Thermal radiative properties of a DLC coating

Thermal radiative properties of a DLC coating were measured in the range of cryogenic and room temperatures. Both the total hemispherical emissivity and absorptivity are significantly dependent on the radiation temperature and change from the value of 0.032 at 15 K to 0.65 at 300 K.     

Direct measurement of total emissivities at cryogenic temperatures: Application to satellite coatings

This paper presents a direct measurement method for optical properties of different materials at cryogenic temperatures from 20 K to 200 K. It has been developed within the framework of the design of Planck program. Planck is a satellite of the European Space Agency (ESA) that will be launched in 2008. The scientific goal of the Planck mission is to make observations of the temperature anisotropy and polarisation of the Cosmic Microwave Background. The equivalent temperature of the observed radiation is about 3 K and the telescope baffle temperature should not exceed 60 K in order to work properly. The large Planck telescope is passively cooled by radiating to the Deep Space, so that a good knowledge of the thermo-optical properties of its coating is of utmost importance for thermal modelling. However, up to now, few measurements have been done at such low temperatures. We derived a direct measurement method for the total directional emissivity of various coatings of interest for satellites applications. The effective spectral range chosen the measurements covers 6–800 μm. We will describe the design of the measurement apparatus and present results for several coatings.     

Structure and corrosion resistance of nickel coatings containing tungsten and silicon powders

Ni + W + Si coatings were prepared by nickel deposition from a bath containing a suspension of tungsten and silicon powders. These coatings were obtained at galvanostatic conditions, at the current density of j_dep = − 0.100 A cm^− 2 and at the temperature of 338 K. For determination of the influence of phase composition and surface morphology of these coatings on changes in the corrosion resistance, these coatings were modified in an argon atmosphere by thermal treatment at 1373 K during 1 h. A scanning electron microscope was used for surface morphology characterization of the coatings. The chemical composition of the coatings was determined by EDS and phase composition investigations were conducted by X-ray diffraction. It was found that the as-deposited coatings consist of a three-phase structure, i.e., nickel, tungsten and silicon. The phase composition for the Ni + W + Si coatings after thermal treatment is markedly different. The main peaks corresponding to Ni and W coexist with the new phases: NiW, NiWSi and a solid solution of W in Ni.Electrochemical corrosion resistance investigations were carried out in 5 M KOH, using potentiodynamic and electrochemical impedance spectroscopy (EIS) methods. On the basis of these investigations it was found that the Ni + W + Si coatings after thermal treatment are more corrosion resistant in alkaline solution than the as-deposited coatings. The reasons for this are a reduction in the amount of free nickel and tungsten, the presence of new phases (in particular polymetallic silicides), and a decrease of the active surface area of the coatings after thermal treatment.     

Carbon nanotubes doped SiO2/SiO2–PbO double layer high emissivity coating

Carbon nanotubes (CNTs) doped SiO₂/SiO₂–PbO double layer coating is prepared on Ni alloy plate by hybrid SiO₂ sol-gel method and SiO₂–PbO powders with certain heat treatment. The SiO₂–PbO top layer is observed to possess a kind of porous and skeleton-like structure. The emissivity enhancement mechanisms of the coating's structure and doping carbon nanotubes are investigated in this study. Spectral emissivity measurements from 1.28 to 25 μm at 570 and 820 K show that the carbon nanotubes doped SiO₂/SiO₂–PbO double layer coating possesses strong blackbody character and the coating's emissivity can reach as high as 0.94 at 820 K.     

Comparison of high temperature wear behaviour of plasma sprayed WC–Co coated and hard chromium plated AISI 304 austenitic stainless steel

The wear behaviour of plasma sprayed coating and hard chrome plating on AISI 304 austenitic stainless steel substrate is experimentally investigated in unlubricated conditions. Experiments were conducted at different temperatures (room temp, 100 °C, 200 °C and 300 °C) with 50 N load and 1 m/s sliding velocity. Wear tests were carried out by dry sliding contact of EN-24 medium carbon steel pin as counterpart on a pin-on-disc wear testing machine. In both coatings, specimens were characterised by hardness, microstructure, coating density and sliding wear resistance. Wear studies showed that the hard chromium coating exhibited improved tribological performance than that of the plasma sprayed WC–Co coating. X-ray diffraction analysis (XRD) of the coatings showed that the better wear resistance at high temperature has been attributed to the formation of a protective oxide layer at the surface during sliding. The wear mechanisms were investigated through scanning electron microscopy (SEM) and XRD. It was observed that the chromium coating provided higher hardness, good adhesion with the substrate and nearly five times the wear resistance than that obtained by uncoated AISI 304 austenitic stainless steel.     

18.6 K single-stage high frequency multi-bypass coaxial pulse tube cryocooler

A single-stage high frequency multi-bypass coaxial pulse tube cryocooler (PTC) has been developed for physical experiments. The performance characteristics are presented. At present, the cooler has reached the lowest temperature of 18.6 K with an electric input power of 268 W, which is the reported lowest temperature for single-stage high frequency PTC. The cooler typically provides 0.2 W at 20.6 K and 0.5 W at 24.1 K with the input power of 260 W at 300 K ambient temperature. The cooperation phase adjustment method of multi-bypass and double-inlet shows its advantages in experiments, they might be the best way to get temperature below 20 K for single-stage high frequency PTC. The temperature stability of the developed PTC is also observed.     

Microstructure and gas-surface interaction studies of a low-density carbon-bonded carbon fiber composite in atmospheric entry plasmas

Carbon-bonded carbon fiber (CBCF) composites are a cost-effective solution for the production of low-density carbon-phenolic Thermal Protection Systems (TPS). This new TPS for spacecraft requires new experimental data for model development and validation. Ablation experiments of a CBCF composite were carried out in an inductively-coupled plasma generator to assess the performance in high-enthalpy flows. Surface temperatures up to 2900 K led to strong surface ablation and test samples of hemispherical shape responded with constant surface temperatures and recession rates. Cylindrical samples experienced a continuous surface temperature increase. Emission spectra of the cyano radical CN were indicative of a 4–5 mm reactive boundary layer. Deviation from thermal equilibrium was found by comparison to simulated spectra. Micrographs revealed an oxidation zone in the order of 0.2 mm at the surface, suggesting a gas phase diffusion controlled ablation regime. Strong corrosion of the fibers in nitrogen plasma is attributed to wall nitridation.     

Effects of high temperature treatment on microstructure and mechanical properties of laser-clad NiCrBSi/WC coatings on titanium alloy substrate

Laser-clad composite coatings on the Ti6Al4V substrate were heat-treated at 700, 800, and 900 °C for 1 h. The effects of post-heat treatment on the microstructure, microhardness, and fracture toughness of the coatings were investigated by scanning electron microscopy, X-ray diffractometry, energy dispersive spectroscopy, and optical microscopy. The wear resistance of the coatings was evaluated under dry reciprocating sliding friction at room temperature. The coatings mainly comprised some coarse gray blocky (W,Ti)C particles accompanied by the fine white WC particles, a large number of black TiC cellular/dendrites, and the matrix composed of NiTi and Ni₃Ti; some unknown rich Ni- and Ti-rich particles with sizes ranging from 10 nm to 50 nm were precipitated and uniformly distributed in the Ni₃Ti phase to form a thin granular layer after heat treatment at 700 °C. The granular layer spread from the edge toward the center of the Ni₃Ti phase with increasing temperature. A large number of fine equiaxed Cr₂₃C₆ particles with 0.2–0.5 μm sizes were observed around the edges of the NiTi supersaturated solid solution when the temperature was further increased to 900 °C. The microhardness and fracture toughness of the coatings were improved with increased temperature due to the dispersion-strengthening effect of the precipitates. Dominant wear mechanisms for all the coatings included abrasive and delamination wear. The post-heat treatment not only reduced wear volume and friction coefficient, but also decreased cracking susceptibility during sliding friction. Comparatively speaking, the heat-treated coating at 900 °C presented the most excellent wear resistance.     

Surface microstructure and cell biocompatibility of silicon-substituted hydroxyapatite coating on titanium substrate prepared by a biomimetic process

Silicon-substituted hydroxyapatite (Si-HA) coatings with 0.14 to 1.14 at.% Si on pure titanium were prepared by a biomimetic process. The microstructure characterization and the cell compatibility of the Si-HA coatings were studied in comparison with that of hydroxyapatite (HA) coating prepared in the same way. The prepared Si-HA coatings and HA coating were only partially crystallized or in nano-scaled crystals. The introduction of Si element in HA significantly reduced P and Ca content, but densified the coating. The atom ratio of Ca to (P + Si) in the Si-HA coatings was in a range of 1.61–1.73, increasing slightly with an increase in the Si content. FTIR results displayed that Si entered HA in a form of SiO₄ unit by substituting for PO₄ unit. The cell attachment test showed that the HA and Si-HA coatings exhibited better cell response than the uncoated titanium, but no difference was observed in the cell response between the HA coating and the Si-HA coatings. Both the HA coating and the Si-HA coatings demonstrated a significantly higher cell growth rate than the uncoated pure titanium (p < 0.05) in all incubation periods while the Si-HA coating exhibited a significantly higher cell growth rate than the HA coating (p < 0.05). Si-HA with 0.42 at.% Si presented the best cell biocompatibility in all of the incubation periods. It was suggested that the synthesis mode of HA and Si-HA coatings in a simulated body environment in the biomimetic process contribute significantly to good cell biocompatibility.     

Alumina shunt for precooling a cryogen-free 4He or 3He refrigerator

In this technical report a cryogen-free 1 K cryostat is described where the pot of the ⁴He refrigeration unit is precooled by the 2nd stage of a pulse tube cryocooler (PTC) from room temperature to T ∼ 3 K via a shunt made from sintered alumina (SA); the total mass of the 1 K stage is 3.5 kg. SA has high thermal conductivity at high temperatures; but below ∼50 K the thermal conductivity drops rapidly, almost following a T³-law. This makes SA an interesting candidate for the construction of a thermal shunt, especially as the heat capacity of metals drops by several orders of magnitude in the temperature range from 300 K to 3 K. At the base temperature of the PTC, the heat conduction of the shunt is so small that the heat leak into the 1 K stage is negligible.     

Thermal conductivity of Cu/diamond composites prepared by a new pretreatment of diamond powder

Cu/diamond composites were fabricated by spark plasma sintering (SPS) after the surface pretreatment of the diamond powders, in which the diamond particles were mixed with copper powder and tungsten powder (carbide forming element W). The effects of the pretreatment temperature and the diamond particle size on the thermal conductivity of diamond/copper composites were investigated. It was found that when 300 μm diamond particles and Cu–5 wt.% W were mixed and preheated at 1313 K, the composites has a relatively higher density and its thermal conductivity approaches 672 W (m K)⁻¹.     

Microstructure and corrosion behavior of Ti nanoparticles reinforced Ni–Ti composite coatings by electrodeposition

A survey on electrochemical codeposition of Ti nanoparticles in Ni matrix coating is given. The influences of Ti nanoparticle loadings in electrolyte on the microstructure, microhardness and corrosion behavior of Ni–Ti coatings were investigated. The results showed that a pyramidal surface structure evolved into a spherical surface structure of the coatings with increasing Ti nanoparticle loading. The content of Ti in the Ni–Ti coatings first increased and reached the maximum value of 7.1 vol.% at the loading of 16 g/L, then decreased due to agglomeration of nanoparticles. The [2 0 0] preferred orientation gradually evolved to [1 1 1] orientation with increasing Ti nanoparticle loading. At Ti nanoparticle loading of 16 g/L, the minimum crystallite size (44 nm) and maximum microstrain (0.25%) were obtained. The microhardness of the Ni–Ti coatings was improved and obtained the maximum value at the loading of 16 g/L. The anti-corrosion behavior of the Ni–Ti coatings had increased trend with increasing Ti nanoparticle loading. The pitting corrosion and the selective dissolution of Ti nanoparticles happened in corrosion of Ni–Ti coating electrodeposited at the loading of 16 g/L in a 3.5 wt.% NaCl solution.     

Design and experimental investigation of the high efficiency 1.5 W/4.2 K pneumatic-drive G-M cryocooler

The development of a high cooling power and high efficiency 4.2 K two stage G-M cryocooler is critically important given its broad applications in low temperature superconductors, MRI, infrared detector and cryogenic electronics. A high efficiency 1.5 W/4.2 K pneumatic-drive G-M cryocooler has recently been designed and developed by ARS. The effect of expansion volume rate and operation conditions on the cooling performance has been experimentally investigated. A typical cooling performance of 1.5 W/4.2 K has been achieved, and the minimum temperature of the second stage is 2.46 K. The steady input power of the compressor at 60 Hz is 6.8 kW, while the operation speed of the rotary valve is 30 rpm. A maximum cooling power of 1.75 W/4.2 K has been obtained in test runs.     

Nanocomposite protective coatings based on Ti–N–Cr/Ni–Cr–B–Si–Fe,their structure and properties

The first results of manufacturing and investigations of a new type of nanocomposite protective coatings are presented. They were manufactured using a combination of two technologies: plasma-detonation coating deposition with the help of plasma jets and thin coating vacuum-arc deposition. We investigated structure, morphology, physical and mechanical properties of the coatings of 80–90 μm thickness, as well as defined the hardness, elastic Young modulus and their corrosion resistance in different media. Grain dimensions of the nanocomposite coatings on Ti–N–Cr base varied from 2.8 to 4 nm. The following phases and compounds formed as a result of plasma interaction with the thick coating surface were found in the coatings: Ti–N–Cr (200), (220), γ-Ni₃–Fe, a hexagonal Cr₂–Ti, Fe₃–Ni, (Fe, Ni)N and the following Ti–Ni compounds: Ti₂Ni, Ni₃Ti, Ni₄Ti, etc. We also found that the nanocomposite coating microhardness increased to H = 31.6 ± 1.1 GPa. The Young elastic modulus was determined to be E = 319 ± 27 GPa – it was derived from the loading–unloading curves. The protective coating demonstrated the increased corrosion resistance in acidic and alkaline media in comparison with that of the stainless steel substrate.     

Effects of heat treatment on the microstructure of amorphous boron carbide coating deposited on graphite substrates by chemical vapor deposition

A two-layer boron carbide coating is deposited on a graphite substrate by chemical vapor deposition from a CH₄/BCl₃/H₂ precursor mixture at a low temperature of 950 °C and a reduced pressure of 10 KPa. Coated substrates are annealed at 1600 °C, 1700 °C, 1800 °C, 1900 °C and 2000 °C in high purity argon for 2 h, respectively. Structural evolution of the coatings is explored by electron microscopy and spectroscopy. Results demonstrate that the as-deposited coating is composed of pyrolytic carbon and amorphous boron carbide. A composition gradient of B and C is induced in each deposition. After annealing, B₄C crystallites precipitate out of the amorphous boron carbide and grow to several hundreds nanometers by receiving B and C from boron-doped pyrolytic carbon. Energy-dispersive spectroscopy proves that the crystallization is controlled by element diffusion activated by high temperature annealing, after that a larger concentration gradient of B and C is induced in the coating. Quantified Raman spectrum identifies a graphitization enhancement of pyrolytic carbon. Transmission electron microscopy exhibits an epitaxial growth of B₄C at layer/layer interface of the annealed coatings. Mechanism concerning the structural evolution on the basis of the experimental results is proposed.     

Vacuum-plasma-sprayed silicon coatings for biomedical application

Silicon coating was deposited on titanium alloy substrates by vacuum plasma spraying technology. The morphologies and phase composition of the coatings were analyzed by field-emission scanning electron microscopy and X-ray diffraction. The thermal expansion coefficient of silicon coating was measured to be about 3.70 × 10⁻⁶ K⁻¹. The bond strength of coating was approximately 20.6 MPa. The density, open porosity, roughness and Young's modulus of silicon coating were also measured. The as-sprayed silicon coating was treated by deionized water at 60 °C, 80 °C and 100 °C for a period of time and soaked in simulated body fluids to evaluate its bioactivity. The results showed that the water-treated coating could induce apatite to precipitate on its surface in simulated body fluid, indicating that the bioactivity of silicon coating was improved. The increase of temperature and duration of water treatment had a positive effect on the bioactivity of silicon coatings.     

Effect of substrate surface roughening and cold spray coating on the fatigue life of AA2024 specimens

The effects of cold spray coating and substrate surface preparation on crack initiation under cyclic loading have been studied on Al2024 alloy specimens. Commercially pure (CP) aluminum feedstock powder has been deposited on Al2024-T351 samples using a cold-spray coating technique known as high velocity particle consolidation. Substrate specimens were prepared by surface grit blasting or shot peening prior to coating. The fatigue behavior of both coated and uncoated specimens was then tested under rotating bend conditions at two stress levels, 180 MPa and 210 MPa. Scanning electron microscopy was used to analyze failure surfaces and identify failure mechanisms. The results indicate that the fatigue strength was significantly improved on average, up to 50% at 180 MPa and up to 38% at 210 MPa, by the deposition of the cold-sprayed CP-Al coatings. Coated specimens first prepared by glass bead grit blasting experienced the largest average increase in fatigue life over bare specimens. The results display a strong dependency of the fatigue strength on the surface preparation and cold spray parameters.     

Initial phase hot corrosion mechanism of gas tunnel type plasma sprayed thermal barrier coatings

The hot corrosion resistance of the top layer in TBC is one of the main constructive factors which determines the lifetime of the coatings under critical operating environments. In the present study, 8 wt% yttria stabilized zirconia (8YSZ), lanthanum zirconate (La₂Zr₂O₇) and equal weight percentage of its composite (50%8YSZ + 50% La₂Zr₂O₇) coatings were prepared by using gas tunnel type plasma spray torch at optimum spraying conditions. The hot corrosion performances of the above thermal barrier coatings were examined against 40 wt%V₂O₅–60 wt%Na₂SO₄ corrosive ash at 1173 K for 5 h in open air atmosphere. After hot-corrosion testing, the coating surface was studied using a scanning electron microscope to observe the microstructure and X-ray diffraction techniques were used to identify the phase compositions. The results showed that LaVO₄ and YVO₄ are the main hot corrosion products along with the ZrO₂ phase transformation from tetragonal to monoclinic phases in La₂Zr₂O₇ and 8YSZ coatings respectively. The microstructure and phase formation mechanism of the hot corrosion products varied with each coating and among these, composition of 50%8YSZ + 50%La₂Zr₂O₇ coating exhibited least degradation against V₂O₅–Na₂SO₄ corrosive environment compared to the other coatings.     

Infrared spectrally selective low emissivity from Ge/ZnS one-dimensional heterostructure photonic crystal

Ge/ZnS one-dimensional heterostructure photonic crystal (1DHPC) was successfully prepared by alternating thin films of Ge and ZnS on the quartz substrate by using the optical coating technology. The microstructure and spectral emissivity of as-prepared 1DHPC were characterized by using scanning electron microscopy (SEM) and fourier transform infrared spectrometer (FTIR), respectively. The test result of spectral emissivity shows that the average emissivities of as-prepared Ge/ZnS 1DHPC in the atmospheric windows of 3–5 μm and 8–14 μm can be as low as 0.046 and 0.190, respectively, but the average emissivity in the non-atmospheric window of 5–8 μm can be as high as 0.579. The results indicate that the as-prepared Ge/ZnS 1DHPC has obviously infrared spectrally selective low emissivity characteristic, basically meets the requirements of our design. The as-prepared 1DHPC with infrared spectrally selective low emissivity is promising for use as a material to unify the infrared stealth and effective cooling of the aircraft.