纳米晶须的合成及其性能的研究
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摘要
本论文中,以硼砂和锌盐为主要原料,通过简单的液相法,首次一步原位制备出晶态疏水性的纳米硼酸锌晶须。用磷酸酯作表面改性剂,降低了硼酸锌纳米粒子的表面能,提高了与聚合物之间的相溶性。用X-射线衍射(XRD)、透射电子显微镜(TEM)以及差热—热重(DTA-TGA)等分析手段,考察了产物粒子的形貌、成分、尺寸等。并讨论了可能的反应过程、溶液不同的pH对产物的影响以及反应温度对产物粒度的影响。
将合成的不同形貌的硼酸锌颗粒添加到聚乙烯中进行复合,考察了此复合材料的热力学稳定性。从电镜照片中可以看出,硼酸锌晶须与聚乙烯可以很好的复合,在试验过程中,硼酸锌颗粒很好的溶入到了聚乙烯中,根据相似相溶原理,也可以理解为,产物具有了很好的疏水性,所以与无极性的有机物分子可以很好的相溶。硼酸锌晶须的加入,使复合后的硼酸锌/聚乙烯有着较好的热力学稳定性,分解温度提高了将近150度,在此基础上,考察了此反应的反应机理,相关的活化能的变化,从理论上证明了此复合物的热稳定性的真实可靠。
同时,考察了掺杂后的硼酸锌的光学性能,不同浓度激活离子铕离子的掺杂,对硼酸盐纳米发光材料性质具有很大的影响。虽然对以硼酸盐为基质的纳米发光材料的发光性质的研究有很多,本论文中掺杂后材料的发光性能有了很大程度的提高,通过实验,得出结论Eu掺杂的硼酸锌纳米晶体得到了Eu的最佳掺杂量为摩尔5%掺杂,最佳反应时间为6-8h,最佳反应温度为60℃,虽然还做了反滴以及加入表面活性剂的实验,但是对实验结果并没有明显的影响,可喜的是产物经400℃烧结后发光性能能够达到工业应用标准。在此基础上,从发光机理上讨论这种改变。
以硼砂和硫酸铜为主要原料,通过简单的液相法,首次一步原位制备出晶态疏水性的水合硼酸铜晶须。用磷酸酯作表面改性剂,降低了硼酸铜纳米粒子的表面能,通过温度的变化,实现对形貌的控制。用X-射线衍射(XRD)、透射电子显微镜(TEM)、以及差热—热重(DTA-TGA)等分析手段,考察了产物粒子的形貌、成分、尺寸等。通过对硼酸铜合成实验条件的探讨,总结了反应过程中,粒子的形成过程,探讨了此实验的反应机理。同时,将硼酸铜添加到基础油中,改性后的硼酸铜与基础油有着很好的相容性,说明经过实验大大地改善了无机粒子与有机物之间的相容性,使无机粒子能够很好地分散在有机溶液中,解决了无机粒子在油相中难以均匀分散的问题。同时,大大降低了基础油的摩擦系数。
无论是硼酸锌的制备还是硼酸铜的合成,在制备过程中,都遇到了相同的问题,滤液中含有大量的硫酸钠。在我国许多的工业生产中,都有大量的硫酸钠排放,对环境产生了很大的污染。因此,本论文中,希望可以找到解决方法。我们以硫酸钠为原料,试着合成工业上所需要的硫酸钙晶须,以便对硫酸钠进行回收再利用。
The crystal and hydrophobic zinc borate nanowhiskers were successfully prepared by a wet method using borax and zinc salts as raw materials in situ aqueous solution, and phosphate ester as the modifying surface agent. Surface energy of zinc borate nanoparticles was reduced, and the comparability between zinc borate nanoparticles and polymers was enhanced.The morphology, composition, diameter, size, differential thermal and weight loss of zinc borate particles were measured by X-ray diffraction (XRD), transmission electron microscopy (TEM) equipped with an energy-dispersive X-ray spectrometer(EDS), and differential thermal and thermogravimetric analysis (DTA-TGA) in air. The possible reaction route, the different pH values of the solution on synthesis of pure zinc borate and the reaction temperature on the size of zinc borate were discussed.
The different shape of zinc borate will be added to the polyethylene, we investigated the thermodynamics stability of the composite material. We can see that zinc borate whiskers can be well composited with PE through our experiment from the electron micrograph. Zinc borate particles can be well infused into polyethylene. According to the similar phase, we also can include that the products have very good hydrophobicity, so they will be easily dissolved with organic molecules. The compound of zinc borate/polyethylene has perfect stability with adding the zinc borate, and the thermodynamics decomposition temperatures have been increased nearly 150 degrees. Therefore, we investigated the reaction mechanism, and the changes of related activation energy. This will be proved theoretically.
At the same time, we also investigated the optical properties of zinc borates. The different concentrations of activation ion Eu ions doped have great effects the the luminescent properties of the materials. Although there are a lot of reports for the research of materials luminescence properties of borate for the matrix, the material luminous property has been improved largely in my experiments. It is concluded that the best doping quantity of Eu doped zinc borate nanocrystal is 5%, and the optimum reaction time for 6-8 hours, and the best reaction temperature for 60℃. We also attempted to reverse drops and change surfactants, but the results of the experiments have not successed. The good news is that the properties of products can achieve industrial application standards with 400℃sintering. Then, we discussed the mechanism about this change.
The crystal and hydrophobic copper borate nanowhiskers were successfully prepared by a wet method using borax and bluestone as raw materials in situ aqueous solution, and phosphate ester as the modifying surface agent. The morphology, size, and differential thermal-thermogravimetric situation have been investigated by the X-ray diffraction (XRD), transmission electron microscope (TEM), and differential thermal-thermogravimetic analysis (DTA-TGA) analysis method. Based on the discussion of experimental condition, we have summarized the reaction process, particle formation process and the reaction mechanism of this experiment. Meanwhile, we add copper borate to the base oil, and the modified copper borate can be easily mixed with organic materials, which can show us greatly capability of dispersing with organic matter, and solve the difficult problem the uniform dispersion of inorganic polymer particles, and also can greatly reduce the friction coefficient of the base oil.
No matter what the preparation of zinc borate or copper, we have met the same question that there is plenty of the filtrate of sodium sulfite during the experiments. In our country, there are a large number of sodium discharges in industrial production, which bring the great pollution to the environment. Therefore, we hope to find the way to solve this problem in my thesis. We try to use the sodium sulfate as the raw material to react with calcium salt to synthesize calcium sulfate whiskers, which have been largely needed in the industry, and also recycle and reuse sodium sulfate.
将合成的不同形貌的硼酸锌颗粒添加到聚乙烯中进行复合,考察了此复合材料的热力学稳定性。从电镜照片中可以看出,硼酸锌晶须与聚乙烯可以很好的复合,在试验过程中,硼酸锌颗粒很好的溶入到了聚乙烯中,根据相似相溶原理,也可以理解为,产物具有了很好的疏水性,所以与无极性的有机物分子可以很好的相溶。硼酸锌晶须的加入,使复合后的硼酸锌/聚乙烯有着较好的热力学稳定性,分解温度提高了将近150度,在此基础上,考察了此反应的反应机理,相关的活化能的变化,从理论上证明了此复合物的热稳定性的真实可靠。
同时,考察了掺杂后的硼酸锌的光学性能,不同浓度激活离子铕离子的掺杂,对硼酸盐纳米发光材料性质具有很大的影响。虽然对以硼酸盐为基质的纳米发光材料的发光性质的研究有很多,本论文中掺杂后材料的发光性能有了很大程度的提高,通过实验,得出结论Eu掺杂的硼酸锌纳米晶体得到了Eu的最佳掺杂量为摩尔5%掺杂,最佳反应时间为6-8h,最佳反应温度为60℃,虽然还做了反滴以及加入表面活性剂的实验,但是对实验结果并没有明显的影响,可喜的是产物经400℃烧结后发光性能能够达到工业应用标准。在此基础上,从发光机理上讨论这种改变。
以硼砂和硫酸铜为主要原料,通过简单的液相法,首次一步原位制备出晶态疏水性的水合硼酸铜晶须。用磷酸酯作表面改性剂,降低了硼酸铜纳米粒子的表面能,通过温度的变化,实现对形貌的控制。用X-射线衍射(XRD)、透射电子显微镜(TEM)、以及差热—热重(DTA-TGA)等分析手段,考察了产物粒子的形貌、成分、尺寸等。通过对硼酸铜合成实验条件的探讨,总结了反应过程中,粒子的形成过程,探讨了此实验的反应机理。同时,将硼酸铜添加到基础油中,改性后的硼酸铜与基础油有着很好的相容性,说明经过实验大大地改善了无机粒子与有机物之间的相容性,使无机粒子能够很好地分散在有机溶液中,解决了无机粒子在油相中难以均匀分散的问题。同时,大大降低了基础油的摩擦系数。
无论是硼酸锌的制备还是硼酸铜的合成,在制备过程中,都遇到了相同的问题,滤液中含有大量的硫酸钠。在我国许多的工业生产中,都有大量的硫酸钠排放,对环境产生了很大的污染。因此,本论文中,希望可以找到解决方法。我们以硫酸钠为原料,试着合成工业上所需要的硫酸钙晶须,以便对硫酸钠进行回收再利用。
The crystal and hydrophobic zinc borate nanowhiskers were successfully prepared by a wet method using borax and zinc salts as raw materials in situ aqueous solution, and phosphate ester as the modifying surface agent. Surface energy of zinc borate nanoparticles was reduced, and the comparability between zinc borate nanoparticles and polymers was enhanced.The morphology, composition, diameter, size, differential thermal and weight loss of zinc borate particles were measured by X-ray diffraction (XRD), transmission electron microscopy (TEM) equipped with an energy-dispersive X-ray spectrometer(EDS), and differential thermal and thermogravimetric analysis (DTA-TGA) in air. The possible reaction route, the different pH values of the solution on synthesis of pure zinc borate and the reaction temperature on the size of zinc borate were discussed.
The different shape of zinc borate will be added to the polyethylene, we investigated the thermodynamics stability of the composite material. We can see that zinc borate whiskers can be well composited with PE through our experiment from the electron micrograph. Zinc borate particles can be well infused into polyethylene. According to the similar phase, we also can include that the products have very good hydrophobicity, so they will be easily dissolved with organic molecules. The compound of zinc borate/polyethylene has perfect stability with adding the zinc borate, and the thermodynamics decomposition temperatures have been increased nearly 150 degrees. Therefore, we investigated the reaction mechanism, and the changes of related activation energy. This will be proved theoretically.
At the same time, we also investigated the optical properties of zinc borates. The different concentrations of activation ion Eu ions doped have great effects the the luminescent properties of the materials. Although there are a lot of reports for the research of materials luminescence properties of borate for the matrix, the material luminous property has been improved largely in my experiments. It is concluded that the best doping quantity of Eu doped zinc borate nanocrystal is 5%, and the optimum reaction time for 6-8 hours, and the best reaction temperature for 60℃. We also attempted to reverse drops and change surfactants, but the results of the experiments have not successed. The good news is that the properties of products can achieve industrial application standards with 400℃sintering. Then, we discussed the mechanism about this change.
The crystal and hydrophobic copper borate nanowhiskers were successfully prepared by a wet method using borax and bluestone as raw materials in situ aqueous solution, and phosphate ester as the modifying surface agent. The morphology, size, and differential thermal-thermogravimetric situation have been investigated by the X-ray diffraction (XRD), transmission electron microscope (TEM), and differential thermal-thermogravimetic analysis (DTA-TGA) analysis method. Based on the discussion of experimental condition, we have summarized the reaction process, particle formation process and the reaction mechanism of this experiment. Meanwhile, we add copper borate to the base oil, and the modified copper borate can be easily mixed with organic materials, which can show us greatly capability of dispersing with organic matter, and solve the difficult problem the uniform dispersion of inorganic polymer particles, and also can greatly reduce the friction coefficient of the base oil.
No matter what the preparation of zinc borate or copper, we have met the same question that there is plenty of the filtrate of sodium sulfite during the experiments. In our country, there are a large number of sodium discharges in industrial production, which bring the great pollution to the environment. Therefore, we hope to find the way to solve this problem in my thesis. We try to use the sodium sulfate as the raw material to react with calcium salt to synthesize calcium sulfate whiskers, which have been largely needed in the industry, and also recycle and reuse sodium sulfate.
引文
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