Post about "sol-gel"

Porous Silicon Carbide Ceramic Prepared from Bamboo and Study on the Electromagnetic Wave Absorption Properties of It

After thousands of years’ natural evolution, wood and bamboo are endowed with unique structure and performance. After proper physical or chemical treatment, they can be used to prepare ceramic material with controllable structure and excellent performance and the structure and performance is programmable. At present the most reports in literature are to synthesize ceramic with wood. With the increasingly serious global environment problems, the enhancement of human environment protect consciousness and the startup of Chinese natural forest protect project, the conflict between supply and demand of domestic wood is increasingly serious. Bamboo can grow quickly, regenerate fast and easily and can be continually used after successful forestation. So it is an important approach to replace wood with bamboo to relax the conflict between supply and demand of wood and protect the environment.Ceramic block and powder of SiC was prepared through sol-gel and liquid silicon infiltration with bambusa arundinacea and bamboo charcoal powder as raw material. Wave-adsorption material was also prepared by the infiltration of magnetic metal. The phases, morphology and RAM reflectivity was characterized by XRD, SEM, EDX, TEM and RAM reflectivity testing system.Results show that the bamboo charcoal and the final SiC ceramics both inherit the porous microstructure of bamboo. The reaction from carbon to ceramic occurred mainly on the wall of the holes. Ceramic whiskers appear in some holes when using sol-gel method. The conversion rate from bamboo charcoal to SiC and the the degree of crystallization can be improved by increasing the reaction temperature and prolonging the time of the highest temperature in liquid silicon infiltration method. But the conversion rate can not be improved by increasing the reaction temperature and prolonging the time of the highest temperature in sol-gel method. The restrict factor of the conversion rate is the infiltration effect during the sol infiltration step. The conversion rate from charcoal to ceramic of bamboo charcoal powder is higher than bamboo charcoal block in whatever method. The porous ceramic with SiC whiskers in some holes prepared by sol-gel method show some electromagnetic wave adsorption properties in the low frequency band.

The Preparation, Characterization and Application of Doped TiO2 Photocatalyst

To improve photocatalytic ability of TiO2 catalyst, N or Fe ions were involved in the crystal of TiO2 via sol-gel method used urea or Fe(NO33·9H2O as the doping which brought the visible-light sensitization of TiO2 catalyst, and studied the different effect mechanism of nonmetal and metal doping. To evaluate the research of industrialisation application, the photooxidation of industrial waste was carried out in a series of experiments. The primary study was listed as following:(1) Calcined at 400℃in air atmosphere, as-prepared N/TiO2 catalysts are entirely anatase phase. The surface of as-prepared N/TiO2 catalyst is 109.1 m2·g-1. average pore size is 69.9 nm, and the grain pathway is about 17.7 nm. Better surface structural improve the adsorption power of the pollutants, and the catalysts show high photocatalytic activity. The optimum N-content in N/TiO2 is dertermined as 2.98 at.%. Moreover, the light absorption of as-prepared N/TiO2 shows red-shift to 435 nm, the band gaps is determined to be 2.85 eV. The nitrogen atom enters into the TiO2 lattice, occupies the position of oxygen atom, forms the bond of N-Ti-O, narrows the band gaps and makes as prepared N/TiO2 shifted into the visible ragion.(2) In as-prepared Fe/TiO2 catalysts, the optimum Fe-content is dertermined as 0.64 at.%. The Fe-doping not only depresses the grain growth of TiO2 particles, but also reduces the phase transformation temperature of anatase to rutile. Calcined at 300℃in air atmosphere, as-prepared Fe/TiO2 catalysts are anatase phase, the grain pathway is about 8 nm. The surface of as-prepared Fe/TiO2 catalysts is 91.3 m2·g-1, average pore size is 57.9 nm. The existence of Fe changes the surface structure of catalysts, which consequently reduces the chance of the recombination of the photoinduced electrons and holes. Calcined in air atmosphere at the temperature of 400℃, the light absorption of as-prepared Fe/TiO2 shows red-shift to 459 nm, the band gaps reduces to 2.7 eV. The promoting effect of Fe-doping on the photocatalytic activity could be attributed to the formation of intermediate energy level that allows Fe/TiO2 to be activated easily in the visible area.(3) In the multiphase photocatalysis reaction system, The application of photocatalysis is studied through the photodegradation of industrial waste diluted 1 times in oxygenated aqueous suspensions containing as-prepared TiO2. The experiment result shows: after 180 minutes’ photoreaction, the degradation rate of TOC is higher than 80%. The concentration of TOC falling demonstrated the organic pollutants in the industrial waste were photodegraded. The total carbon in the system falling is due to the final outcome CO2 departing from the reaction system, but TN has no change, this indicated the N element of the organic pollutants were not photodegraded to be N2. The 10% degradation rate of Pb2+ in the industrial waste is owing to the adsorption ability of the as-prepared photocatalyst.

The Preparation, Characterization and Application of Doped TiO2 Photocatalyst

To improve photocatalytic ability of TiO2 catalyst, N or Fe ions were involved in the crystal of TiO2 via sol-gel method used urea or Fe(NO33·9H2O as the doping which brought the visible-light sensitization of TiO2 catalyst, and studied the different effect mechanism of nonmetal and metal doping. To evaluate the research of industrialisation application, the photooxidation of industrial waste was carried out in a series of experiments. The primary study was listed as following:(1) Calcined at 400℃in air atmosphere, as-prepared N/TiO2 catalysts are entirely anatase phase. The surface of as-prepared N/TiO2 catalyst is 109.1 m2·g-1. average pore size is 69.9 nm, and the grain pathway is about 17.7 nm. Better surface structural improve the adsorption power of the pollutants, and the catalysts show high photocatalytic activity. The optimum N-content in N/TiO2 is dertermined as 2.98 at.%. Moreover, the light absorption of as-prepared N/TiO2 shows red-shift to 435 nm, the band gaps is determined to be 2.85 eV. The nitrogen atom enters into the TiO2 lattice, occupies the position of oxygen atom, forms the bond of N-Ti-O, narrows the band gaps and makes as prepared N/TiO2 shifted into the visible ragion.(2) In as-prepared Fe/TiO2 catalysts, the optimum Fe-content is dertermined as 0.64 at.%. The Fe-doping not only depresses the grain growth of TiO2 particles, but also reduces the phase transformation temperature of anatase to rutile. Calcined at 300℃in air atmosphere, as-prepared Fe/TiO2 catalysts are anatase phase, the grain pathway is about 8 nm. The surface of as-prepared Fe/TiO2 catalysts is 91.3 m2·g-1, average pore size is 57.9 nm. The existence of Fe changes the surface structure of catalysts, which consequently reduces the chance of the recombination of the photoinduced electrons and holes. Calcined in air atmosphere at the temperature of 400℃, the light absorption of as-prepared Fe/TiO2 shows red-shift to 459 nm, the band gaps reduces to 2.7 eV. The promoting effect of Fe-doping on the photocatalytic activity could be attributed to the formation of intermediate energy level that allows Fe/TiO2 to be activated easily in the visible area.(3) In the multiphase photocatalysis reaction system, The application of photocatalysis is studied through the photodegradation of industrial waste diluted 1 times in oxygenated aqueous suspensions containing as-prepared TiO2. The experiment result shows: after 180 minutes’ photoreaction, the degradation rate of TOC is higher than 80%. The concentration of TOC falling demonstrated the organic pollutants in the industrial waste were photodegraded. The total carbon in the system falling is due to the final outcome CO2 departing from the reaction system, but TN has no change, this indicated the N element of the organic pollutants were not photodegraded to be N2. The 10% degradation rate of Pb2+ in the industrial waste is owing to the adsorption ability of the as-prepared photocatalyst.

Preparation of Triethylamine Modified Titanium Dioxide Film in Normal Temperature and Its’ Photocatalytic Performance Study

The problem of environment and energy become more and more serious now.All over the world focus the problem and try to deal it.Titanium dioxide,as an excellent photocatalytic materials is researched thoroughly because of low price,non-toxic,high catalytic efficiency and easy to operate.However,weak visible spectral response and fast recombination rate of photo-generated electron-hole pair limits its application in practice.So the research to enhance the visible light activity is very important in this field.N-doped was a possible method to improve its’ visible light activity.The process of high-heat treatment limited the application of TiO2.Based on the actuality,the preparation and properties of triethylamine modified titanium dioxide film in room-temperature was posed in this paper.The TiO2-sol in anatase phase was synthesized at room temperature through sol-gel method.In this study,butyl titanate was used as precursor,ethanol as impregnate and HCl as catalyzer.Then under violent agitating,the triethylamine was used as modifying agent to be doped into the TiO2 solution.The dosage and temperature were changed to look for the optimum.Triethylamine with butyl titanate was used as a precursor to prepare Triethylamine modified TiO2-sol.The TiO2 films were prepared by the dip-coating for thrice used the solutions prepared as above.After that,the crystal structure and the photocatalytic efficiency of the samples completed were tested through XRD,SEM,TEM,Volume analyzer,UV-Vis,FT-IR.The research results were shown below:Firstly,the modified TiO2 sol remained be anatase crystalline,the difference is that the TiO2 modified as Triethylamine doped later has a better property than the one doped with butyl titanate.Secondly,when the pH of sol was change to neutral as Triethylamine doped the TiO2-sol show out worst stability.Then it will re-stable as Triethylamine being kept on doping.But it won’t improve the visible light photocatalytic ability.The mass ratio of m (Triethylamine):m(butyl titanate)reaches to 1:1 show out to be the best.As the temperature rises,the modified TiO2 displays better visible-light absorptivity even though the volume of particle growth quite fast because of the high temperature,which weaken the photocatalytic ability.From above,the optimum temperature was 65℃and modified TiO2 flims showd the best photodecomposition performance. The modified TiO2 perform better visible-light absorptive than the pure TiO2.At the same time,the modified TiO2 has better photocatalytic activity than the pure one from the degradation of Rhodamine B under visible-light.The degradation speed constant is seven times more than the pure one.The modified TiO2 remind has a steady catalytic activity in long-last experiment.

Study on the Synthesis of AcetylTri-n-ButylCitrate and Pilot Design

AcetylTri-n-ButylCitrate is one kind of outward appearance colorless transparent liquid. It is be internationally recognized as an non-toxic plasticizer at present, In opposite to the traditional phthalic acid ester plasticizer it is green environmental protection merit in professions and so on be widely applied in medicine health, food packing, child toy, having the broad prospects for development. Take the citric acid as raw material, through the esterification and the acylation responded that synthesizes ATBC is the general synthetic method. The key lies in selects the appropriate catalyst to guarantee the product’s purity and luster, and reduction production cost as far as possible. This article studies’ innovation lies in take the solid acidify as the esterification reaction’s catalyst, take NaHSO4 as the acylation reaction’s catalyst, finally obtained the product purity is not only high, moreover solved the formerly question that decolorized difficultly. The catalyst easy to separate, the redundant use is simple, and the stability is good. In obtained each technological parameter under the condition to carry on the experimental line design.First, this article introduced in the plasticizer’s application and the present world’s production and the demand status, then had carried on the narration to the new non-toxic plasticizer ATBC’s nature research and the production status of domestic and foreign. From this may see, ATBC compares the similar products to have the obvious superiority, the development potential is big, especially in domestic, designs a reasonable industry production line to have the very realistic significance.Second, uses the sol-gel law load phosphorus tungsten to prepare the most effective solidification acid catalyst to use in the esterification response. The findings indicated that the solidification acid catalysis’ effect factor to be many. In the fixed phospho-wolframic acid solution and under the hydrochloric acid density condition, explored each kind of factor take the esterification rate as the target to solidify the acid catalysis effect the influence, obtained the ideal catalyst. By 2 g phospho-wolframic acid idea, dissolves with 3 ml distilled water, joins the catalyst activeness which 1 mol/l the hydrochloric acid 3 ml systems result to be the best. Under the same esterification condition obtains, the solid acidify’s activation temperature should in 110℃-200℃, the best capacity be 10%. Under the above condition the catalyst esterification rate is high, repeatedly used 7 still had the suitable activeness from now on.Third, in had determined in each step response catalyst’s foundation, studies the ATBC synthesis craft route with the orthogonal tests method, and determines the pilot experimental technological parameter through the confirmation experiment, the optimum esterification conditions were determind as follows:molar ration of citric acid to butyl alcohol is 1:4,the mass of catalyst is 3%(based on citric acid),solid quantity is 1/10,reaction time is 4 hours. Mid-product purity is high, the luster is good. Select NaSO4 as the acylation reaction catalyst. After the reaction fluid’s temperature decreased, the catalyst can be separated by the solid state, the response condition be temperate. The technological conditions are: The batch feeding ration (TBC and acid anhydride mole of ratio) 1:1.5, the catalyst amount used 5%, the reaction temperature 70℃, the reaction time is 60min. After reduced pressure distillation recycling acid anhydride, again menses and soda lye wash, after two reduced pressure distillation, the obtained product index of refraction is 1.4429, the purity reaches 99.2%, has achieved the quality requirement.Fourth, obtains the technological conditions through the above experiment, carried on the yearly produced 60 ton ATBC experimental lines’ design, and carried on the computation to the material and the quantity of heat. This experimental line production method is the batch operation, the construction cost is low, the simplify operation, Hopefully to realize the industrialization.

Study on the Ceramic Flame Retardant Poplar Plywood

As China’s rapid economic development, people’s increasing demand for wood products, to ease the contradiction between supply and demand for wood, the state vigorously develop the plantation cultivation. However, the lack of natural wood plantations is limit to the scope of application of wood products, how to improve the nature of wood, to expand the use of plantations and increased utilization of wood into value-added is the issue requiring to be solved.In this paper, to solve the problems of fast-growing poplar plantation material soft and easy to burn, low hardness, poor size stability, wear poor resistance shortcomings, through Sol – gel method, fix fire-retardants and Sol-Gel together, the method used vacuum pressure Poplar veneer of a soaking with the Poplar veneer of impregnating conditions and burning effects were studied to determine the appropriate conditions for dealing with soaking through orthogonal experimental design, preparation of a ceramic Flame Retardant plywood, and product’s Physical performance indicators and the performance of combustion testing and analysis, select the best process; do a simple analysis with product’s application and promotion.The main conclusions of the study are as follows:1. With the increase in vacuum pressure time, the poplar wood veneer’s weight gain rate of increase in the 0.5 h, when the rate of weight gain can achieve the desired results;2. Differential scanning calorimeter (DSC) analysis showed that the Flame Retardant plywood ceramic thermal decomposition of the DSC is divided into three peaks, that is a endothermic peak, the two exothermic peak. Ordinary plywood and ceramics Flame Retardant plywood DSC curves in 65℃, due to evaporation have a endothermic peak and peak are negative, in the first exothermic peak, with an increase rate of weight gain, temperature of the extension exothermic peak is postponed, plywood from the 336.87℃, gradually deal with Flame Retardant plywood until after the 342.75℃; peak in the second heat, the peak temperature after the extension is the same, but the Flame Retardant effect more evident than the veneer, 455.25℃after the extension to 515.19℃.3. If oxygen index of ceramics the Flame Retardant plywood achieved flame retardant materials B1-level requirements, have Flame Retardant effect significantly. Variance analysis showed that Flame Retardant on the Flame Retardant plywood results in the 0.05 is significant impact, the Flame Retardant effect can be applied to all types of industrial and civil engineering structure used in all kinds of materials and decoration materials. 4. Ceramic Flame Retardant treatment of the plywood, glue bond strength is higher than the national standard. The proportion of Flame Retardant is on the level of 0.01, theglue bond strength have a very significant impact, and in the level of 0.05 cases significantly, in the level of 0.10 glue bond strength glue consumption have a significant impact on glue bond strength, the processing time was not obvious.Compare with poplar plywood general Modulus, ceramics Flame Retardant plywood MOE increased by 27 percent.5. Through the integrated score, considering the ceramics of Flame Retardant plywood mechanical properties and Flame Retardant properties, optimized the best combination of technology, according to the sort of impact on the size, the ratio of six percent for the flame retardants, sizing of 270 g / m2, processing time of 0.2 h is the best one.Ceramics Flame Retardant wood can be used for building decoration materials, furniture manufacturing, engineering, public places and other parts, can also be used as a special fire-retardant, anti-corrosion-and-pest materials. Ceramics Flame Retardant treatment is an integrated technology, and have a important significance for improving the performance and value-added timber, promote wood processing technological progress, expand the application of timber plantations, timber conservation and protection of ecological environment.

Sol-gel Method Preparation and Performance Testing of High Temperature Resistance and Porous Low Dielectric Constant Material

There is an increasing interest to develop low dielectric constant and low loss materials that can operate in the GHz range for wireless telecommunication systems. One of these new materials are BN/SiCO composite ceramics which arouses people’s widespread interest.Therefore, In this paper, the preparation and property of BN / SiCO, a kind of organic – inorganic compound porous material,is studied in detail.The porous low BN/SiCO were prepared by using sel-gel and pyrolysis. BN/SiCO composite ceramics having a dielectric constant,ε, as low as 2.1 have been made by pyrolysis of filled gels at temperature 1000°C . Such a low value ofεis supposed to be due to a combination of factors: the lowεof BN and of SiCO itself and the high amount of residual porosity present in the samples. The porous microstructure– and the related dielectric properties– obtained at 1000°C show a very good stability. This result has been ascribed to the high viscosity of the SiCO glass and to the platelet shape particles of BN. Both factors hinder the sintering and prevent the closure of the pores. We systematically and comparatively studied the properties of the BN/SiCO, such as preparation, microstructure, chemical bond state, and electrical and mechanical properties. in this paper, the technics of sel-gel is emphasizely illuminated in detail, besides, the experiment flow and the impact of various conditions on experiment result is introduced. The results of SEM indicate that the pore size is 4nm, and the sample have the uniform hole distributing.The electrical and porosity of the BN/SiCO are analyzed by HP test instrumentation and BET test instrumentation, we analyzed the sample chemical bond by the way of FTIR-ATR. The results of the test shows that porous BN/SiCO has good properties, the sample is good at the low dielectric.

Sol-gel Method Preparation and Performance Testing of High Temperature Resistance and Porous Low Dielectric Constant Material

There is an increasing interest to develop low dielectric constant and low loss materials that can operate in the GHz range for wireless telecommunication systems. One of these new materials are BN/SiCO composite ceramics which arouses people’s widespread interest.Therefore, In this paper, the preparation and property of BN / SiCO, a kind of organic – inorganic compound porous material,is studied in detail.The porous low BN/SiCO were prepared by using sel-gel and pyrolysis. BN/SiCO composite ceramics having a dielectric constant,ε, as low as 2.1 have been made by pyrolysis of filled gels at temperature 1000°C . Such a low value ofεis supposed to be due to a combination of factors: the lowεof BN and of SiCO itself and the high amount of residual porosity present in the samples. The porous microstructure– and the related dielectric properties– obtained at 1000°C show a very good stability. This result has been ascribed to the high viscosity of the SiCO glass and to the platelet shape particles of BN. Both factors hinder the sintering and prevent the closure of the pores. We systematically and comparatively studied the properties of the BN/SiCO, such as preparation, microstructure, chemical bond state, and electrical and mechanical properties. in this paper, the technics of sel-gel is emphasizely illuminated in detail, besides, the experiment flow and the impact of various conditions on experiment result is introduced. The results of SEM indicate that the pore size is 4nm, and the sample have the uniform hole distributing.The electrical and porosity of the BN/SiCO are analyzed by HP test instrumentation and BET test instrumentation, we analyzed the sample chemical bond by the way of FTIR-ATR. The results of the test shows that porous BN/SiCO has good properties, the sample is good at the low dielectric.

Preparation and Low Temperature Treatment in N2 of Conducting ZnO Films by Sol-gel Method

ZnO film, a semiconductor with wide direct band gap, has been actively studied because of its potential applications. It can be used in solar cell, piezoelectric device, photoelectric device, gas sensor and UV detector and the characteristics can be modulated by appropriate doping. The transparent ZnO conductive thin films doped with suitable dopants have excellent optical and electrical properties, and are applied widely as transparent and conductive oxide electrodes in various electrical and optical devices including liquid crystal display, solar cell and so on.In this paper, the primary objective is researching the stability in N2 of ZnO flims doped with Al by sol-gel and the influence of dopant concentration and the number of coating on the conductivity and transmittance of ZnO films doped with Li by sol-gel. ZnO thin films doped with Al3+,Li+ were prepared on microslides by sol-gel method successfully. The sol was prepared with 2-methoxyethanol as solvent, Zincacetate as precursor and MEA as stabilizer. The mixture was heated, stirred to obtain the sol, and then homogenous transparent ZnO thin films were prepared from the sol by dipping, drying, pre-heat treatment in air and annealing in N2 atmospheres.XRD, SEM, XPS and Four-Point probe method were used to characterize the structure and optical and electrical properties of the ZnO thin films. The results showed that the kind of dopant, dopant concentration, temperature of pre-heat treatment, the number of coating and annealing atmosphere had influence in various extents on the photoelectric performance of the doped ZnO thin films. Increasing the dopant concentration could reduce resistivity of thin films, but over high dopant concentration would increase the resistivity. The difference of dopants has great influence on the stability of films annealed in N2; the stability of ZnO flims doped with Al is good but that doped with Li is bad. Increasing the number of coating could increase the thickness of thin films, which would reduce the resistivity and the transmittance within the range of visible light. The transmittance of thin films in the range of visible light was not impacted greatly by different dopant concentrations and annealing atmosphere. The different atmospheres can directly influence the electric conductivity. The film with low resistivity can be obtained by heat treatment in N2 at 300℃. In this experiment, the surface configuration of the films is compact, the sizes of crystal grain is uniform, the lowest sheet resistance is 270?/□and the maximum transmittance within the range of visible light is about 83%. The optimum technological parameters for AZO and LZO thin film by sol-gel are as follows: the sol concentration is 0.6 mol/L; the dopant concentrations of Al and Li are 1at% and 2.3at%, respectively; the number of coating is 15 and 10, respectively; the pre-heat treatment temperature is 450℃and the annealing temperature is 550℃in air, 300℃in N2.

Preparation of New Hybrid SiO2 Gel and Investigation on the Coating’s Oxidation Resistance

Silicon dioxide coating as an important kind of thermal protecting coatings is widely used in TransAtmospheric Hypersonic Vehicle’s thermal protection system because of its high melting point and high mechanical strength.According to traditional method’s high cost and high preparation requirement, author produced Boron-doped silicon dioxide coating by hybrid sol-gel method to obtain the ability of high toughness, low cost and more oxidation resistance.DTA and FTIR are used to analyze transformation mechanism of the hybrid gel under heat treatment process. According to the transformation, author establishes a proper gel-solidifying heat treatment technics. Then the interface between gel layer and matrix is studied by SEM, we get information of layer and matrix’s combining condition and analyze the reason of some elements’diffusion phenomenon. XPS and XRD are used to confirm Mullite phase on the layer’s surface. Oxidation resistance measurement and orthogonal test are set to analyze the effect of the concentrations of tetraethoxysilane (TEOS), Solvent A, Solvent B and boracic acid, ultimately the optimum concentration of the sol is obtained.The results indicates that, under heat treatment the gel occurs to dehydrate at a low temperature, then the organic components of the gel decompound during 400℃to 650℃. Under high temperature for a long time, Al and Mn exists in the matrix will diffuse to the gel layer and get enrichment, moreover, Al can be oxidated on the surface. The optimum concentration of the sol (TEOS 87.5g for one sample) is: B 10%, Additive T 15ml, Solvent A 25ml, Solvent B 15ml.