Studies of Preparation and Characteristics in Borosilicate Photosensitive Glass-Ceramics

Photosensitive glass-ceramics have been extensively studied in recent years in that it is an attractive high diffraction efficiency grating materials. It is based on Stookey’s mixed fluoride sodium glass system for us to adopt, design prescriptions on the basis of SiO2-Na2O-Al2O3-ZnO for the glass main component and a series of glass doped with CeO2, AgNO3 and NaF etc. melted at about 1450?C, and the glass have good optical property (homogeneity, without bubble and stripe, high transparency). The borosilicate glass was exposed by ultraviolet light, and then after the heat treatment of the sample, the measurement of ultraviolet-visible-near infrared absorption spectrum and the X ray diffraction of exposure part was performed.

Preparation, Crystallization and Mechanical Properties of Potassium Aluminosilicate Glass-ceramics

In this study,transparent K_(2)O-Al_(2)O_(3)-SiO_(2)(KAS)glass-ceramics with leucite as the main crystalline phase were prepared by melting-quench method and two-step heat treatment.The effects of SiO_(2)/Al_(2)O_(3) ratio and heat treatment on crystallization and mechanical properties were studied.The crystallization kinetics and X-Ray Diffraction(XRD)results showed that SiO_(2)/Al_(2)O_(3) ratio and heat treatment system had a direct impact on the crystallization behavior of potassium aluminosilicate glass-ceramics.When heat-treated at 680℃/2 h and 780℃/1 h,cracks generated on the surface of the sample with the addition of SiO_(2)/Al_(2)O_(3)=4.8(in mol)due to the huge difference in the coefficient of thermal expansion between glass matrix and surface.When the addition of SiO_(2)/Al_(2)O_(3)(in mol)was 4,the sample with leucite as the main crystalline phase showed an excellent fracture toughness(1.46 MPa·m^(0.5))after the heat treatment of 680℃/2 h and 780℃/5 h.And there was a phase transformation from kaliophilite to leucite.The crystalline phases of the sample heat-treated at 680℃/8 h and 780℃/1 h were leucite and kaliophilite,which resulted in the visible light transmittance of 63%and the fracture toughness of 0.91 MPa·m^(0.5).Furthermore,after the heat treatment of 680℃/2 h and 780℃/5 h,the main crystalline phase of the sample with SiO_(2)/Al_(2)O_(3)=3.2(in mol)was still kaliophilite.Because leucite only grows on the surface of the sample and is hard to grow inward,it is hard to achieve the bulk crystallization of leucite in the sample with SiO_(2)/Al_(2)O_(3)=3.2(in mol).

Glass-Ceramics with High Strength and High Transmittance Obtained by Multi-Factor Controlling

The presence of Li_(2)Si_(2)O_(5) and LiAlSi_(4)O_(10) could effectively improve the elastic modulus and transmittance of lithium disilicate(LD)glass-ceramics.Through synergistically modulation of the crystal content and grain size,we obtained high strength and high transmittance of LD glass-ceramics.The optimal sample had a high transmittance of 90.3%,the hardness was 7.72 GPa,the fracture toughness was 1.07 MPa·m^(1/2),and the elastic modulus was 103.1 GPa.

Mixed Alkali-zinc Effects on Thermo-mechanical Properties in Borosilicate Glasses

A series of mixed alkali-zinc borosilicate glasses with various r values(r=molar ratio of[ZnO]/([R^(2)O]+[ZnO]))from 0.00 to 1.00 were fabricated to probe the mixed alkali-zinc effects on thermo-mechanical properties.The nonlinear evolution of glass transition temperature(T_(g))with the addition of ZnO is ascribed to the competition of two converse factors,i e,the T_(g)depression as one of the colligative properties for a solution,on the one hand,and the enhancement of T_(g)due to the higher field strength of zinc cations compared to that of alkali ions.However,the nonlinear evolution of elastic moduli and coefficients of thermal expansion with r is attributed to the variance of intermediate-range clusters,which is confirmed by infrared and Raman scattering spectra.These findings are very helpful in tailoring the performance of borosilicate glasses.

Properties of Ultra-low Thermal Expansion LAS Transparent Glass-ceramics Prepared by Spodumene

The glass-ceramics were prepared with the spodumene mineral as the main raw material,and the effects of ZrO_(2)replacing TiO_(2)on the samples were systematically investigated.The results show that the substitution of ZrO_(2)for TiO_(2)is not conductive to precipitate𝛽β-quartz solid solution phase,but can improve the transparency and flexural strength of glass-ceramics.And the glass-ceramic with the highest visible light transmittance(87%)and flexural strength(231.80 MPa)exhibits an ultra-low thermal expansion of-0.028×10^(-7)K^(-1)in the region of 30-700℃.

Crystallization kinetics and temperature dependence of energy storage properties of niobate glass-ceramics

Glass-ceramic materials of strontium barium niobate system were prepared through a melt-quenching method. The effects of crystallization temperature on the mierostructure, dielectric property, breakdown strength and energy storage density of barium strontium niobate glass-ceramics were studied. The crystallization mechanism of the glass-ceramics was discussed and should be one-dimensional interfacial growth. The results indicate that the breakdown strength remarkably increases with the increase of crystallization temperature. The glass-ceramic heat treated at 900 ℃ was found to possess optimal properties with breakdown strength of 1300 kV/cm and energy storage density of 2.8 J/cm3, which is promising dielectric materials for high energy storage density dielectrics.

Visible to deep ultraviolet range optical absorption of electron irradiated borosilicate glass

To study the room-temperature stable defects induced by electron irradiation, commercial borosilicate glasses were irradiated by 1.2 MeV electrons and then ultraviolet（UV） optical absorption（OA） spectra were measured. Two characteristic bands were revealed before irradiation, and they were attributed to silicon dangling bond（E＇-center） and Fe^3＋species,respectively. The existence of Fe3＋was confirmed by electron paramagnetic resonance（EPR） measurements. After irradiation, the absorption spectra revealed irradiation-induced changes, while the content of E＇-center did not change in the deep ultraviolet（DUV） region. The slightly reduced OA spectra at 4.9 eV was supposed to transform Fe3＋species to Fe^2＋species and this transformation leads to the appearance of 4.3 eV OA band. By calculating intensity variation, the transformation of Fe was estimated to be about 5% and the optical absorption cross section of Fe2＋species is calculated to be 2.2 times larger than that of Fe^3＋species. Peroxy linkage（POL, ≡Si–O–O–Si≡）, which results in a 3.7 eV OA band, is speculated not to be from Si–O bond break but from Si–O–B bond, Si–O–Al bond, or Si–O–Na bond break. The co-presence defect with POL is probably responsible for 2.9-eV OA band.

The Coordination State of B and Al of Borosilicate Glass by IR Spectra

The IR spectra of R2O-RO-B2O3-SiO2 and R2O-RO-B2O3-Al2O3-SiO2 glasses were tested for the study of coordination state of B, Al and their content. The results show that no matter Na2O/B2O3〉1, =1, or〈1, both [BO3] and destroyed Si-O bond exist in glass structure; the addition of Al2O3 to borosilicate glass reduced both the number of non-bridging oxygen in the silicate network and the number of [BO4] units.

Influence of aluminium nitride as a foaming agent on the preparation of foam glass-ceramics from high-titanium blast furnace slag

To effectively reuse high-titanium blast furnace slag （TS）, foam glass-ceramics were successfully prepared by powder sintering at 1000℃. TS and waste glass were used as the main raw materials, aluminium nitride （AIN） as the foaming agent, and borax as the fluxing agent. The influence of the amount of A1N added （lwt%-5wt%） on the crystalline phases, microstructure, and properties of the produced foam glass-ceramics was studied. The results showed that the main crystal phases were perovskite, diopside, and augite. With increasing A1N content, a transformation from diopside to augite occurred and the crystallinity of the pyroxene phases slightly decreased. Initially, the aver- age pore size and porosity of the foam glass-ceramics increased and subsequently decreased; similarly, their bulk density and compressive strength decreased and subsequently increased. The optimal properties were obtained when the foam glass-ceramics were prepared by adding 4wt% AIN.

Luminescence of Er^(3+) in Oxyfluoride Transparent Glass-Ceramics

Erbium doped silicate, germanate, and tellurium-germanate oxyfluoride glasses were prepared in a bulk form. Through appropriate heat treatment of the as-prepared glasses, transparent glass-ceramics （TGCs） were obtained with the formation of β-PbF2：Er^3＋ nanocrystals in the glass matrix were confirmed by X-ray diffraction.Well-defined diffraction peaks were observed in the samples after heat-treatment. The average crystal diameter of these precipitated crystals from full-width at half-maximum （FWHM） of the diffraction peak was estimated to be between 8 and 13 nm. Optical absorption, photoluminescence, and upconversion luminescence were measured on as-prepared glass and glass-ceramics. Luminescence spectra in the TGC samples revealed well-resolved, sharp stark-splitting peaks, which indicates that a majority of Er^3＋ ions has been incorporated into the crystalline phase of the nanocrystals. The intensity of the visible and near infrared luminescence mostly increases in TSG compared to that in the as-prepared glass. In 1.53 μm absorption and emission bands, the maximum absorption peak is blue-shifted from 1531 to 1507 nm, whereas the maximum emission peak is redshifted from 1535 to 1543 nm in TGC, as compared with that in glass. The bandwidth at half-maximum （BWHM） of the emission band is significantly broader in TGC than in glass, which is beneficial to the erbium-doped fiber amplifier （EDFA）. Upconversion luminescence was measured using 800 nm near-infrared light excitation. Drastically increased upconversion 1 was observed from the TGC as compared to that from their corresponding as-prepared glasses. In addition to a strong green emission centered at 545 nm because of ^4S3/2→^4I15/2 transition and a weaker red emission centered at 662 nm because of ^4F9/2→^4I15/2 transition, generally seen from the Er^3＋ doped glasses, two violet emissions centered at 410 nm because of ^2H9/2→^4I15/2 transition and centered at 379 nm because of ^4G11/2→^4I15/2 transition were also observed from the was attributed to the decreased effective phonon energy and the increased energy transfer between the excited ions when Er^3＋ ions were incorporated into the precipitated β-PbF2 nanocrystals. The results indicated two attractive spectroscopic properties of the Er^3＋ doped TGC samples, compared to glass samples, namely a reduced multiphonon decay rate and a reduced inhomogeneous broadening. In addition, these oxyfluoride TGC materials were robust,easy and flexibile to process, and possible to be fabricated in the fiber form for device applications.

Nucleation and crystallization of tailing-based glass-ceramics by microwave heating

The effect of microwave radiation on the nucleation and crystallization of tailing-based glass-ceramics was investigated using a 2.45 GHz multimode microwave cavity. Tailing-based glass samples were prepared fi＇om Shandong gold tailings and Guyang iron tailings utilizing a conventional glass melting technique. For comparison, the tailing-based glass samples were crystallized using two different heat-treatment methods： conventional heating and hybrid microwave heating. The nucleation and crystallization temperatures were determined by performing a differential thermal analysis of the quenched tailing-based glass. The prepared glass-ceramic samples were further characterized by Fourier transform infrared spectroscopy, X-ray diffraction, Raman spectroscopy, thermal expansion coefficient measurements, and scanning electron microscopy. The results demonstrated that hybrid microwave heating could be successfully used to crystallize the tailing-based glass, reduce the processing time, and decrease the crystallization temperature. Furthermore, the results indicated that the nucleation and crystallization mechanism of the hybrid microwave heating process slightly differs fi＇om that of the conventional heating process.

Influence of CeO_2 addition on the preparation of foamed glass-ceramics from high-titanium blast furnace slag

Foamed glass-ceramics doped with cerium oxide（CeO_2）were successfully prepared from high-titanium blast furnace slag by one-step sintering.The influence of CeO_2 addition（1.5wt%–3.5wt%）on the crystalline phases,microstructure,and properties of foamed glass-ceramics was studied.Results show that CeO_2 improves the stability of the glass phase and changes the two-dimensional crystallization mechanism into three-dimensional one.XRD analysis indicates the presence of Ca（Mg,Fe）Si_2O_6 and Ca（Ti,Mg,Al）（Si,Al）_2O_（6 ）in all sintered samples.Added with CeO_2,Ti CeO_4 precipitates,and crystallinity increases,leading to increased thickness of pore walls and uniform pores.The comprehensive properties of foamed glass-ceramics are better than that of samples without CeO_2.In particular,the sample added with a suitable amount of CeO_2（2.5wt%）exhibits bulk density that is similar to and compressive strength（14.9 MPa）that is more than twice of foamed glass-ceramics without CeO_2.

Preparation,crystallization,and wetting of ZnO-Al_2O_3-B_2O_3-SiO_2 glass-ceramics for sealing to Kovar

A novel type of ZnO-Al2O3-B2O3-SiO2 glass-ceramics sealing to Kovar in electronic packaging was developed, whose thermal expansion coefficient and electrical resistance are 5.2× 10^-6/℃ and over 1×10^13 Ω·cm, respectively. The major crystalline phases in the glass-ceramic seals were ZnAl2O4, ZnB2O4, and NaSiAl2O4. The dielectric resistance of the glass-ceramic could be remarkably enhanced through the control of alkali metal ions into crystal lattices. It was found that crystallization happened first on the surface of the sample, leaving the amorphous phase in the inner, which made the glass suitable for sealing. The glass-ceramic showed better wetting on the Kovar surface, and sealing atmosphere and temperature had great effect on the wetting angle. Strong interracial bonding was obtained, which was mainly attributed to the interracial reaction between SiO2 and FeO or Fe3O4.

Effects of SnO on Structure and Propertiesof Borosilicate Glasses

Tin was found in the bottom of float borosilicate glasses. To simulate the enriched amounts of SnO found on the surface of the float borosilicate glasses, a series of glasses were produced in which the stannous concentration was varied from 0.1 wt% to 9.0 wt%, while the relative concentration of other components were held constant. Infrared spectra were obtained to probe the effect of increased amounts of SnO on the structure of the glass samples. The results show that SnO plays the role of an intermediate in glasses studied. When FO/SnO〉1.0, SnO takes the role of network-former. And when FO/SnO〈1.0, SnO can give the free oxygen as network-modifier. Besides, SnO has intensive effect on thermal performance of borosilicate glasses.

Effect of sintering temperature on the microstructure and properties of foamed glass-ceramics prepared from high-titanium blast furnace slag and waste glass

Foamed glass-ceramics were prepared via a single-step sintering method using high-titanium blast furnace slag and waste glass as the main raw materials The influence of sintering temperature(900–1060℃) on the microstructure and properties of foamed glass-ceramics was studied. The results show that the crystal shape changed from grainy to rod-shaped and finally turned to multiple shapes as the sintering temperature was increased from 900 to 1060℃. With increasing sintering temperature, the average pore size of the foamed glass-ceramics increased and subsequently decreased. By contrast, the compressive strength and the bulk density decreased and subsequently increased. An excessively high temperature, however, induced the coalescence of pores and decreased the compressive strength. The optimal properties, including the highest compressive strength(16.64 MPa) among the investigated samples and a relatively low bulk density(0.83 g/cm^3), were attained in the case of the foamed glass-ceramics sintered at 1000℃.

Preparation and Optical Properties of Er^(3+)-Doped Gadolinium Borosilicate Glasses

Er^(3+)-doped Gd_2O_3 -SiO_2 -B_2O_3 -Na_2O glasses were prepared, and formation range of glass of Gd_2O_3 -SiO_2 -B_2O_3 system was experimentally obtained. It is found that the glass phase can be formed only when the content of SiO_2 is 0～50%(molar fraction), Gd_2O_3 is 0～30%(molar fraction) and B_2O_3 is above 20%(molar fraction) in this glass system. The glass can also be obtained but becomes translucent at the contents of 60%(molar fraction) SiO_2 and 30% Gd_2O_3 , or at the contents of 60%(molar fraction) SiO_2 and 30%(molar fraction) B_2O_3. There is no glass phase formed in other glass components. Glass forming ability for Gd_2O_3 content of 10%, was characterized by the value of β, the parameter of crystallization tendency, which is 0.32～1.76, obtained from the differential thermal analysis. The absorption and emission cross section, the J-O parameters Ωt_((2,4,6)) and radiative transition probabilities were calculated by using the theory of McCumber and Judd-Ofelt. The emission properties at 1.5 μm of the samples are discussed with the product of full width at half maximum and stimulated emission cross section. It can be seen that the value of the FWHM×σ_e^(peak) product in the prepared glass is more than those of germanate, silicate and phosphate glasses. Furthermore, the maximum value of the product among these glasses reported in this work is close to that of oxyfluoride silicate glass. Therefore, the Er^(3+)-doped gadolinium borosilicate glass in this paper is a candidate for broadband erbium doped fiber amplifiers.

Effect of Water Washing Pre-treatment on the Properties of Glass-ceramics from Incinerator Fly Ash Using Electronic Arc Furnace

Production of glass-ceramics by sintering the molten slag obtained from electric arc furnace treatment of fly ash was investigated. The effect of washing pretreatment prior to melting the fly ash on the microstructure and properties of the glass-ceramics was examined. The results show that washing pretreatment of fly ash can decrease alkali metal chloride and increase network former in fly ash, which results in the increase of peak crystallization temperature of parent glass and strengthening of properties of bending strength and chemical stability of the glass-ceramics. The optimal heat treatment temperature for parent glass of washed fly ash is 1 173 K, at which the crystalline phase of glass-ceramics is composed of gelignite （Ca2A12SiO7） and akermanite （Ca2MgSi207）. Glass-ceramics produced at optimal heat treatment temperature are excellent in term of the physical and chemical properties and leaching characteristics, indicating attractive potential as substitute of nature materials.

Glass-ceramics made from arc-melting slag of waste incineration fly ash

Grate fly ash and fluidized bed fly ash mixed with glass cullet additive respectively were melted in the electronic arc-furnace. The product, arc-melting slag, was further treated by crushing, pressing and heat treatment in order to make the glass-ceramics. The crystallization behaviors of the produced glass-ceramics were examined by differential thermal analysis （DTA）, X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. Results show that main crystalline phase of the glass-ceramics fi＇om grate fly ash is wollastonite （CaSiO3） with small amount of diopside （Ca（Mg,Al）（Si,Al）206）, and that from fluidized bed fly ash is diopside （Ca（Mg,Al）（Si,Al）206）. It is found that the glass-ceramics sintered at 850 ℃and 1 000℃ from grate fly ash and fluidized bed fly ash respectively have the optimal physical, mechanical and chemical characteristics. Glass-ceramics samples, produced from incinerator fly ash with desirable properties and the low leaching concentration of heavy metals, can be the substitute of nature materials such as marble, granite and porcelain tiles.

Effect of Nucleating Agents and Heat Treatments on the Crystallization of Magnesium Aluminosilicate Transparent Glass-ceramics

The crystallization behavior and transparent property of MgO-A1203-SiO2 （MAS） glasses with TiO2 and TiO2＋ZrO2 as nucleating agents were discussed by differential thermal analysis, X-ray diffraction, field emission-environment scanning electron microscope, energy dispersive spectrum and UV-VIS-NIR scanning spectrophotometer. It was found that the glass crystallized at 950 ℃ with ZrO2 less than 3% could obtain transparent glass ceramic, which presented purple to colorless. With the nucleating agent additives （5% TIO2＋3% ZrO2）, the colorless transparent glass-ceramics with spinel as the main crystal phase could be prepared, and the transmittance reached about 80%. As the crystallized temperature increase to 1 000 ℃, besides spinel（MgA1204）, sapphirine （Mg3.5A19Si1.5O20） and ZrTiO4 precipitated from matrix glass, and the transmitance of glass-ceramic decreased.

Effect of SiO_2/B_2O_3 Ratio on the Property of Borosilicate Glass Applied in Parabolic Trough Solar Power Plant

This work aimed to analyze the glass material used for sealing the end of a thermal collector in a parabolic trough solar power plant. Based on matched sealing requirements and application performance of glass and Kovar alloy 4J29, one borosilicate glass material （GD480S）, whose expansion coefficient was similar to that of Kovar alloy 4J29, was studied. Moreover, the effect of the ratio of SiO2 to B203 on the glass properties was explored in detail by Fourier transform infrared spectroscopy. As the SiO2 to B203 ratio in the glass increased from 4.18 to 5.77, the expansion coefficient showed a decreasing trend from 4.95×10-6/℃ to 4.55℃ 10-6/℃. In addition, the water resistance performance improved, enabling the glass material to seal well with the alloy for application in a trough solar power plant. Thus, the increase in the SiO2 to B2O3 ratio made the glass structure more compact and improved the glass performance to meet the requirements of an industrial tubular receiver.