废弃玻璃粉对水泥石高温抗压强度和微观结构的影响

废弃玻璃粉作为一种高SiO₂含量的固体废弃物,可以有效防止油井水泥石在高温下的强度衰退,从而提升深井、超深井固井水泥环长期封隔完整性。本文研究了150 ℃、21 MPa下,不同粒径废弃玻璃粉对水泥石抗压强度、渗透率和微观结构的影响。结果表明:150 ℃、21 MPa下净浆水泥石180 d抗压强度为8.57 MPa,较1 d衰退76.04%;掺入废弃玻璃粉可以提高水泥石抗压强度的长期稳定性,在内掺40%(质量分数)粒径为45 μm的废弃玻璃粉情况下,水泥石在180 d时抗压强度为31.85 MPa,较1 d仅衰退3.95%,渗透率为1.28×10^-2 mD,较1 d降低16.88%;掺入废弃玻璃粉改变了水泥石150 ℃、21 MPa下的物相组成,净浆水泥石的主要结晶相为氢氧化钙和水硅钙石,掺入不同粒径废弃玻璃粉的水泥石主要结晶相为硬硅钙石和托贝莫来石;内掺40%粒径为45 μm的废弃玻璃粉的水泥石中托贝莫来石晶粒尺寸稳定;随龄期增加,净浆水泥石孔结构向大孔径发展,内掺40%粒径为45 μm的废弃玻璃粉的水泥石的孔结构更加致密,180 d内各龄期均以凝胶孔为主。     

Preparation and characterization of foams from sheet glass and fly ash using carbonates as foaming agents

Glass foams were produced using sheet glass cullet and fly ashes from thermal power plant with added carbonates (commercial dolomite- and calcite-based sludges) as foaming agents. The influence of type and amount of carbonates as well as of the sintering temperature on the apparent density, compressive strength, microstructure and crystalline phases was evaluated. The experimental results showed that homogenous microstructures of large pores could be obtained by adding just 1–2 wt.% carbonates and using low sintering temperature (850 °C), leading to foams presenting apparent density and compressive strength values of about 0.36–0.41 g/cm³ and 2.40–2.80 MPa, respectively. Good correlations between compressive strength, apparent density and microstructure (pore size, struts’ thickness and internal porosity) were observed.     

Preparation of ultra-light ceramic foams from waste glass and fly ash

Ultra-light ceramic foams were successfully prepared by a green spheres technique, which used waste glass powder and fly ash as the main material. Besides, borax and SiC were introduced as fluxing agent and foaming agent, respectively. The effects of fly ash content, borax content and sintering temperature on the microstructures and properties of ceramic foams were systematically investigated. The optimum composition is 30?wt-% fly ash, 70?wt-% waste glass, 15?wt-% borax and 0.5?wt-% SiC. Ultra-light ceramic foams sintered at 680–780°C possess bulk density of 0.14–0.41?g?cm^?3, porosity of 82.9–94.1%, compressive strength of 0.91–6.37?MPa and thermal conductivity of 0.070–0.121?W?m^?1?K^?1, respectively. This method is convenient, low-cost and environment friendly, which makes it a promising way for recycling solid wastes.     

Fabrication of dense and porous biphasic calcium phosphates: Effect of dispersion on sinterability and microstructural development

The particle size distribution of a commercial Mg-doped hydroxyapatite powder was tailored through two different milling procedures, carried out under wet or dry conditions. Wet milling gave rise to finer particles, with a narrower size distribution. Tailoring the particles size was the key to produce homogeneous gelcast green bodies, as well as fully dense and fine microstructures. In fact, wet-milled samples achieved full densification and compressive strength of about 300 MPa, five times higher than the values achieved by the dry milled samples. During the calcination treatments, HA progressively decomposed into β- and α-TCP phases, promoted by the progressive Mg²⁺ substitution inside the HA and β-TCP lattices. As a result, a biphasic (HA/β-TCP) calcium phosphate ceramic was successfully obtained. Gelcast macroporous materials were prepared by direct foaming, starting from both milled powders. Highly porous samples (73%-77% porosity) with a high degree of interconnectivity within pores were successfully produced. However, dry milled-foamed materials were characterized by a significant residual porosity within the struts, whereas in wet-milled foams struts and pore windows were highly compact, the key to provide sufficient mechanical strength to such highly porous open-cell foams, thus suggesting a possible use as implantable scaffolds.     

Preparation and characterization of foam glass from waste container glasses and water glass for application in thermal insulations

Glass foams are modern developed building materials which are now favorably competing with conventional materials for applications in thermal insulation. In this study, glass foams are synthesized solely from waste container glasses of mixed colors using sodium silicate (water glass) as foaming agent. Several glass foams of 150 × 150 × 30 mm were prepared from waste glasses of 75 μm, 150 μm and 250 μm size with addition of 15 wt % sodium silicate respectively and pressed uniaxially under a pressure of 10 MPa. The prepared glass foams were then sintered at temperatures of 800 °C and 850 °C respectively. Tests such as bulk density, estimated porosity, flexural strength, compressive strength and microstructure evaluation were used to assess the performance of the developed glass foams. The results showed that with increasing temperature and grain sizes, the percent porosity of the developed foams increased while the bulk density decreased. The microstructure evaluation showed that the finer the grain sizes used, the more homogenized are the pores formed and the higher the temperature, the larger the pores but are mostly closed. Both compressive and flexural strength were found to decrease with grain sizes and higher temperatures. The thermal conductivities of all the developed foam glasses satisfy the standard requirement to be used as an insulating material as their thermal conductivities did not exceed 0.25 W/m.K.     

Ultra low-density mullite foams by reaction sintering of thermo-foamed alumina-silica powder dispersions in molten sucrose

Ultra low-density mullite foams are prepared by thermo-foaming followed by reaction sintering of alumina-silica powder dispersions in molten sucrose. The foaming & setting time, foam rise, sintering shrinkage, porosity, cell size and compressive strength are studied as a function of ceramic powder loading, foaming temperature and magnesium nitrate (blowing agent and setting agent) concentration. Phase pure mullite is produced by reaction sintering at 1600 °C. The mullite foams produced without magnesium nitrate have porous struts and cell walls due to improper densification. The magnesium nitrate drastically decreases the foaming & setting time and increases the foam rise and cell interconnectivity. The MgO produced from the magnesium nitrate assists the densification of the mullite as evidenced from the non-porous struts and cell walls at higher magnesium nitrate concentrations. The maximum porosity of 94.92 and 96.28 vol.% achieved without and with magnesium nitrate, respectively, is the highest reported for mullite foams.     

The influence of process parameters on in situ inorganic foaming of alkali-bonded SiC based foams

Silicon carbide (SiC) foams were developed with a low temperature process by using an inorganic alkali aluminosilicates binder, also known as geopolymer. The foaming agent was the metallic silicon present as impurity in the SiC powder. Si⁰ in the alkaline solution led to gas evolution that induced the foaming of the slurries. The binder was a geopolymeric resin with atomic ratio Si/Al = 2 and potassium as alkaline cation, classified as (K)poly(silalate-siloxo). The geopolymeric resin was prepared using metakaolin as aluminosilicatic raw powder, while the alkali aqueous solution was KOH/K₂SiO₃. Metakaolin in alkaline conditions dissolved and re-precipitated to form geopolymeric nano-particulates that acted as a glue to stick together SiC particles (90 wt.%). Process parameters such as water addition, mixing time and curing temperature were correlated to the foam structure. The formation of prolate pores induced anisotropy in the compressive strength. The foams were studied by dilatometric analysis in inert and oxidative atmospheres up to 1200 °C.     

Fabrication and characterization of a mullite-foamed ceramic reinforced by in-situ SiC whiskers

In this study, a new mullite-foamed ceramic, reinforced with in-situ SiC whiskers (MCS) and applied as the insulating lining of thermal equipment used in cement production, was investigated. Compared with a conventional mullite-foamed ceramic (MC), the MCS phase composition, microstructure, compressive strength, thermal conductivity and alkali corrosion resistance were investigated by using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and Factsage® software. The results showed that after being fired in granular coke, the SiC whiskers formed into MCS struts and were distributed in the pores between the interconnected needle-like mullite. Although the formation of SiC with higher conduction slightly increased MCS thermal conductivity, it significantly enhanced the compressive strength and alkali corrosion resistance of the foamed ceramic. Compared with the MC, although the MCS had higher bulk density (3.9%), and higher thermal conductivity (9.5% at 800 °C), it was more important that greatly improved compressive strength (by 60%) and better alkali corrosion resistance was achieved.     

Direct ink writing of wollastonite-diopside glass-ceramic scaffolds from a silicone resin and engineered fillers

Wollastonite-diopside scaffolds have been successfully developed by direct ink writing of an ink made of silicone polymer and inorganic fillers. The main reason for using a silicone in the ink formulation consisted in its double effect, in controlling the ink rheology and in developing of wollastonite and diopside crystalline phases upon heat treatment. The obtained 3D wollastonite-diopside scaffolds featured regular geometries, and a high compressive strength (3.9–4.9 MPa) when considering the large amount of porosity (68–76 vol.%). A glass with the same oxide composition as the silicone-based ink and crystallizing into wollastonite and diopside, was produced and used as additional filler. This addition enabled the fabrication of even stronger 3D printed scaffolds (∼8 MPa for a porosity of 67 vol%), owing to the enhanced viscous flow upon firing which reduced the micro-cracks in the scaffold struts generated by the preceramic polymer decomposition. The obtained highly porous wollastonite-diopside glass-ceramic scaffolds are suitable candidates for bone tissue engineering.     

Behaviour of open-cell cordierite foams under compression

Cordierite foams were produced using the polymer foam replication method. The effects of both the structure of the polymeric foam template and the slurry's solid loads on the compressive strength and the sintered structure of the ceramic foam were evaluated in order to achieve the optimal manufacturing conditions. The compressive strengths of cordierite foams were measured at room temperature. Polyurethane (PU) foams were used as templates. Aqueous ceramic suspensions were prepared with solids weight fraction ranging from 50 to 65%. The effects of both the PU density and the solids volume fraction on porosity and strength of the developed cordierite foams were evaluated. The cordierite foams produced are of semiclosed-cell type. Some impregnation difficulties were experienced with increasing of the PU density. The compressive strength of the cordierite foams increased (from 0.1 to 2 MPa) with increasing solids volume fraction. These data are in agreement with the predictions of the model developed by Gibson and Ashby. However, the exponent of the model was half of the measured one (≈3) over the range of relative densities investigated (80–90%). Such discrepancy might be related to several factors such as the morphological differences in the structural unit of the developed foams with respect to a cubic open-cell foam or to the mixture of both open and closed cells or to the presence of non-periodic cells. In addition, it was found that the compressive strengths depended on the cell size for foams of similar relative densities and generally decreased with increasing of the cell size, which deviates from the theoretical predictions. When the starting polymeric substrate contained a higher fraction of closed cell windows, however, the ceramic material present on the cellular structure was not only distributed on the struts but also filled the cell walls. This contributed to an increase of the relative density of the cordierite foams and consequently to higher compressive strengths.     

Biobased Polyurethane Composite Foams Reinforced with Plum Stones and Silanized Plum Stones

In the following study, ground plum stones and silanized ground plum stones were used as natural fillers for novel polyurethane (PUR) composite foams. The impact of 1, 2, and 5 wt.% of fillers on the cellular structure, foaming parameters, and mechanical, thermomechanical, and thermal properties of produced foams were assessed. The results showed that the silanization process leads to acquiring fillers with a smoother surface compared to unmodified filler. The results also showed that the morphology of the obtained materials is affected by the type and content of filler. Moreover, the modified PUR foams showed improved properties. For example, compared with the reference foam (PUR_REF), the foam with the addition of 1 wt.% of unmodified plum filler showed better mechanical properties, such as higher compressive strength (~8% improvement) and better flexural strength (~6% improvement). The addition of silanized plum filler improved the thermal stability and hydrophobic character of PUR foams. This work shows the relationship between the mechanical, thermal, and application properties of the obtained PUR composites depending on the modification of the filler used during synthesis.     

Performance of glass-ceramic-based lightweight aggregates manufactured from waste glass and muck

Lightweight aggregates (LWAs) with microcrystalline diopside as the main constituent were prepared in this study. Waste glass and waste muck were used as the main raw materials, and the formula was designed according to the chemical composition of diopside, rather than using the Riley scheme. The effects of the glass content and nucleating agent on the mechanical properties, mineral composition, and microstructure of LWAs were studied. The results indicated that the presence of diopside crystallites can significantly improve the mechanical properties of LWAs. With an increase in the glass content from 0 wt % to 70 wt %, the strength of the LWAs increased from 12.21 MPa to 19.31 MPa with similar densities in the range of 1.667–1.687 g/cm³. The addition of a nucleating agent has a fluxing effect and promotes the formation and growth of diopside, which provides aggregates with high strength and low density. For example, the addition of CaF₂ decreased the density of the LWAs from 1.687 g/cm³ to 1.461 g/cm³ and increased the strength from 17.59 MPa to 20.81 MPa under the same calcination regime. The effect of the pore structure on the mechanical properties of the LWA in this experiment was far less than that of the crystal phase composition. With the addition of a nucleating agent, the diopside was co-precipitated from both the muck and glass. If no nucleating agent is added, diopside mainly precipitates from glass, and muck mainly forms a glass phase.     

高密度聚氨酯硬泡塑料／玻纤粉复合材料的研究

以聚醚多元醇、PAPI、催化剂、发泡剂和玻璃纤维等为原料,制备高密度聚氨酯硬泡及它与磨碎玻纤粉的复合材料。研究了不同密度硬泡的强度及磨碎玻纤粉粒径、预处理及其含量对复合材料强度的影响,不同复合材料的热稳定性。结果表明,随着密度的增加,硬泡的各种强度值总体上均呈逐渐增加趋势,其中500kg/m^3的聚氨酯的拉伸强度比200kg/m^3的提高了104．74％,冲击强度提高了194．84％;400目粒径的玻纤粉可使复合材料具有更高的拉伸强度、弯曲强度及压缩强度;玻纤的加入将降低材料的强度值,但偶联剂预处理可使它们有所改善;加入磨碎玻纤粉后,材料的热稳定性增加,且采用偶联剂KH550对玻纤粉进行预处理可进一步改善复合材料的耐热性能。     

Bio-cellular glass–ceramic composite with embedded calcium phosphate from eggshell for alternative biomaterials in medical and dental applications

Green biomaterial foams with nontoxicity, low weight, low density, and high-compressive strength, which can be easily manufactured at low cost, are urgently sought. When implanted as a scaffold, bio-cellular glass–ceramic composite has potential for bone bonding, connective tissue growth, and reconstruction of lost tissue. The present study investigates the physical-thermo-mechanical properties of bio-cellular glass–ceramic composite supplemented with calcium phosphate from eggshell powder (0, 1, 3, or 5 wt%) and sodium-silicate binder. The composite materials were prepared by hand pressing and fired at 800 or 900°C for 1 h. The composites containing 1 and 3 wt% calcium phosphate from eggshell powder and fired at 800°C achieved suitable porosity (74–79%), pore size (20–800 μm), bulk density (0.57–0.70 g/cm³), true density (0.98–1.06 g/cm³), water absorption (10.31–21.41%), compressive strength (2.71–3.23 MPa), and thermal expansion coefficient ([5.95–5.98] × 10⁻⁶°C⁻¹) for practical applications. The obtained bio-cellular glass–ceramic composite is an alternative biomaterial for biomedical and dental applications.     

Compressive strength and wear properties of SiC/Al6061 composites reinforced with high contents of SiC fabricated by pressure-assisted infiltration

Pressure-assisted infiltration was used to synthesize SiC/Al 6061 composites containing high weight percentages of SiC. A combination of PEG and glass water was used to fabricate SiC preforms and the effect of the presence of glass water on the microstructure and mechanical properties of the preforms was evaluated by performing compression tests on the preforms. Also, the compressive strength and the hardness of the SiC/Al composites were investigated. The results revealed that the glass water improved the compressive strength of the preforms by about five times. The microstructural characterization of the composites showed that the penetration of the aluminum melt into the preforms was completed and almost no porosity could be seen in the microstructures of the composites. Moreover, the composite containing 75 wt% SiC exhibited the highest compressive strength as well as the maximum hardness. The results of the wear tests showed that increasing the SiC content reduces the wear rate so that the Al-75 wt% SiC composite has a lower wear rate and a lower coefficient of friction than those of Al-67 wt% SiC composite. This indicated higher wear resistance in these composites than the Al alloy due to the formation of a tribological layer on the surface of the composites.     

Oxidation resistant ceramic foam from a silicone preceramic polymer/polyurethane blend

Silicon oxycarbide (SiOC) ceramic foams, produced by the pyrolysis of a foamed blend of a methylsilicone preceramic polymer and polyurethane (PU) in a 1/1 wt.% ratio, exhibit excellent physical and mechanical properties. The proposed process allows to easily modify the density and morphology of the foams, making them suitable for several engineering applications. However, it has been shown that, due to residual carbon present in the oxycarbide phase after pyrolysis, the foams are subjected to an oxidation process that reduces their strength after high temperature exposure to air (12 h 1200°C). A modified process, employing the same silicone resin preceramic polymer but a much lower PU content (silicone resin/PU=5.25/1 wt.% ratio), has been developed and is reported in this paper. Microstructural investigations showed that carbon rich regions deriving from the decomposition of the polyurethane template are still present in the SiOC foam, but have a much smaller dimension than those found in foams with a higher PU content. Thermal gravimetric studies performed in air or oxygen showed that the low-PU containing ceramic foams display an excellent oxidation resistance, because the carbon-rich areas are embedded inside the struts or cell walls and are thus protected by the dense silicon oxycarbide matrix surrounding them. SiOC foams obtained with the novel process are capable to maintain their mechanical strength after oxidation treatments at 800 and 1200°C (12 h), while SiOC foams obtained with a higher amount of PU show about a 30% strength decrease after oxidation at 1200°C (12 h).     

Low‐Density Open Cellular Silicon Carbide Foams from Sucrose and Silicon Powder

Open cellular SiC foams with low densities were prepared by thermo‐foaming and setting (130°C–150°C) of silicon powder dispersions in molten sucrose followed by pyrolysis and reaction sintering at 1500°C. The bubbles generated in the dispersion by water vapor produced by the –OH condensation was stabilized by the adsorption of silicon particles on the air‐molten sucrose interface. The composition of a sucrose‐silicon powder mixture for producing SiC foam without considerable unreacted carbon was optimized. The sucrose in the thermo‐foamed silicon powder dispersion leaves 24 wt% carbon during the pyrolysis. The sintering additives such as alumina and yttria promoted the silicon‐carbon reaction. SiC nanowires with diameters in the range of 35–55 nm and length >10 μm observed on the cell walls as well as in the fractured strut region were grown by both vapor–liquid–solid and vapor–solid mechanisms. Large SiC foam bodies without crack could be prepared as the total shrinkage during pyrolysis and reaction sintering was only ~30 vol%. The relatively low compressive strength (0.06–0.41 MPa) and Young's modulus (14.9–24.2 MPa) observed was due to the large cell size (1.1–1.6 mm) and high porosity (93%–96%).     

Mechanical Properties of Silicon Oxycarbide Ceramic Foams

The mechanical properties of ceramic foams obtained through a novel process that uses the direct foaming and pyrolysis of preceramic polymer/polyurethane solutions were investigated. The elastic modulus, flexural strength, and compressive strengths were obtained for foams in the as-pyrolyzed condition; values up to 7.1 GPa, 13 MPa, and 11 MPa, respectively, were obtained. The strength of the foam was virtually unchanged at temperatures up to 1200°C in air; however, long-term exposure at 1200°C led to a moderate degradation in strength, which was attributed to the evolution of intrastrut porosity during the oxidation of residual free carbon, as well as devitrification of the foams struts.     

Porosity and Strength of Silicon Carbide Foams Prepared Using Preceramic Polymers

Two types of polymeric precursors for silicon carbide (SiC) were dissolved in dichloromethane. Subsequently, between 10–80 wt% of silicon nitride (Si₃N₄) and titanium carbide (TiC) powder were added separately into the solutions to make SiC-Si₃N₄ and SiC-TiC suspensions. Cubes of polyurethane (PU) foams were soaked in precursor solution and suspensions and pyrolyzed in flowing nitrogen to produce SiC, SiC-Si₃N₄ and SiC-TiC composite foams. Some foams were heated further in nitrogen to 1600°C. Shrinkage observed after pyrolysis and further heating the foams was measured and can be reduced by varying the concentration of polymeric precursor, Si₃N₄ and TiC content. The foams produced have porosities in the range 85–96%. The average compressive strength of the foams is in the range of 1.1–1.6 MPa.     

Synthesis,morphological and thermomechanical characterization of light weight silica foam via reaction generated thermo-foaming process

Low-cost thermo-foaming technique involving sucrose dehydration reaction with H₂SO₄ has been used for ceramic foam processing. The heat and gas generated during the reaction induces a thermo-foaming effect in the sucrose-ceramic mixture. This converts the sucrose-ceramic slurry into a carbonaceous porous ceramic-scaffold. The converted carbon is seen to agglutinate with the ceramic particles. During sintering, they are removed subsequently, thereby enlarging the pores. Influence of solids-loading, sintering temperature and H₂SO₄ concentration on the foaming behaviour, pore morphology and thermo-mechanical properties are studied. The fabricated silica foams are found to have porosity within the range of 70 %? 90 % and compressive strength of 0.8–2.8 MPa. The extreme porosity of the silica foams and their intercrystallite pores within the struts results in the low thermal conductivity (0.0943 Wm^?1K^?1) of the specimens. The fabricated foam is seen as a promising material for insulation applications like catalyst supports, filters and bio-scaffolds.