Influence of heat-treatment protocols on mechanical behavior of lithium silicate dental ceramics

In this work, three different commercial lithium silicate (LS) glass-ceramics for computer aided design/computer aided machining systems, CeltraDuo-Dentsply (LS-C), E-MaxCAD-Ivoclar (LS-E), and Suprinity-Vita (LS-S), were comparatively characterized. Following the protocols recommended by the manufacturers, the glass-ceramics were heat-treated under low vacuum and characterized by X-ray diffraction, scanning electron microscopy, hardness, fracture toughness, Young's modulus, and flexural strength. Rietveld refinement indicated that the materials “as-received” present mostly amorphous phase and Li₂SiO₃ as secondary crystalline phase in LS-E and LS-S specimens, while LS-C specimens also present Li₂Si₂O₅ and Li₃PO₄ as crystalline phases. All “as-received” glass-ceramics present hardness, fracture toughness, and Young's modulus of around 647-678 HV, 1.15-1.40 MPa.m^1/2, and 82-92 GPa, respectively. After heat treatment, the LS-C and LS-S specimens presented decreasing of amorphous phase associated to Li₂SiO₃ and Li₂Si₂O₅ grains with low aspect ratio, while LS-E indicates a reduction of amorphous phase and Li₂Si₂O₅ elongated grains. Fracture toughness and Young's modulus increase about 10% due to the crystallization of residual amorphous phase for all materials. Moreover, crystallographic and microstructural characteristics are responsible for the higher flexural strength of LS-E (327 MPa), regarding LS-C and LS-S. However, the glass-ceramics LS-E present lower Weibull modulus (m = 5.4) comparatively to LS-C (m = 9) and LS-S (m = 6).     

热处理温度对磷渣-煤矸石微晶玻璃结构和性能的影响

以磷渣和煤矸石为原料,采用一步烧结法制备了性能优良的CaO?Al2O3?SiO2(CAS)系微晶玻璃,用差示扫描量热法(DSC),X射线衍射(XRD)和扫描电子显微镜(SEM)等对其进行分析和表征,研究了热处理温度对微晶玻璃晶相组成、微观结构和宏观性能的影响规律。结果表明,固废利用率达100%,微晶玻璃性能良好;以磷渣和煤矸石为原料在1250℃下熔融2 h、于850℃热处理保温2 h可制备主晶相为假硅灰石Ca3(Si3O9)的微晶玻璃,其抗折强度、显微硬度和体积密度分别为74.4 MPa,566.9 HV和2.75 g/cm3。随热处理温度升高,微晶玻璃主晶相由Ca3(Si3O9)相转变为硅灰石CaSiO3相,晶体形态由球状向针状、短柱状改变,对提高微晶玻璃抗折性能有利,而显微硬度和体积密度均先增加后降低。     

Mechanical and leaching properties of neodymium-contaminated soil glass-ceramics

The safe treatment of radioactive-contaminated soil is of great significance. In this work, neodymium-contaminated soil was successfully immobilized using microwave sintering to form glass-ceramics. The microstructure, morphology, elemental distribution, Vickers hardness, and chemical durability of the sintered samples were analyzed. The results showed that the glass-ceramic is more suitable to immobilize the waste compared with the glass matrix. XRD and SEM-EDS results proved that the waste form has been totally immobilized in the sintered matrix whether in glass-ceramics and glass. However, the leaching rate of element Nd in glass-ceramic was lower than the glass matrix at 28 d. Moreover, the Vickers hardness results of glass-ceramic were higher than that of glass. Thus, glass-ceramics can not only reduce sintering temperature and save energy but also achieve a better immobilizing effect. Our investigation reflects that glass-ceramics are more suitable for neodymium-contaminated soil immobilization using the microwave sintering method.     

Effect of heat treatment on the roughness and mechanical properties of dental lithium disilicate glass-ceramics

In dental clinics, it is common to perform small fitting adjustments in dentures using a micro-grinding tool after testing them in the patient's mouth. This procedure increases local roughness and can lead to formation of microcracks on the prosthesis surface. This study aimed to investigate the benefits of a post-finishing heat treatment to surface roughness and crack healing and its effect on the flexural strength of lithium disilicate (LD) dental glass-ceramics. Commercially available lithium metasilicate, Li₂SiO₃, samples were heat treated at 840 °C for 7 min to induce the phase transformation into LD, Li₂Si₂O₅. The LD samples were characterized by X-ray Diffraction, Scanning Electron Microscopy, Vickers hardness, Young’s modulus, and fracture toughness. One of the surfaces of the LD samples was sanded aiming to simulate the denture fitting adjustments performed in the dentist’s laboratory, generating a rough surface, Group 1. Half of the LD samples had their biaxial flexural strength evaluated by the piston-on-three-ball test (P–3B) and the other half were submitted to a second short-term heat treatment (840 °C - 5 min), Group 2, and later assessed by the P–3B. Roughness parameters in both groups were measured by 3D optical profilometry. After the crystallization heat treatment, formation of elongated LD crystals, Li₂Si₂O₅, 35% amorphous phase, and residual Li₃PO₄ was observed. In addition, the following mechanical property values were obtained: Vickers hardness = 5.8 ± 0.1 GPa, fracture toughness = 2.2 ± 0.1 MPa m^1/2, and Young’s modulus = 100.3 ± 0.3 GPa. The samples in Group 1 showed bending strength of 206 ± 30 MPa and the following roughness parameters: Ra = 0.45 ± 0.16 μm, Rz = 22.7 ± 6.7 μm, and PV = 27.7 ± 7.1 μm. In the samples in Group 2, the Ra, Rz and PV roughness parameters were 0.31 ± 0.12 μm, 5.2 ± 2.5 μm, and 9.2 ± 4.7 μm, respectively. With this decrease in roughness, the bending strength increased by 62%, with a mean value of 331 ± 59 MPa. In the need for machine finishing of LD-based glass-ceramic dental prostheses, the use of a second short-term heat treatment at 840 °C for 5 min generates considerable gains in bending strength, increasing the lifecycle of the prosthesis as a result of reduced surface roughness caused by softening of the remaining amorphous phase in the glass-ceramic. These conditions can be adapted to each chemical and crystallographic composition of the glass-ceramic under study.     

热处理对杂环芳纶结构与性能的影响

采用了热失重分析仪(TGA)、傅里叶变换红外光谱(FTIR),扫描电子显微镜(SEM),广角X射线衍射(WAXD)等手段研究热处理对含杂环的共聚芳香族聚酰胺纤维结构与性能的影响。结果表明:热处理条件为氮气气氛,温度420℃,时间4 min,拉伸倍数为1;经过热处理后杂环芳纶的化学结构没有明显的变化,纤维结晶度由11.2%提高到51.6%,纤维的取向度显著提高,纤维的表面更加光滑致密;纤维的热稳定性无明显变化,纤维的线密度有略微变小,断裂强度为23.8 cN/dtex,弹性模量为1 041.43 cN/dtex。     

热处理对轮胎帘子线用Lyocell纤维性能的影响

在自制的热处理装置上对尚未干燥过的Lyocell初生纤维进行热处理,探讨了张力和热处理温度对纤维性能的影响。结果表明,热处理能提高Lyocell纤维的断裂强度和初始模量。预张力为0.75 cN/dtex、热处理张力为0.60 cN/dtex、热处理温度为130℃,热处理时间为11 s时,热处理效果较好,Lyocell纤维断裂强度达5.8 cN/dtex、初始模量达86.9 cN/dtex、干热收缩率小于1.1%,经热处理后的Lyocell纤维符合轮胎帘子线性能要求。     

热处理对PTT短纤维力学性能的影响

研究了PTT短纤维热处理前后的力学性能,并与PET纤维进行了对比。结果表明,PTT短纤维具有优良的弹性性能,其断裂伸长率和弹性回复比PET纤维高。经100℃热处理后,PTT纤维的强伸性能降低,在应力1.0cN和10%伸长下的弹性显著减弱,说明热处理对PTT的弹性性能具有较大的影响。     

Failure mechanisms in in-situ SEM micropillar compressions of pre-crystallized and crystallized zirconia-containing lithium silicate glass-ceramics

Microscale microstructure-property relations for zirconia-containing lithium silicate glass-ceramics (ZLS) are critical for their applications as load-bearing restorations. This study investigated in-situ scanning electron microscopy (SEM) micropillar compression responses of pre-crystallized and crystallized ZLS materials with a flat diamond punch. Micromechanical properties (moduli, strength, ductility, resilience and toughness) of the two materials were determined. Pre-crystallized and crystallized ZLS materials showed distinct ductile-brittle failure mechanisms. Pre-crystallized ZLS containing weaker lithium metasilicate crystals and higher concentrated glass matrix revealed its ductile mode featured with bending and delamination, and side-splitting fractures originated from fragmentation and microcracking. Crystallized ZLS with stronger lithium disilicate crystals and lower concentrated glass matrix demonstrated bending and shear-band initiation, shear fracture from shear-band expansion and fragmentation. Further, crystallized ZLS yielded much higher moduli, strength, ductility, resilience and toughness than pre-crystallized ZLS. This study provides vital insights into the basic understanding of micromechanical behavior of ZLS materials for load-bearing applications.     

Synthesis of glass-ceramics in the Na2O/K2O-CaO-MgO-SiO2-P2O5-CaF2 system as candidate materials for dental applications

This study reports on the sintering behavior, crystallization process, and mechanical properties of novel glass-ceramics (CGs) produced by the glass powder compact consolidation method. Substitution of K₂O for Na₂O and MgO for CaO was attempted in the parent glasses belonging to Na₂O-CaO-MgO-SiO₂-P₂O₅-CaF₂ system. Glass powder compacts were heat treated at various temperatures between 700°C and 900°C, taking under consideration the glass transition (T_g) and the crystallization peak (T_p) temperatures, which were experimentally determined for each investigated glass by thermal analysis (dilatometry and differential scanning calorimetry). The experimental results showed that sintering always preceded crystallization, regardless of the type of substitution. In the case of MgO substitution for CaO, crystallization was advanced in the range of 800°C-850°C, resulting in the formation of an assembly of crystalline phases, such as diopside, fluorapatite, and wollastonite. The substitution of K₂O for Na₂O increased the activation energy for crystallization, shifting crystallization process to a high temperature region, with the formation of alpha-potassium magnesium silicate, instead of wollastonite. The GCs produced had values of 22-31 GPa regarding the modulus of elasticity, 5.0-6.1 GPa concerning the microhardness, and 1.4-1.9 MPa⋅m^0.5 as regard the fracture toughness, which are similar to those of the human jawbone.     

Effects of heat treatment on tensile properties of diacetate fibers

Diacetate filaments were heat‐treated (without tension or with tension) under dry‐heat or wet‐heat environment, respectively. The effects of temperature, time, and tension on tensile properties of diacetate fibers after heat treatments were discussed. The results show that diacetate fibers present no obvious improvement on its tensile properties after dry‐heat treatments without tension. It was also found that during dry heat treatments with tension, the increase in tensile properties of fibers mainly depends on temperature and tension. Moreover, being dry‐heat treated with tension instant after wet‐heat treatment without tension, diacetate fibers exhibit a higher improvement on its tensile properties comparing with dry heat method with tension. The shrinking measurement for the fibers indicates different supermolecular structures were developed in the fiber before treatment and after treatment, which leads to the different extent in the improvement of tensile properties for the fibers. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101:787–791, 2006     

Development of poly(dimethylsiloxane)–titania nanocomposites with controlled dielectric properties: Effect of heat treatment of titania on electrical properties

Polymer–ceramic composites were prepared using poly(dimethylsiloxane) as base matrix and normal as well as heat‐treated titania as fillers. Dielectric and mechanical properties of the composites were measured and found that dielectric constant of the composites was increased dramatically with the addition of filler, whereas resistivity was decreased. Hardness and modulus were found to increase but tensile strength, % elongation at break, and tear strength were decreased with the filler loading. Neat titania contains some moisture (physisorbed and chemisorbed) as revealed from thermogravimetric analysis. Both electrical and mechanical properties of the composites were affected by filler heat treatment. Further, untreated titania contains Ti³⁺ and Ti⁴⁺, which on heat treatment, increases the concentration of Ti⁴⁺, as a result electrical properties were affected. Filler dispersion in the composites was studied by field emission scanning electron microscopy and high resolution transmission electron microscopy. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

The effect of heat treatment on tensile properties of 2D C/SiC composites

Two-dimensional (2D) carbon fiber reinforced silicon carbide (C/SiC) composites with different initial strength were prepared by chemical vapor infiltration (CVI). After tensile property testing, results exhibited that as the heat-treatment temperature (HTT) increases to 1900°C, the tensile strength and toughness of the low strength specimen (LSS) increased by 110% and 530%, while the high strength specimen (HSS) increased by 5.4% and 550%, respectively. As observed from morphologies, the heat treatment increases the graphitization of the amorphous PyC interphase, which leads to the weakening of interfacial bonding strength (IBS). Meanwhile, the defects arising from heat treatment cause thermal residual stress relaxation. Therefore, the tensile strength and toughness of LSS with relatively high initial IBS increase significantly as HTT increases. For HSS with moderate initial IBS, the heat treatment slightly improves the tensile strength, but significantly improves the toughness. Consequently, the post-heat-treatment tensile properties of 2D C/SiC composites can be regulated by varying HTTs and different initial strength.     

热处理对PET/PTT复合纤维力学性能的影响

对不同线密度的聚对苯二甲酸乙二醇酯/聚对苯二甲酸丙二醇酯(PET/PTT)复合纤维分别进行干热处理,常压沸水处理,120℃及0.2MPa的高压沸水处理,研究了其热处理前后的力学性能。结果表明:PET/PTT复合纤维经常压沸水处理后,初始模量下降,断裂伸长率及断裂功增大,断裂强度略有减小;复合纤维经高压沸水处理后,其力学性能明显提高,常压沸水处理其次,干热处理则变化不大;复合纤维经干热处理后,其初始模量、断裂强度、断裂伸长率及断裂功随温度的升高均先升高后降低,150℃时达到最大。     

Effect of dopant precursors on the optical properties of rare-earths doped oxyfluoride glass-ceramics

The crystallization of fluoride nanocrystals (NCs) in chemically and mechanically stable aluminosilicate glasses has shown interesting optical properties even for small crystal fractions (10-15 wt%). When rare-earth (RE) ions are used as dopants, crystal-like features can be reproduced and an increase in the emission and/or energy transfer processes, with respect to the starting glasses, is observed. A crucial point for these materials is the study of the local surrounding of RE ions and their incorporation in the NCs. In fact, the effective concentration in the NCs can be much higher than the nominal concentration, up to one order of magnitude or even higher. The knowledge of RE ions incorporation in the NCs permits choosing proper doping levels to optimize both linear and nonlinear optical properties. In this work, transparent oxyfluoride glass-ceramics with LaF₃ NCs, doped with Nd³⁺ and Er³⁺ using oxide and fluoride precursors, were prepared using the melt-quenching method and controlled crystallization. The local surrounding of the RE ions was studied using X-ray absorption spectroscopy, electron paramagnetic resonance and photoluminiscence. The results show that most RE ions are already in a fluorine-rich amorphous environment even in the initial glass. The crystallization process provokes the RE ion redistribution and incorporation in the fluoride NCs. The different RE precursors, used as oxides or fluorides, have an influence on the incorporation of the RE in the NCs and, as a consequence, on the final optical properties.     

热处理工艺对石英纤维复合材料介电性能的影响

通过热处理温度、热处理气氛和防潮涂层对石英纤维增强复合材料介电性能影响的研究,结果表明:在800℃或500℃通氧条件下进行热处理,才可以较彻底的排除石英纤维增强复合材料中残余的游离碳。经高温处理后介电性能较好,进行防潮处理后能达到更好的效果,更好的应用于航天领域。     

热处理工艺对三元共聚聚酰亚胺纤维结构和性能的影响

采用傅立叶红外光谱(FTIR)、扫描电子显微镜(SEM)、声速取向、热重分析仪(TGA)等表征手段研究了热处理对湿法纺丝制备的3,3’,4,4’—二苯酮四酸二酐(BTDA)—二异氰酸甲苯酯(TDI)/二异氰酸二苯甲烷酯(MDI)三元共聚聚酰亚胺纤维结构与性能的影响。结果表明:热处理对纤维结构无明显影响;热处理使纤维表面更加致密,提高了纤维的取向度;与初生纤维相比,热处理之后纤维力学性能提高了近3倍,模量提高了2倍,同时热稳定性能得到了增强。     

锂渣掺量对水泥-减水剂浆体流变特性和混凝土性能的影响

本文研究了锂渣掺量对水泥-减水剂浆体流变特性、新拌混凝土工作性及硬化混凝土强度的影响。从紧密堆积理论和固体颗粒体积分数角度解释了锂渣掺量对水泥-减水剂浆体流变性能的影响。结果表明：锂渣水化初始的屈服应力和塑性黏度均随锂渣掺量的增加而增大,流变性能劣化。新拌混凝土的工作性与锂渣掺量呈负相关;随锂渣掺量的增加,7 d抗压强度不断降低,28 d抗压强度呈现出先增后降的趋势。     

Effect of Heat-Treatment Temperature on the Properties of a Lithium Aluminosilicate Glass

The effects of isochronal heat treatments on the properties of a lithium aluminosilicate glass have been measured. Heat treatment of the base glass at temperatures between 700° and 1100°C initially results in phase separation of the glass, followed by the formation of β-quartz solid solution ( ss ) at about 850°C. The β-quartz( ss ) converts to β-spodumene in the temperature range between 950°C and 1000°C. The dependence of the properties of the material on the heat-treatment temperature is controlled by phase separation below 850°C, by the rapid crystallization of β-quartz( ss ) between 850°C and 900°C, and by the lack of change in morphology with heat treatment above 900°C. The effects of heat treatment on the properties of this material are explained on the basis of the changes in the composition and morphology of the residual amorphous and crystalline phases.     

纤维表面处理对复合材料力学性能的影响

本文研究了碳纤维表面处理方法对纤维-基体界面剪切强度的影响．研究结果表明，相对于未进行表面处詈的碳纤维-所采用的胺基化处理和偶联剂处理两种表面处理方法都能够提高碳纤维界面的剪切强度，从而提高复合材料整体的抗拉强度和弹性模量。并且偶联剂处理方法具有更好的工艺性．     

热处理对MMT填充PP的力学性能影响

研究了热处理对聚丙烯(PP)/钠基蒙脱土(MMT)复合材料力学性能的影响。结果表明:适当地对共混体系进行热处理,可有效改善材料的拉伸性能、弯曲性能及冲击性能,拉伸强度及弯曲强度最大增幅分别可提高2 MPa和4 MPa。PP/MMT共混体系力学性能的增加在于体系中聚合物结晶结构的完善及热应力的消除。