Effect of soda-lime glass on sintering and technological properties of porcelain stoneware tiles

The feasibility of waste glass recycling in ceramic tile production was assessed with special reference to fully vitrified products (porcelain stoneware). Soda-lime float or container glass was introduced, in replacement of sodic feldspar, in typical porcelain stoneware bodies (up to 10 wt.%) that underwent a laboratory simulation of tilemaking process, with a technological and compositional characterization of both fired and unfired tiles. Soda-lime glass had no significant effect on semi-finished products, but it influenced remarkably the firing behaviour, increasing shrinkage and closed porosity, decreasing open porosity and bulk density, and lowering mechanical and tribological performances. Waste glass promotes a more effective melting of quartz and a partial dissolution of mullite, leading to a more abundant and less viscous liquid phase, which accelerates the sintering kinetics. In conclusion, soda-lime glass can be used in small amounts (5% or less) with tolerable modifications of technological behaviour and performances of porcelain stoneware tiles.     

一种碱性玻璃腐蚀工艺的研究

本文针对光学玻璃镀膜工艺对表面粗糙度的要求,提出有异于传统玻璃腐蚀方法的一种新工艺,将玻璃在腐蚀溶液中浸泡24h后再进行超声处理,超声频率53kHz,超声时间40m in,超声温度60℃。经过该工艺处理后的玻璃,表面粗糙度大大提高,在后续的镀膜工艺中,能有效提高膜层和玻璃基板之间的附着力,从而改善玻璃作为光学显示器的各...     

Effect of normal scratch load and HF etching on the mechanical behavior of annealed and chemically strengthened aluminosilicate glass

Micro-cracks generated by hard body scratch are a major cause of strength decrease for silicate glass. The influence of normal scratch load on the cracking patterns and flexural strength of annealed glass (AG) and chemically strengthened glass (CSG) were studied. With the increase of the normal load, the load capacity of scratched AG specimens decreased to about 40 MPa at 20gf immediately. However, the residual strength of CSG decreased to a steady value of 145 MPa as the scratch load increased to 500gf. Then the effect of hydrofluoric acid (HF) etching on the surface morphology and mechanical properties of the 500gf scratched glass were investigated. After 8min (for CSG) and 16 min (for AG) acid treatment, the flexural strength of CSG and AG increased to a considerable value of 900 MPa, which is 3.6 and 5.5 times higher than the flexural strength of undamaged specimens. Microscopic observations show that the blunting and eliminating of median cracks as well as the formation of new surfaces are the main causes of strength enhancement.     

Physicochemical surface characterizations of four dental CAD/CAM lithium disilicate-based glass ceramics on HF etching: An XPS study

The surfaces of four lithium disilicate glass ceramics (LDGC) were characterized at the nanolevel. The goal was to detect the chemical alteration of the surface on etching with hydrofluoric acid (HF). The four LDGC tested were Celtra Duo, IPS e.max CAD, Straumann n!ce and Vita Suprinity. Four blocks of each LDGC were sectioned to ∼ 1 mm thicknesses. The requirement for firing, or not, was carried out following the manufacturer’s recommendations. The samples were then divided into two groups: a control and an etched group. Etching was carried out using a solution of 5% HF for 20 s, rinsed for 20 s and dried for 10 s, using an air jet. The atomic percentages of the first atomic layers were probed using X-ray photoelectron spectroscopy (XPS) in the survey mode (n = 12). The oxygen and silicon peaks (O1s and Si2p) were then analyzed in the high resolution mode. The samples were also characterized using scanning electronic microscopy at high magnification (60 k). XPS showed the amounts of the major elements, Si, O and Li, were changed on etching. For all samples, trace elements, such as P, Zn, Y, Na and Sr, disappeared on glassy phase dissolution. Zr and Al percentages varied, based on the LDGC analyzed. High resolution spectra of the O1s and Si2p peaks showed that the chemical environments were qualitatively different in all samples. Acid etching, using 5% HF for 20 s, modified not only the topographic structure, but also the chemical composition of the LDGC surface.     

Laser Zone Melting and microstructure of waveguide coatings obtained on soda-lime glass

This study presents a Laser Zone Melting method with potential for producing planar waveguides at large scale, based on the surface coupling of two chemically compatible glass layers which exhibit distinct indices of refraction. The method is based on a recent patent, particularly applicable to process glass and ceramics with low thermal shock resistance. Glass coatings containing 76.24% by weight PbO are thus here reported, as obtained by this method on commercial soda-lime planar glass substrates. Their higher indices of refraction (1.58 vs 1.52 for commercial soda-lime glass) result in attractive waveguiding potential, as demonstrated with measurements using focused light from a He-Ne laser beam. Scanning and transmission electron microscopy studies reveal excellent integration and compatibility between the observed coatings and substrates, where diffusion in the proximity of the interface was studied by EDS analysis. Crystalline phases have not been found within the coating, or within the substrate, as concluded from the absence of Bragg-peaks in XRD experiments.     

Photoluminescence properties of porous silicon layers prepared by electrochemical etching in extremely dilute HF solutions

Dilute HF solutions with concentrations down to 0.03% have been used to obtain luminescent porous silicon (PSi) layers on p-type Si wafers. The experimental results show that with a constant etching time of 30 min, PSi layers with sufficient luminescence efficiencies can be formed for HF concentrations as low as 0.1%. Because of a significantly lowered critical current density, only very low etching current densities of  ≤0.1 mA cm⁻² can result in the formation of luminescent PSi samples in 0.1% HF solutions. A notable result is that these low etching current densities cannot be used to form luminescent PSi layers in concentrated ( ≥1%) HF solutions. The behavior of PL intensity as a function of etching current density has been analyzed over a wide range of HF concentration. The PL intensity is determined by the ratio of the etching current density to the critical current density, suggesting that the presence of silicon oxides plays an important role in the formation of luminescent Si nanostructures in PSi layers.     

Polymer-derived SiOC aerogel with hierarchical porosity through HF etching

Silicon oxycarbide (SiOC) aerogels have been synthesized from preceramic polymers via pyrolysis in inert atmosphere at 1200 and 1300 °C. The as synthesized materials have a typical colloidal microstructure with mesoporosity in the range 10–50 nm and no microporosity. HF acid attack of the SiOC aerogels dissolves preferentially the SiO₂-rich phase and creates micro-and (small)mesopores (<10 nm) in the aerogels microstructure finally leading to a materials with hierarchical porosity. The HF post-pyrolysis treatment is more efficient for the SiOC aerogels pyrolyzed at the maximum temperature, i.e. 1300 °C, leading to a maximum value of specific surface area of 530 m²/g and total porosity of 0.649 cc/g.     

Effects of acid leaching treatment of soda-lime silicate glass on crack initiation and fracture

Water or acid soaking surface treatments have been shown to increase the mechanical strength of soda-lime silicate (SLS) glasses. This increase in strength has traditionally been attributed to effects related to residual stress or changes in fracture resistance. In this work, we report experimental data that cannot be explained based on the existing knowledge of glass surface mechanics. In dry environments, annealed and acid-leached SLS surfaces have comparable crack initiation stress and fracture stress as measured by Hertzian indentation and biaxial bending tests, respectively. Yet, in the presence of humidity, acid-leached surfaces have higher failure stress than the annealed surfaces. This apparent enhancement in the crack resistance of the acid-leached surface of SLS glass in humid environments supports the hypothesis that acid-leached surface chemistry can lower the transport kinetics of molecular water to critical flaws.     

Surface and subsurface alterations in freshly fractured and corroded soda-lime float glass

We have investigated the corrosion behavior of the soda-lime silicate float glass on freshly created active surfaces. The process of ion diffusion and ion exchange during surface corrosion is explained at the initial stages. We have reported a unique subsurface activity in the glass, which achieves equilibrium. This varies at the subsurface depth level of ≈ 10–30 nm and is visible as a broad peak in the elemental depth profile. The prolonged corrosion and heating process assists surface relaxation of the glass samples. We have observed the formation of active nucleation sites for the corrosion process on the surface. In this study, we report that the sodium ions and its corrosion compounds are decoupled from other metal ions present in the glass during diffusion relaxation and ion exchange. A combination of time of flight secondary ion mass spectrometry (TOF-SIMS) and energy dispersive X-ray (EDX) microanalysis help to explain the evolution and quantify the changes at the initial stages in the freshly formed glass surface.     

Antireflective grassy surface on glass substrates with self-masked dry etching

Although recently developed bio-inspired nanostructures exhibit superior optic performance, their practical applications are limited due to cost issues. We present highly transparent glasses with grassy surface fabricated with self-masked dry etch process. Simultaneously generated nanoclusters during reactive ion etch process with simple gas mixture (i.e., CF₄/O₂) enables lithography-free, one-step nanostructure fabrication. The resulting grassy surfaces, composed of tapered subwavelength structures, exhibit antireflective (AR) properties in 300 to 1,800-nm wavelength ranges as well as improved hydrophilicity for antifogging. Rigorous coupled-wave analysis calculation provides design guidelines for AR surface on glass substrates.     

The dual role of silver during silicon etching in HF solution

ABSTRACT: It was reported that during silicon etching, silver was subjected to have a controversial role. Some researchers debate that silver protects silicon, and, at the same time, other ones confirm that silver catalyzes silicon underneath. In this paper, we give experimental results arguing the dual role that silver has during the formation of silicon nanostructures. We give a proof that the role of silver depends on the experimental details and the intrinsic properties of silver during its deposition on the silicon wafer. Through our investigations, we tracked the silver particles that indicated which mechanism is involved. Characterizations of the prepared samples were made using a Scanning Electron Microscope (SEM).     

Effect of HF and NaOH etching on the composition and structure of SiOC ceramics

Porous SiOC ceramics were prepared with tetraethoxysilane (TEOS) and vinyltriethoxysilane (VTES) as sol?gel precursors, and followed by etching with HF and NaOH solution. The microstructure evolution and chemical etching as a function of pyrolysis temperature were investigated. The amorphous carbon increases as rising the temperature from 800 ^oC to 1200 ^oC, and the graphitic carbon increases with further etching by HF and NaOH. However, the effect of pyrolysis temperature on the structure of C is more significant. The hydroxylation reaction and phase separation of SiOC ceramics results in the increase of SiO₄ unit, which reacts with HF and NaOH to form micro- and mesopores. The existence of mesopore after HF etching provides more specific surface area and pore volume. However, NaOH etching produces more micropores, and the contribution of micropores to specific surface area and pore volume is higher than that of mesopores. Although HF and NaOH etching increase the specific surface area of SiOC ceramics, the etching effect of NaOH is superior to that of HF etching, and the carbon-enriched SiOC ceramics are obtained after NaOH etching.     

Surface properties of glass micropipettes and their effect on biological studies

In this paper, an investigation on surface properties of glass micropipettes and their effect on biological applications is reported. Pipettes were pulled under different pulling conditions and the effect of each pulling parameter was analyzed. SEM stereoscopic technique was used to reveal the surface roughness properties of pipette tip and pipette inner wall in 3D. More than 20 pipettes were reconstructed. Pipette heads were split open using focused ion beam (FIB) milling for access to the inner walls. It is found that surface roughness parameters are strongly related on the tip size. Bigger pipettes have higher average surface roughness and lower developed interfacial area ratio. Furthermore, the autocorrelation of roughness model of the inner surface shows that the inner surface does not have any tendency of orientation and is not affected by pulling direction. To investigate the effect of surface roughness properties on biological applications, patch-clamping tests were carried out by conventional and FIB-polished pipettes. The results of the experiments show that polished pipettes make significantly better seals. The results of this work are of important reference value for achieving pipettes with desired surface properties and can be used to explain biological phenomenon such as giga-seal formation.     

蒙砂粉熟化过程与蚀刻玻璃表面的研究

固体蒙砂粉的熟化质量是决定玻璃蚀刻效果的重要因素。用X射线衍射（XRD）、能谱仪（EDS）、拉曼光谱、粘度计、Zeta电位和碱滴定等方法研究了用柠檬酸和氟化氢铵为主要成分配制的蒙砂粉的理化性质随熟化时间的变化规律,考察和评价了熟化时间对GG6手机盖板玻璃蚀刻效果的影响。结果表明：熟化时间为36 h,得到的熟化液的黏度和氢离子浓度最大,GG6玻璃蚀刻后的粗糙度为265 nm、雾度为84%、透光率为92.4%、光泽度为11.7%,符合工业上手机玻璃盖板的蚀刻加工质量要求,蚀刻后的GG6玻璃表面形成一层微量的氟硅酸物晶体,构成的微纳蚀孔结构更均匀。测定蒙砂液的理化性质能有助于更好地了解蒙砂粉的熟化过程,对蒙砂粉蚀刻工艺具有指导作用,提高玻璃防眩工艺的生产效率。     

Contact residual stress relaxation in soda-lime glass: Part I. Measurement using nanoindentation

The contact residual stress field created by a Vickers indentation is a micro-size region of high and varying stresses. Stress relaxation studies in such a micro-region may not be accessible to the conventional methods of investigation. In this paper the elastic response during nanoindentation has been used to study the isothermal stress relaxation of a Vickers residual stress field in soda-lime glass at 540 and 630 °C. At each temperature, the stress relaxation profile varied from one location of the stress field to the other suggesting non-linear response to stress. Also, the relaxation profiles at identical positions were different for the two temperatures suggesting that the Vickers residual stress field is not a thermorheologically simple region of material.     

Interdiffusion between silica thin films and soda-lime glass substrate during annealing at high temperature

We study the diffusive interaction between soda-lime glass substrates and sputtered aluminum-doped silica thin films at 650°C, the temperature of commercial soda-lime glass shaping or tempering. A first rapid migration of alkali ions from substrate to thin film has been described in a companion paper (J Am Ceram Soc. 2018;101:1516). Using the same samples as (J Am Ceram Soc. 2018;101:1516), we focus here on later interactions, when the layer is consumed by the substrate resulting from diffusive interactions. Using Secondary Ion Mass Spectroscopy profilometry, we show that the interdiffusion rate increases with the aluminum doping content of the layer. We show that the alkali uptake of silica layers accelerates diffusive exchanges with the substrate, consistently with a decrease of viscosity of the layer. Diffusion profiles of silicon are well reproduced when solving the diffusion equation for a diffusivity having an exponential dependence with silicon concentration. The diffusivity of aluminum is shown to be 10 times slower than the diffusion of silicon. Specific exchanges of the two network formers with network modifiers are deduced from the composition-space trajectories, providing evidence for multicomponent diffusive couplings between species.     

The effect of residual stresses on the user properties of glass tubes

Glass and Ceramics -