Preparation And Characterization Of Low Temperature Ceramic Bond With Glass Material By Sol-gel Method

Traditional preparation methods of ceramic glass, mostly by high temperature melt cooling method, using this method is of high temperature, and easy to cause uneven of the components between the glass phase, phase. Currently, in terms of preparation of low temperature ceramic frit, compared with traditional melt-cooling method, developed in recent years the sol-gel（Sol-Gel,SG） technology has many advantages: component mixing uniformity, high purity, reaction under the lower temperature, the simple equipment, low production cost, simple operation, controllable particle size, easy to realize industrialized production, etc. At present, the sol-gel technique has been successfully applied in the preparation of fiber, functional ceramics, microcrystalline glass material, coated film,etc.,aspects of multi-component oxide composite material for the application of conventional techniques are difficult to prepare, superconducting materials, SG with the new technology also try and break.Based on the reference to a number of domestic and foreign literature, this paper mainly studies the sol-gel method of low temperature ceramic bond with technological parameters and technological process of the glass. The main contents include: based on the comparison of the various process parameters and the reaction way, such as reaction temperature, reaction time, concentration of each material, calcining temperature, calcining time and pH, etc.,confirmed with organic alcohol salt zinc acetate（Zn（Ac）2·2H2O）, ethyl orthosilicate（TEOS）and boric acid（H3BO3） as precursors, ethanol（EtOH） and deionized water as the solvent,hydrochloric acid（HCl） as catalyst, prepared by sol-gel method ZnO-B₂O₃-SiO₂ glass frit, and the factors that affect the preparation process were studied, and the samples prepared by thermal gravimetric analysis, FTIR analysis, XRD analysis were characterized, and its flexural strength, thermal expansion coefficient, hardness, and other performance were tested.The results show that:（1） Sol-gel technique for preparing the best optimum conditions ZnO-B₂O₃-SiO₂ as:incubation temperature is 40℃, the amount ofwater is about 150 g, catalyst for hydrochloric acid, pH value of 4.5, stirring time is 80 min,drying temperature is 80℃, and the resulting gel was calcined 3 h at 730℃.（2） when the zinc content is 30%, glass material at 684℃ can precipitate grain, under 730℃ temperature forms stable Zn2SiO4 and little scale quartz SiO₂ phase, small grain size of 39.0 nm, with the increase of heat treatment temperature, precipitation phase species did not change, the increase of grain size have obvious.（3） the more content of zinc, the more easily precipitate Zn2SiO4 and Zn4B6O13 crystalline phase, as the temperature rises, metastable crystalline phase state Zn3B2O6 happened to steady-state Zn4B6O13 phase transformation. Glass material of the preparation of the bending strength of 40MP; thermal expansion coefficient of 3.50 x 10-6 /℃.