with increasing ion energy was obtained, where for all deposition modes, hardness and elastic modulus increase linearly with increasing bias voltage. Films with hardness as high as 25 GPa were synthesized by MFMS at 120 V , while the softer film yielded a hardness of 7 GPa and was deposited by HiPIMS at 20 V . The elastic recovery of the films differs with increasing ion energies, presenting a correlation with the C sp2 bond content. The highest elastic recovery of 90% was extracted for the film deposited by MFMS at 120 V and is a value similar to the elastic recovery obtained for FL-CNx films. All films developed compressive residual stresses, depending also on the ion energies and the deposition mode used. It is demonstrated that the induced stresses in the films increase when denser and more homogeneous film morphologies are obtained and with higher Ar intercalcation. Low friction coefficients were obtained for all films between 0.05 and 0.07, although the deposition conditions are not detrimental for the development of friction coefficient. The wear resistance of the films was found to be dependent on the morphology and to some extent on the microstructure of the films. Harder, denser, and more homogeneous films have higher wear resistance. Especially, CNx films deposited by MFMS at 120 V present no wear.The tribological characteristics of the surface of the films were also investigated at nanoscale by a new reciprocal wear test. In this wear test, the recording of the track profile is performed in between consecutive test cycles, eliminating also thermal drift. The very low wear of the films deposited by MFMS at 100 V and 120 V revealed that during the wear test a phase transformation on the surface may take place, possibly graphitization. It is also demonstrated the way that the surface characteristics, such as asperities and roughness affects the tribological measurements. Attention is also turned to the presence of large asperities on the film surface and the way they affect the obtained average friction coefficient and tribological measured data.
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| 6. |
- Bakoglidis, Konstantinos D., et al.
(author)
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Low-temperature growth of low friction wear-resistant amorphous carbon nitride thin films by mid-frequency, high power impulse, and direct current magnetron sputtering
- 2015
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In: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films. - : American Vacuum Society. - 0734-2101 .- 1520-8559. ; 33:5
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Journal article (peer-reviewed)abstract
- Amorphous carbon nitride (a-CNx) thin films were deposited on steel AISI52100 and Si(001) substrates using mid-frequency magnetron sputtering (MFMS) with an MF bias voltage, high power impulse magnetron sputtering (HiPIMS) with a synchronized HiPIMS bias voltage, and direct current magnetron sputtering (DCMS) with a DC bias voltage. The films were deposited at a low substrate temperature of 150 °C and a N2/Ar flow ratio of 0.16 at the total pressure of 400 mPa. The negative bias voltage (Vs) was varied from 20 V to 120 V in each of the three deposition modes. The microstructure of the films was characterized by high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), while the film morphology was investigated by scanning electron microscopy (SEM). All films possessed amorphous microstructure with clearly developed columns extending throughout the entire film thickness. Layers grown with the lowest substrate bias of 20 V exhibited pronounced intercolumnar porosity, independent of the technique used. Voids closed and dense films formed at Vs ≥ 60 V, Vs ≥ 100 V and Vs = 120 V for MFMS, DCMS and HiPIMS, respectively. X-ray photoelectron spectroscopy (XPS) revealed that the nitrogen-to-carbon ratio, N/C, of the films ranged between 0.2 and 0.24. Elastic recoil detection analysis (ERDA) showed that Ar content varied between 0 and 0.8 at% and increases as a function of Vs for all deposition techniques. All films exhibited compressive residual stress, σ, which depends on the growth method; HiPIMS produces the least stressed films with stress between – 0.4 and – 1.2 GPa for all Vs values, while for CNx films deposited by MFMS σ = – 4.2 GPa. Nanoindentation showed a significant increase in film hardness and reduced elastic modulus with increasing Vs for all techniques. The harder films were produced by MFMS with hardness as high as 25 GPa. Low friction coefficients, between 0.05 and 0.06, were recorded for all films. Furthermore, CNx films produced by MFMS and DCMS at Vs = 100 V and 120 V presented a high wear resistance with wear coefficients of k ≤ 2.3 x 10-5 mm3/Nm.
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| 7. |
- Bakoglidis, Konstantinos D., et al.
(author)
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Nanotribological properties of wear resistant a-CNx thin films deposited by mid-frequency magnetron sputtering
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Other publication (other academic/artistic)abstract
- The nanotribological properties of amorphous carbon nitride (a-CNx) thin films deposited with mid-frequency magnetron sputtering (MFMS) were investigated at the nanoscale using an in-situ technique in a Hysitron Triboindenter TI 950. The friction coefficient, wear rate, track roughness, and the track profiles were recorded as a function of the number of linear reciprocal cycles, revealing the manner that the nanotribological and surface properties change during the wear test. The surface composition of the films was evaluated by x-ray photoelectron spectroscopy (XPS). The friction coefficient ranges between 0.05 – 0.07, while the wear coefficient ranges from 9.4 x 10-8 up to 1.5 x 10-4 mm3/Nm. Debris particles and surface modifications characterize the friction and lubrication behavior in the track. The friction and main lubrication mechanism on the modified surface changes after the removal of debris particles, while this change appears at different cycle for each CNx film depending on the substrate bias voltage. Films grown at higher bias are modified earlier than films grown at lower bias. The wear behavior can be divided into two, track roughnessdependent, regimes; (1) films with track roughness > 1 nm showed wear with obvious tracks and (2) the films with roughness < 1 nm showed negative wear at the nanometer scale with a volume of material projected in the area of the wear track. This material volume is believed to be result of a surface modification, where the molar volume of the modified surface is larger than the molar volume of the surface before the wear test.
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| 8. |
- Bakoglidis, Konstantinos, et al.
(author)
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Improved adhesion of carbon nitride coatings on steel substrates using metal HiPIMS pretreatments
- 2016
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In: Surface & Coatings Technology. - : ELSEVIER SCIENCE SA. - 0257-8972 .- 1879-3347. ; 302, s. 454-462
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Journal article (peer-reviewed)abstract
- We investigate the effect of low-temperature metal pretreatments in order to improve the adhesion of CNx coatings on steel substrates, which is crucial for tribological applications. The substrate pretreatments were conducted using five different metal targets: Ti, Zr, Al, Cr, and W, operated in high power impulse magnetron sputtering mode, known to produce significant ionization of the sputtered material flux. The CNx adhesion, as assessed by Rockwell C tests, did not improve upon Ti and Zr pretreatments. This is primarily ascribed to the fact that no interlayer was formed owing to severe re-sputtering due to high fluxes of doubly-ionized metal species in the plasma. A slight improvement in adhesion was observed in the case an Al pretreatment was carried out, while the best results were obtained using Cr and W. Here, 30-s-long pretreatments were sufficient to clean the steel surface and form a metallic interlayer between substrate and coating. Transmission electron microscopy in combination with energy dispersive X-ray spectroscopy revealed that Al, Cr, and W created intermixing zones at the interlayer/substrate and the interlayer/CNx interfaces. The steel surfaces, pretreated using Cr or W, showed the highest work of adhesion with W-adh(Cr) = 1.77 J/m(2) and W-adh(W) = 1.66 J/m(2), respectively. (C) 2016 Elsevier B.V. All rights reserved.
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| 9. |
- Bakoglidis, Konstantinos
(author)
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Low-friction and wear-resistant carbon nitride coatings for bearing components grown by magnetron sputtering
- 2016
-
Doctoral thesis (other academic/artistic)abstract
- The scope of this thesis is the investigation of magnetron sputtered carbon nitride coatings suitable for roller bearing components. The research field of tribology of bearings focuses on minimizing friction between components by improving the lubricants. The development of lubricants is, however, expensive and involves environmentally deleterious chemical byproducts. A solution to avoid such harmful conditions, reduce the processing cost, and more importantly, minimize the friction, is to apply a low-friction and wear-resistant coating on the surface of the bearing. The deposition of such coatings on components can substantially increase their lifetime, reduce the maintenance costs, and eventually increase the reliability of the machinery.Carbon nitride (CNx) coatings have high resiliency and can withstand the demanding conditions of bearing operation. The morphology of CNx coatings is highly affected by applying a negative substrate bias voltage. At high bias (100-120 V ), the coatings become denser and more homogeneous with decreased porosity, resulting in more wear-resistant materials. I also found that the duty cycle of the applied bias affects the layer morphology. Less homogeneous films are produced using lower duty cycles (i.e., in high power impulse magnetron sputtering, HiPIMS) for a specific value of bias voltage. Thus, changing bias voltage, we can manipulate the structure of CNx and design layers, depending on the requirements of the bearing application.My results show that denser films yield higher hardness and wear-resistance, but also higher compressive stress, which is a disadvantage for the coating-substrate adhesion. In order to obtain improved adhesion on bearing steel, we developed an in-situ surface treatment, prior to the CNx deposition, which also surpasses the limitations set by the properties of each material. The steel substrates are successfully pretreated using W or Cr ions originating from a HiPIMS source. Plasma ions are accelerated to the substrates with energies of 900 eV , due to the application of a synchronized high bias voltage, which clean effectively the substrate surface from residual contaminants and strengthen the interfacial bonding.CNx-coated rollers are tested in rolling operation and show the absence of run-in period in all lubrication regimes. This is a big advantage for applications which rotate under boundary lubrication (BL). The coated rollers yield friction coefficients in the range of 0:020 and 0:025 in elastohydrodynamic (EHDL) and hydrodynamic (HDL) lubrication regimes, being lower than the friction coefficients of 0:026-0:052, exhibited by the uncoated rollers. Here, friction decreases steadily with increasing number of cycles, due to the presence of CNx in the contact. In BL, CNx-coated rollers present an increased friction coefficient of 0:052, but the wear is much lower than in the case of uncoated rollers. All rollers are covered with CNx in the wear tracks after the tests, avoiding failures and presenting low abrasive wear. The obtained tribological performance of the CNx-coated rollers in rolling is overall improved compared to the established operation of uncoated rollers. Thus, CNx layers can function as low-friction and wear-resistant coatings protecting the steel components in several roller bearing applications, such as in gearboxes and wheels in automotive, aerospace, marine, and turbine industry.
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| 10. |
- Bakoglidis, Konstantinos, et al.
(author)
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Rolling contact fatigue of bearing components coated with carbon nitride thin films
- 2016
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In: Tribology International. - : ELSEVIER SCI LTD. - 0301-679X .- 1879-2464. ; 98, s. 100-107
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Journal article (peer-reviewed)abstract
- Bearing rollers were coated with CNx films using high power impulse magnetron sputtering deposition in order to reduce their rolling-contact fatigue as investigated using a Micro-Pitting Rig tribometer under poly-alpha-olefin lubricated conditions. Coated rollers with a similar to 15 nm thick W adhesion layer to the substrate, exhibit the best performance, presenting mild wear and no fatigue after 700 kcycles. The steady-state friction coefficient was similar to 0.05 for both uncoated and coated rollers. Uncoated rollers show run-in friction in the first 50 kcycles, because of steel-to-steel contact, which is absent for coated rollers. Analytical transmission electron microscopy and X-ray photoelectron spectroscopy show that the presence of a CNx coating prevents steel-to-steel contact of the counterparts, prior to the elastohydrodynamic lubrication, reducing their wear and increasing the lifetime expectancy. (C) 2016 Elsevier Ltd. All rights reserved.
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