Uniform color coating of multilayered TiO<Subscript>2</Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> films by atomic layer deposition

Thin film optics, based on light interference characteristics, are attracting increasing interest because of their ability to enable a functional color coating for various applications in optical, electronic, and solar industries. Here, we report on the dependence of coloring characteristics on single-layer TiO₂ thicknesses and alternating TiO₂/Al₂O₃ multilayer structures prepared by atomic layer deposition (ALD) at a low growth temperature. The ALD TiO₂ and Al₂O₃ thin films were studied at a low growth temperature of 80°C. Then, the coloring features in the single-layer TiO₂ and alternating TiO₂/Al₂O₃ multilayers using both the ALD processes were experimentally examined on a TiN/cut stainless steel sheet. The Essential Macleod software was used to estimate and compare the color coating results. The simulation results revealed that five different colors of the single TiO₂ layers were shown experimentally, depending on the film thickness. For the purpose of highly uniform pink color coating, the film structures of TiO₂/Al₂O₃ multilayers were designed in advance. It was experimentally demonstrated that the evaluated colors corresponded well with the simulated color spectrum results, exhibiting a uniform pink color with wide incident angles ranging from 0° to 75°. This article advances practical applications requiring highly uniform color coatings of surfaces in a variety of optical coating areas with complex topographical structures.     

Chemical vapor deposition of ZrO2 and C/ZrO2 on mullite fibers for interfaces in mullite/aluminosilicate fiber-reinforced composites

For the realization of crack deflection and fiber pull-out in aluminosilicate fiber-reinforced dense mullite-matrix composites, suitable fiber/matrix-interfaces are an important requirement in order to obtain sufficiently weak bondings between fibers and matrices. Two types of chemical vapor deposited (CVD) fiber/matrix-interfaces have been studied in the present work porous ZrO₂ and C/ZrO₂-double layers. In the latter case, carbon was burned out to form a gap during the processing of composites (fugitive coating). Porous ZrO₂ coatings were produced by an optimized CVD-process with Zr-acetylacetonate as a precursor. The constancy of the layer thickness depended on the deposition temperature. It was found that at a temperature of approximately 300°C and a pressure of 5 hPa, suitably uniform layers with thickness ranging between 100 and 300 nm were achieved. The coatings contained approximately 15 wt% carbon which produced, after annealing in air, a porous structure. The deposition kinetics can be described by a first order reaction. The carbon layer in C/ZrO₂-double layers was produced by using propane. The thickness of carbon layer was 10 and 100 nm, respectively. Aluminosilicate fiber/mullite matrix composite prepegs were fabricated by infiltration of coated and unidirectionally oriented fiber (0°) with a slurry, containing a pre-mullite powder, calcined at 1100°C. Uniaxial hot-pressing of dried prepegs was carried out at <1250°C for 15 min, at 20 MPa. Prepegs with ZrO₂ fiber/matrix-interfaces were hot-pressed in air, while the samples with C/ZrO₂-interfaces were processed in flowing argon. After hot-pressing, samples with C/ZrO₂-interfaces were heat-treated in air (1000°C) in order to burn out the C-layer (fugitive coating). These composites yielded a controlled fracture with a high deflection rate and a favorable fracture strength of about 200 MPa, due to crack-deflection and fiber pull-out. Composites with ZrO₂-interfaces, on the contrary yielded no crack deflection or pull-out. Therefore, they are less damage tolerant than those having C/ZrO₂ double layer systems.     

The yttria-stabilized zirconia and interfacial coating on Nicalon™ fiber

Sols of yttria-stabilized zirconia may be used as simple, readily processable and accurate controllable precursors for the ZrO₂ interfacial coatings on SiC-based Nicalon™ fibers. The ZrO₂ interfacial coatings of predictable crystal phase compositions were obtained in dependence of yttria dopant level. The morphology, composition and oxidation resistance of coated fibers were evaluated by SEM, EDS, XPS, XRD, and Raman analysis. All coatings obtained are uniform, continuous and adherent to substrates. The delamination within the ZrO₂ interfacial coating was found. Possible reasons of this phenomenon are discussed. The peculiarities of the behavior of Y-stabilized ZrO₂-coated fibers in air at elevated temperature are considered.     

Composite ceramic coating with enhanced thermal shock resistance formed by the in-situ synthesis of nano-ZrO2

In this research, nano-ZrO₂/TiO₂ composite coatings were designed for titanium alloys by the in-situ incorporation of ZrO₂ nanoparticles into a TiO₂ ceramic coating. Precise control over the content and structure of nano-ZrO₂ in this nanocomposite coating was achieved by manipulating the pH of the electrolyte during plasma electrolytic oxidation (PEO). The synthesis process and mechanism of tetragonal zirconia (t-ZrO₂) were revealed by analyzing the phase composition and microstructure of the coating. The influence of pH on the formation of t-ZrO₂ was also revealed. By detecting changes in the electrolyte solute composition before and after PEO, the Zr(OH)₄ precursor was determined to be the source of the t-ZrO₂ nanoparticles in the composite coating. The yield of t-ZrO₂ in the composite coating increased upon increasing the pH of the electrolyte. Moreover, the thermal shock tests showed that increasing the t-ZrO₂ content remarkably improved the thermal resistance of the coatings. This strategy and the research outcomes are expected to have great significance for developing advanced nanocomposite coatings on titanium alloys with enhanced thermal shock resistance.     

Uniform coating of TiO2 nanoparticles using biotemplates for photocatalytic wastewater treatment

Immobilization of TiO₂ particles over substrates like glass can facilitate the separation after photocatalytic runs. Photocatalytic activity of TiO₂ coatings is related to its morphology, crystallography, optical properties and adherence of the coating. Biotemplates, including animal-based and herbal-based templates are inexpensive, biocompatible and abundant and can control the quality of TiO₂ coating. In this study the effects of biotemplates such as agar, gelatin, and starch on the physiochemical properties of TiO₂ coatings were investigated. Synthesized coatings were characterized by XRD, BET, FESEM, TEM, FTIR, EDX, and UV-Vis DRS analyses. The results showed that using biotemplates reduces the TiO₂ crystallite size. Template-free TiO₂ had 30 nm crystallite size, but using templates like agar decreased the size to 18 nm. Moreover, the addition of biotemplates decreased the thickness of TiO₂ coatings compared to template free coating. And the use of biotemplates also limits the pore size distribution and increases BET surface area. According to EDX, TiO₂ coating with agar indicated a uniform Ti distribution and crack-free homogenous morphology. TEM analysis of agar-templated TiO₂ film showed a uniform morphology of TiO₂ particles with average particle size of 20 nm. The UV-Vis DRS also confirmed a reduction in the band gap of TiO₂ after the introduction of biotemplates. The study of the photocatalytic performance of samples showed that agar-templated TiO₂ coating was able to remove 62.4% of methylene blue, while the coatings synthesized with gelatin and starch were just able to remove 42.77% and 35%, respectively. The TiO₂ coating with agar was studied at different pH values and different initial methylene blue concentrations as well. The stability test of agar-templated TiO₂ coating after four runs indicated just 5% of activity lost.     

Abrasion resistance of ceramic thin films of ZrO2/SiO2 on stretched grade polymethyl methacrylate substrates

Abrasion resistance of stretched grade polymethyl methacrylate (PMMA) was increased by using the sol–gel method to have it coated with a ZrO₂/SiO₂ thin film. Different molar ratios of Zr(OPr)₄/Si(OPr)₄ sols were prepared as precursors with propanol. These sols were used for dip-coating the stretched PMMA surfaces to establish very smooth thin films of amorphous Zr–O–Si. Fourier Transform Infrared spectroscopy (FT-IR) was employed to study vibrations of Zr–O–Si bonds within the thin film. The phase analysis was undertaken via X-ray Diffraction (XRD) method. The morphology and thickness of coatings on PMMA were investigated by means of Scanning Electron Microscopy (SEM). The results showed that coating had an amorphous structure with its thickness within the range of 80–100 nm. The water contact angle of PMMA substrates altered from 73° before coating to less than 64° after coating. Once coated, the PMMA substrate had its transparency characteristic (within the UV–vis region) increased. Furthermore, the influences of thermal treatment temperature and molar ratio of precursors (Zr(OPr)₄/Si(OPr)₄) on abrasion resistance of the coatings were studied.     

Study on thermal shock resistance of Sc2O3 and Y2O3 co-stabilized ZrO2 thermal barrier coatings

In order to reveal the effect of Sc₂O₃ and Y₂O₃ co-doping system on the thermal shock resistance of ZrO₂ thermal barrier coatings, Y₂O₃ stabilized ZrO₂ thermal barrier coatings (YSZ TBCs) and Sc₂O₃–Y₂O₃ co-stabilized ZrO₂ thermal barrier coatings (ScYSZ TBCs) were prepared by atmospheric plasma spraying technology. The surface and cross-section micromorphologies of YSZ ceramic coating and ScYSZ ceramic coatings were compared, and their phase composition before and after heat treatment at 1200 °C was analyzed. Whereupon, the thermal shock experiment of the two TBCs at 1100 °C was carried out. The results show that the micromorphologies of YSZ ceramic coating and ScYSZ ceramic coating were not much different, but the porosity of the latter was slightly higher. Before heat treatment, the phase composition of both YSZ ceramic coating and ScYSZ ceramic coating was a single T′ phase. After heat treatment, the phase composition of YSZ ceramic coating was a mixture of M phase, T phase, and C phase, while that of ScYSZ ceramic coating was still a single T′ phase, indicating ScYSZ ceramic coating had better T′ phase stability, which could be attributed to the co-doping system of Sc₂O₃ and Y₂O₃ facilitated the formation of defect clusters. In the thermal shock experiment, the thermal shock life of YSZ TBCs was 310 times, while that of ScYSZ TBCs was 370 times, indicating the latter had better thermal shock resistance. The difference in thermal shock resistance could be attributed to the different sintering resistance of ceramic coatings and the different growth rates of thermally grown oxide in the two TBCs. Furthermore, the thermal shock failure modes of YSZ TBCs and ScYSZ TBCs were different, the former was delamination, while the latter was delamination and shallow spallation.     

Incorporation of ZnO–ZrO2 nanoparticles into TiO2 coatings obtained by PEO on Ti–6Al–4V substrate and evaluation of its corrosion behavior,microstructural and antibacterial effects exposed to SBF solution

In this research, Plasma Electrolytic Oxidation technique was used to incorporate ZnO–ZrO₂ nanoparticles into TiO₂ ceramic coating on Ti6–Al–4V using sodium phosphate as an electrolyte. The effect of adding these nanoparticles on corrosion, morphology, wettability and antibacterial properties in the simulated body fluid (SBF) solution was investigated. The results indicated nanoparticles modified the microstructure of coating, which increased corrosion resistance 12 times higher than that of substrate. Besides, ZrO₂ nanoparticles had the most significant effect on increasing the contact angle. In addition, due to the compatibility of zirconium and zinc oxides with human body environment, the antibacterial properties of coatings were significantly improved.     

Corrosion behavior of titania films coated by liquid‐phase deposition on AISI304 stainless steel substrates

Fouling deposition and localized corrosion on the heat‐transfer surfaces of the stainless steel equipments often simultaneously exist, which can introduce additional thermal resistance to heat‐transfer and damage heat‐transfer surfaces. It is a good anticorrosion way to coat a barrier layer of certain materials on the metal surface. In this article, the TiO₂ coatings with nanoscale thicknesses were obtained by liquid‐phase deposition method on the substrates of AISI304 stainless steel (ASS). The coating thickness, surface roughness, surface morphology, crystal phase, and chemical element were characterized with the film thickness measuring instrument, roughmeter, atomic force microscopy, field emission scanning electron microscopy, X‐ray diffraction, and energy‐dispersive X‐ray spectroscopy analyzer, respectively. Corrosion behavior of the TiO₂ coatings was evaluated by potentiodynamic polarization, cyclic voltammograms scanning, and electrochemical impedance spectroscopy tests with the mixed corrosion solution composed of 3.5 wt. % NaCl and 0.05 M NaOH. It is shown that the TiO₂ coating is composed of the nanoparticles with smooth, crack‐free, dense, and uniform surface topography; the roughness of coating surface increases slightly compared with that of the polished ASS substrate. The anatase‐phase TiO₂ coatings are obtained when sintering temperature being varied from 573.15 to 923.15 K and exhibit better anticorrosion behavior compared with ASS surfaces. The corrosion current density decreases and the polarization resistance increases with the increase of the coating thickness. The corrosion resistance of the TiO₂ coatings deteriorates with the increase of the corrosion time. The capacitance and the resistance of the corrosion product layer between the interface of the ASS substrate and the TiO₂ coating are found after the corrosion time of 240 h. A corrosion model was introduced, and a possible new explanation on the anticorrosion mechanisms of the TiO₂ coating was also analyzed. The corrosion mechanism of the TiO₂ coating might comply with the multistage corrosion process. © 2011 American Institute of Chemical Engineers AIChE J, 58: 1907–1920, 2012     

TiO2/ZnO double-layer broadband antireflective and down-shifting coatings for solar applications

Making full use of sunlight in solar cells requires reducing the reflection of light and minimizing spectral mismatch. Here, a TiO₂/ZnO double-layer coating with both wider band antireflection and down-shifting performance was prepared. TiO₂ sols and ZnO nanoparticles were synthesized via the sol-gel method and then successively coated on the surface of the Si substrate by dip-coating. Computational simulations were used to obtain the optimal refractive index and thickness of the coatings. In the experiments, the thicknesses of the TiO₂ and ZnO coatings were adjusted by changing the lifting speed, and the refractive index of the TiO₂ and ZnO coatings were adjusted by adding the porosity inducing agent and varying the concentration of the solution. The TiO₂/ZnO coating reduces the reflectivity of the silicon substrate by 24.97% in the 400–1100 nm band, and the ZnO nanoparticles can convert light at approximately 345 nm–527 nm, reducing the spectral mismatch of the solar cell. The photocurrent of solar cells coated with TiO₂/ZnO coatings was markedly improved, with an increase of 29% in the average photocurrent at 300–800 nm. Herein, TiO₂/ZnO coatings have the potential to benefit the development of multifunctional coatings that are important for improving the efficiency of solar cells.     

The comparative study of photocatalytic self‐cleaning properties of synthesized nanoscale titania and zirconia onto polyacrylonitrile fibers

The photocatalytic activity of TiO₂ and ZrO₂‐coated polyacrylonitrile (PAN) fibers was compared through the self‐cleaning of methylene blue and eosin yellowish. TiO₂ and ZrO₂ nanocrystals were successfully synthesized and deposited onto PAN fibers with photocatalytic self‐cleaning activity using the sol‐gel process at low temperature. The pristine and treated samples have been characterized by several techniques, such as scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, diffuse reflectance spectroscopy, X‐ray diffraction, and thermogravimetric analysis. The TiO₂ nanoparticles with 10–20 nm in size, and ZrO₂ with 20–40 nm have been synthesized to form dispersed particles on the fiber surface, which shows photocatalytic properties when exposed to UV–Vis light. The photocatalytic activity, tested by measuring the degradation of adsorbed methylene blue and Eosin Y. Photocatalytic activity of TiO₂‐coated fibers toward dyes degradation was higher than that of ZrO₂‐coated fibers. This preparation technique can be also applied to new fabrics to create self‐cleaning and UV irradiation protection properties in them. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Low–thermal–conductivity and high–toughness CeO2–Gd2O3 co–stabilized zirconia ceramic for potential thermal barrier coating applications

Yttria partially stabilized zirconia (～4.0?mol% Y₂O₃–ZrO₂, 4YSZ) has been widely employed as thermal barrier coatings (TBCs) to protect the high–temperature components of gas–turbine engines. The phase stability problem existing in the conventional 4YSZ has limited it to application below 1200?°C. Here we report an excellent zirconia system co–doped with 16?mol% CeO₂ and 4?mol% Gd₂O₃ (16Ce–4Gd) presenting nontransformable feature up to 1500?°C, in which no detrimental monoclinic (m) ZrO₂ phase formed on partitioning. It also exhibits a high fracture toughness of ～46?J m^?2 and shows high sintering resistance. Besides, the thermal conductivity and thermal expansion coefficient of 16Ce–4Gd are more competent for TBCs applications as compared to the 4YSZ. The combination of properties suggests that the 16Ce–4Gd system could be of potential use as a thermal barrier coating at 1500?°C.     

Ablation behavior of C/SiC with YSZ and ZrB2 coatings under high-energy laser irradiation

Carbon fiber-reinforced silicon carbide (C/SiC) composites are important candidates for laser protection materials. In this study, ablation mechanism of C/SiC coated with ZrO₂/Mo and ZrB₂–SiC/ZrO₂/Mo under laser irradiation was studied. ZrB₂–SiC multiphase ceramic and ZrO₂ ceramic were successfully coated on C/SiC composite by atmospheric plasma spraying technology with Mo as transition layer. Phase evolution and morphology of composite were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Moreover, ablation behavior of the composite was investigated by laser confocal microscopy. Results showed that ablation mechanism of C/SiC composite was controlled by phase transformation, thermal reaction, and thermal diffusion, with solid–liquid transition of ZrB₂ and ZrO₂ being dominant factor. Endothermic reaction and good thermal diffusivity of coatings were also important factors affecting ablation performance. Reflectivity effect of ZrO₂ coating was limited under high-energy laser irradiation. Compared with ZrO₂/Mo single-phase-monolayer coating, designed ZrB₂–SiC/ZrO₂/Mo coating showed better ablation performance, and breakdown time of C/SiC increased from 10 to 40 s. The depletion of liquid phase in molten pool was identified as an important factor responsible for rapid failure of C/SiC. The coating failed when the entire liquid phase was consumed within molten pool, followed by rapid damage of C/SiC substrate. Results of this study can provide theoretical guidance and research ideas for design and application of laser protective materials.     

Nano- and micrometre additions of SiO2, ZrO2 and TiO2 in fine grained alumina refractory ceramics for improved thermal shock performance

The present contribution investigates the influence of micro-metre- as well as nano-metre-additions of zirconia (ZrO₂), titania (TiO₂), silica (SiO₂) and magnesia (MgO) into alumina-rich fine grained ceramic materials for refractory applications. Slip casted samples in the system alumina–zirconia–titania (AZT), alumina–zirconia–titania–silica (AZTS) and alumina–zirconia–titania–magnesia (AZTM) were sintered and the physical as well as mechanical properties were investigated as fired and after thermal shock treatments. The generation of a micro-crack network after sintering due to the formation of phases with different thermal expansion coefficients and the formation and decomposition of aluminium titanate (Al₂TiO₅) before and after thermal shock exposure leads to higher strengths after thermal shock attack.     

Preparation and antibacterial activity of Ag/TiO2-functionalized ceramic tiles

An Ag/TiO₂ coating was deposited onto glazed ceramic tiles by a sol-gel and spraying method at high temperatures. The coating was characterized by X-ray diffraction, scanning electron microscopy, and atomic force microscopy. The results showed that silver was present in rutile-TiO₂, and the temperature did not change the phase composition of the samples. The Ag/TiO₂ coating had a higher roughness than the TiO₂ coating. The tape test (D 3359–08) showed that the coatings prepared at 950 °C and 1000 °C had good adhesion to the ceramic tile substrate. The antibacterial activity of the coating was tested by photocatalytic sterilization experiments. The results showed that the Ag/TiO₂ coating had a higher antibacterial activity than the TiO₂ coating, and the sterilization efficiency of Escherichia coli, Staphylococcus aureus, Shigella, and Salmonella exceeded 99.655% under 2 h of visible light irradiation. This research provides a method to create Ag/TiO₂ coatings with good thermal resistance, adhesion, and antibacterial activity. This improves the low photocatalytic activity caused by the anatase-to-rutile transformation of TiO₂ at high temperatures and the poor adhesion at low temperatures.     

Preparation and heat-insulating property of the bio-inspired ZrO2 fibers based on the silk template

Natural silk fibers were used as the template to prepare biomorphic ZrO₂ fibers. Silk fibers were first immersed into a Zr(NO₃)₄ solution and then sintered in air at high temperatures to produce the final ZrO₂ fibers. Their microstructures, phases, synthesis process, infrared absorption spectra and thermal conductivity were analyzed. The results show that these synthesized fibers retained the morphologies of silk faithfully. These ZrO₂ fibers also obtained the ability of absorbing infrared from the silk, so that they possessed better heat-insulating property than the traditional ZrO₂ fibers.     

Alkali resistance,microstructural and mechanical performance of zirconia-coated basalt fibers

Sol–gel approach was developed to apply zirconia coatings on basalt fibers. Dense or porous ZrO₂ coatings were obtained, depending on the process parameters. The alkali resistance of uncoated and ZrO₂-coated basalt fibers in alkali solution was studied. The morphology, elemental and phase composition of etched fibers as a function of etching time were studied by means of a set of analytical methods. A scheme of etching of as-received and coated basalt fiber was proposed. Zirconia coating slows down the corrosion of basalt fiber in alkali solution. The denser zirconia coating slows down the corrosion to a higher extent than the porous coating. The uncoated and coated basalt fibers were tested in mini composites with cement matrix. It was shown that the surface of the coated fiber is affected by the alkaline medium of the cement matrix to a smaller extent than the surface of as-received basalt fiber.     

High emissivity MoSi2–ZrO2–borosilicate glass multiphase coating with SiB6 addition for fibrous ZrO2 ceramic

To develop a high emissivity coating on the low thermal conductivity ZrO₂ ceramic insulation for reusable thermal protective system, the MoSi₂–ZrO₂–borosilicate glass multiphase coatings with SiB₆ addition were designed and prepared with slurry dipping and subsequent sintering method. The influence of SiB₆ content on the microstructure, radiative property and thermal shock behavior of the coatings has been investigated. The coating prepared with SiB₆ included the top dense glass layer, the surface porous coating layer and the interfacial transition layer, forming a gradient structure and exhibiting superior compatibility and adherence with the substrate. The emissivity of the coating with 3 wt% SiB₆ addition was up to 0.8 in the range of 0.3–2.5 μm and 0.85 in the range of 0.8–2.5 μm at room temperature, and the “V-shaped grooves” surface roughness morphology had a positive effect on the emissivity. The MZB-3S coating showed excellent thermal shock resistance with only 1.81% weight loss after 10 thermal cycles between 1773 K and room temperature, which was attributed to the synergistic effect of porous gradient structure, self-sealing property of oxidized SiB₆ and the match of thermal expansion coefficient between the coating and substrate. Thus, the high emissivity MoSi₂–ZrO₂–borosilicate glass coating with high temperature resistance presented a promising potential for application in thermal insulation materials.     

Modified thick thermal barrier coatings: microstructural characterization

Thick thermal barrier coatings were modified with laser glazing and phosphate based sealing treatments. Surface porosity of the sealed coatings decreased significantly in all cases. Structural analysis showed a strong preferred crystal orientation of the t′ZrO₂ phase in direction [002] in laser-glazed 25CeO₂–2.5Y₂O₃–ZrO₂ coating. In laser-glazed 22MgO–ZrO₂ coating the major phase was rhombohedral Mg₂Zr₅O₁₂. In phosphate sealed 8Y₂O₃–ZrO₂ coating the strengthening mechanism was identified as adhesive binding without chemical bonding. Coating microstructures were determined by scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy and optical microscopy. Coatings were also characterized by X-ray diffraction, microhardness and porosity.     

Fabrication of lightweight ZrO2 fiberboards using hollow ZrO2 fibers

ZrO₂ fiberboards with ultra-low densities (0.34–0.40 g/cm³) were fabricated using biomorphic ZrO₂ hollow fibers, which have a lower density and better thermal insulation than traditional ZrO₂ solid fibers. The effects of sol binder content, sintering temperature, and proportion of solid fibers on the density, microstructure, compressive strength, linear shrinkage, and thermal conductivity of lightweight ZrO₂ fiberboards were investigated. The results showed that the hollow features of biomorphic ZrO₂ fibers were successfully maintained after they were made into ZrO₂ fiberboards, which made them less dense and thermally conductive. The best conditions were found to be a sol binder content of 30 vol%, sintering temperature of 1400 °C, and 20 wt% sintered solid fibers to balance thermal insulation and compressive strength. The results show that the density and thermal conductivity of lightweight ZrO₂ fiberboard gives it obvious advantages as a heat-insulating ceramic. Specifically, when the sintering temperature was 1400 °C, the sample had an ultra-low density of 0.34–0.40 g/cm³, a thermal conductivity of 0.101–0.116 W/(m·K) (at 500 °C), a compressive strength of 0.05–0.24 MPa, and a linear shrinkage of 9.4–13%.