不同酸碱度水热法可控制备硅基纳米材料及氢氧化镍纳米片的研究
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摘要
在当今世界,对材料的尺寸要求越来越小；随着科技发展对新型及传统材料的性能要求也越来越高。由于一维硅纳米材料特殊的晶体构造以及新奇的光、电学特性,目前被普遍认为是一种极具潜力的半导体材料。
本课题组已采用水热法制备了硅纳米管,但在制备硅纳米管时,仅采用纯水作溶剂,采用水热法制备硅纳米材料时,溶液的酸碱度是硅纳米材料形成过程中重要的因素,为了解决这一问题并揭示纳米材料在水热环境中的生长机理,本论文着重研究了不同溶液pH值对于纳米材料生长的影响。我们展开了以下几个方面的研究,首先在不同酸碱度条件下,研究原料前驱物溶液的黏度、粒度以及ζ电位的变化规律。通过实验结果分析认为,当溶液的pH值为3-6时,原料的分散程度较好。接下来,在酸性条件下制备出了硅纳米线,典型的实验条件为pH=6、470℃、8MPa、保温4h,硅纳米线平均直径约为80nm,纳米线的外层有无定形氧化硅外层。值得注意的是,当pH=5时,得到一种在高能电子束照射下产生变形的硅纳米线,高分辨电镜观察发现这种纳米线是由分散的纳米颗粒组成,颗粒之间的空隙由无定形氧化物填充。通过分析酸性环境制备硅纳米线的实验结果,我们认为纳米线的生长过程存在两个阶段,一是成核阶段,在这一阶段成核大小受酸碱度的影响较大。二是纳米线生长阶段,在这一阶段遵循“氧化物辅助生长机制”。随着温度的升高,晶核内不断析出晶体硅,在某个特定方向上,氧扩散能力弱,使得在此方向上不断析出晶体硅,保证了晶核沿一维方向生长。水热法在中性条件下能生长出硅纳米管,而在酸性条件仅能生长出硅纳米线,产生这样结果的原因是溶液的酸碱度对硅纳米材料的成核和生长产生了影响。为了研究这-变化的规律,利用第一性原理计算模拟,从理论角度研究硅纳米管的稳定性。研究发现表面不存在Si-H键的硅纳米管易于塌陷,最终形成线状结构。而表面存在Si-H键的硅纳米管相对稳定。
调节水热溶液为碱性,结果显示,在碱性环境下能制备出氧化硅纳米球,典型的实验条件为pH=9、350℃、14MPa、保温4h。纳米球表面光滑,直径分布均匀,且纯度较高,随着pH值的升高,纳米球粒径呈现单调增长。在达到反应温度以后,氧化硅纳米球的粒径随着保温温度的升高而增大。氧化硅纳米球的粒径还会随着压力的增加而减小,这与硅纳米线直径与压力的关系一致,论文在4章中给出了pH值、温度、压力对粒径影响的详细机理分析。氧化硅纳米球具有良好的光致发光特性。样品的红外光谱显示,纳米球的表面存在Si-OH键以及Si-O-Si.通过碱性环境中的实验结果分析,在碱性环境中原料溶解后形成的硅酸根单体增加,同时碱性环境中存在的大量OH-离子进入成核中心形成Si-OH键,随着反应的进行硅酸根单体Si-OH之间形成Si-O-Si链,最终形成氧化硅纳米球。碱性环境中大量存在的OH-是无定形氧化硅颗粒生成的主要原因。
另外,在中性和碱性的实验中我们意外地收集到一种无定形氧化硅纳米线,这种纳米线在反应釜顶端能够收集到,直径分布很广,从数十纳米到数微米不等。TEM分析表明氧化硅纳米线是一种非晶结构。在酸性环境下,这种纳米线无法生成,当pH≥7时,随着pH值的升高纳米线的直径明显增加。初步认为这种无定形纳米线的生成是受到温度梯度的影响。论文第4章详细讨论了其中机理。
最后,尝试采用水热法制备其他纳米材料,使用Ni为原料,研究水热工艺条件对其生长的影响。实验得到的产物为氢氧化镍纳米片。典型实验条件为：pH=7,470℃,9MPa、保温时间4h。得到的氢氧化镍纳米片的厚度约为30nm,直径大约为150nm,纳米片聚集成球状。水热溶液酸碱度对产物的影响主要表现在酸性环境下无法形成氢氧化镍纳米片,当pH值大于7时,随着pH值的升高,纳米片的晶粒尺寸有先减小后增加。
综上所述,本文通过理论结合实验研究不同酸碱度条件下水热制备硅纳米材料的形成过程。着重从实验角度研究在不同酸碱度条件下硅纳米材料在水热环境中的形成过程。通过实验研究发现,在酸性环境下得到的为晶体硅纳米线,而在碱性环境下得到的产物为无定形氧化硅纳米球和氧化硅纳米线。根据实验结果,分析了硅纳米材料的生长机理。调整水热溶液的酸碱度可实现可控制备硅纳米材料,这为下一步通过调整水热工艺参数宏量制备硅基纳米材料奠定了实验基础。
New kinds of materials with special characters are required in pressing because of addition of energy depletion and pollution of environment. The sizes of materials are needed to be smaller, because that the electronic devices are become samller and intelligent. And the characters of materials are neeed to be better, because that high speed developments of advance manufacture technology. One dimension nano materials have different structure, such as nanowires, nanorod, nanobelt, nanotube and so on. All of these kinds of materials have shown quite different character, such as quantum size effect, macroscopic quantum tunneling effect, coulomb blocked effect, small size effect, surface effect and so on. New kind research fields have been explored for scientist.
The silicon nanotubes (SiNTs) have been synthesized by hydrothermal method with pure water. The pH value of solution which is one of important parameters of hydrothermal have not been considered. So we study the affection of pH value to the structure and morphology of nano materials mainly. The viscosity, grain size and ζ potential of precursor in solution have been studied in different pH value condition. The dispersion was better when pH value was3-6than the others. In acid environment, the silicon nanowires (SiNWs) have been synthesized. The typical experimental condition is470℃in temperature,8MPa in pressure, and4hours in reaction time. The average diameter of SiNWs with amorphous outside is80nm. The special SiNWs which would be deformed under high power electron beam illumination were composed of disposed nano particles by TEM image. The space between the nano particles is amorphous SiO. The SiNWs growth mechanism have two stage. The fist is nucleation stage, in which the size of crystal nucleus have been influence by pH value of solution. The precursor would dissolve to form silicate aggregation. When the temperature rised, the silicate aggregation would hydrolyze to form crystal nucleus. The Si-O bond located on the crystal nucleus would be broken and transform to Si-H bond, which ensure the growth of SiNWs continually. The second stage is growth stage of SiNWs, which fellow the oxide-assisted growth mechanism. The silicon would separate out from nucleus with temperature rising., The crystal silicon would separate out in direction which the diffusibility of oxygen atom was lower. The SiNTs would synthesized in neutral solution, as the SiNWs would synthesize in acid solution. The key parameter is pH value of solution in the transformation, which play an important role in nucleation and growth stage of crystal silicon nano materials. The simulation method have been used to study the mechanism of silicon nano materials growth. The nanotubes without Si-H bond on surface tend to collapse. The Si-H bond play an important role in stability of silicon nano material.
In alkalescence solution, the production of experiment is silica nanospheres. The typical experiment parameter:pH is9, temperature is350℃, pressure is14MPa, soaking time is4hours. The nanosphere is smooth in surface, uniform in diameter and high purity. The diameter of nanosphere increase with the pH value of solution and temperature, and that decrease with the pressure. The photoluminescence spectrum of silica nanosphere shown that there are obviously peak located in411nm. The PL character of silica nanospheres still good when the sample place for long time. The Si-OH bond and Si-O-Si bond located on the surface of nanosphere synthesized by infra-red spectrum.
The silicate monomer would increase in the alkalescence form the result of experiment with high pH value. The silicate monomer would hydrolyze to form the nucleation central, at the same time the OH-ion enter the central to form the Si-OH bond. The Si-OH bond would link each other to form Si-O-Si bond, and then the silica nanospheres generated at last. The amount of defect exist on the nanosphere surface because that the OH-take up the location of O2-, which induce the amorphous structure of nanospheres.
The amorphous silica nanowires have been synthesize in neutral and alkalescence solution. The silica naowires locate on the top of reaction kettle. The diameter distribution rang are wide. The TEM image of sample shown that the nanowires are amorphous. The diameter of silica nanowires would increase with the pH value.
The Ni(OH)2nanosheets have been synthesized by hydrothermal. The typical experiment condition:pH value was7, temperature was470℃and the pressure is9MPa. The thickness of Ni(OH)2nanosheets is about30nm, the diameter is about150nm. The temperature was higher than200℃is necessary condition of growth Ni(OH)2nanosheet. The aggregation of Ni(OH)2nanosheets have trend to dissolve when the temperature rise. The size of crystalline grain of Ni(OH)2nanosheets show a trend of first increase and then decrease with the pH value.
In summary, the Si-H bond play an important role in growth proceeding. The pH value in solution is a crucial factor in synthesized silicon nano materials. The production is SiNWs in acid solution, and amorphous silica nanospheres in alkalescence solution. We discuss the growth mechanism of silicon nano materials in different experiment condition including temperature, pressure, reaction time and all. The Si-O bond on the surface of crystal nucleus were replaced by Si-H or Si-OH bond. The Si-H bond had advantage of stability of silicon crystal, which indicated that production is SiNWs in acid solution and amorphous nanospheres in alkalescence solution. The controllable silicon nano materials have been synthesized initially, which lay the foundation of silicon nano materials synthesis by hydrothermal method.
本课题组已采用水热法制备了硅纳米管,但在制备硅纳米管时,仅采用纯水作溶剂,采用水热法制备硅纳米材料时,溶液的酸碱度是硅纳米材料形成过程中重要的因素,为了解决这一问题并揭示纳米材料在水热环境中的生长机理,本论文着重研究了不同溶液pH值对于纳米材料生长的影响。我们展开了以下几个方面的研究,首先在不同酸碱度条件下,研究原料前驱物溶液的黏度、粒度以及ζ电位的变化规律。通过实验结果分析认为,当溶液的pH值为3-6时,原料的分散程度较好。接下来,在酸性条件下制备出了硅纳米线,典型的实验条件为pH=6、470℃、8MPa、保温4h,硅纳米线平均直径约为80nm,纳米线的外层有无定形氧化硅外层。值得注意的是,当pH=5时,得到一种在高能电子束照射下产生变形的硅纳米线,高分辨电镜观察发现这种纳米线是由分散的纳米颗粒组成,颗粒之间的空隙由无定形氧化物填充。通过分析酸性环境制备硅纳米线的实验结果,我们认为纳米线的生长过程存在两个阶段,一是成核阶段,在这一阶段成核大小受酸碱度的影响较大。二是纳米线生长阶段,在这一阶段遵循“氧化物辅助生长机制”。随着温度的升高,晶核内不断析出晶体硅,在某个特定方向上,氧扩散能力弱,使得在此方向上不断析出晶体硅,保证了晶核沿一维方向生长。水热法在中性条件下能生长出硅纳米管,而在酸性条件仅能生长出硅纳米线,产生这样结果的原因是溶液的酸碱度对硅纳米材料的成核和生长产生了影响。为了研究这-变化的规律,利用第一性原理计算模拟,从理论角度研究硅纳米管的稳定性。研究发现表面不存在Si-H键的硅纳米管易于塌陷,最终形成线状结构。而表面存在Si-H键的硅纳米管相对稳定。
调节水热溶液为碱性,结果显示,在碱性环境下能制备出氧化硅纳米球,典型的实验条件为pH=9、350℃、14MPa、保温4h。纳米球表面光滑,直径分布均匀,且纯度较高,随着pH值的升高,纳米球粒径呈现单调增长。在达到反应温度以后,氧化硅纳米球的粒径随着保温温度的升高而增大。氧化硅纳米球的粒径还会随着压力的增加而减小,这与硅纳米线直径与压力的关系一致,论文在4章中给出了pH值、温度、压力对粒径影响的详细机理分析。氧化硅纳米球具有良好的光致发光特性。样品的红外光谱显示,纳米球的表面存在Si-OH键以及Si-O-Si.通过碱性环境中的实验结果分析,在碱性环境中原料溶解后形成的硅酸根单体增加,同时碱性环境中存在的大量OH-离子进入成核中心形成Si-OH键,随着反应的进行硅酸根单体Si-OH之间形成Si-O-Si链,最终形成氧化硅纳米球。碱性环境中大量存在的OH-是无定形氧化硅颗粒生成的主要原因。
另外,在中性和碱性的实验中我们意外地收集到一种无定形氧化硅纳米线,这种纳米线在反应釜顶端能够收集到,直径分布很广,从数十纳米到数微米不等。TEM分析表明氧化硅纳米线是一种非晶结构。在酸性环境下,这种纳米线无法生成,当pH≥7时,随着pH值的升高纳米线的直径明显增加。初步认为这种无定形纳米线的生成是受到温度梯度的影响。论文第4章详细讨论了其中机理。
最后,尝试采用水热法制备其他纳米材料,使用Ni为原料,研究水热工艺条件对其生长的影响。实验得到的产物为氢氧化镍纳米片。典型实验条件为：pH=7,470℃,9MPa、保温时间4h。得到的氢氧化镍纳米片的厚度约为30nm,直径大约为150nm,纳米片聚集成球状。水热溶液酸碱度对产物的影响主要表现在酸性环境下无法形成氢氧化镍纳米片,当pH值大于7时,随着pH值的升高,纳米片的晶粒尺寸有先减小后增加。
综上所述,本文通过理论结合实验研究不同酸碱度条件下水热制备硅纳米材料的形成过程。着重从实验角度研究在不同酸碱度条件下硅纳米材料在水热环境中的形成过程。通过实验研究发现,在酸性环境下得到的为晶体硅纳米线,而在碱性环境下得到的产物为无定形氧化硅纳米球和氧化硅纳米线。根据实验结果,分析了硅纳米材料的生长机理。调整水热溶液的酸碱度可实现可控制备硅纳米材料,这为下一步通过调整水热工艺参数宏量制备硅基纳米材料奠定了实验基础。
New kinds of materials with special characters are required in pressing because of addition of energy depletion and pollution of environment. The sizes of materials are needed to be smaller, because that the electronic devices are become samller and intelligent. And the characters of materials are neeed to be better, because that high speed developments of advance manufacture technology. One dimension nano materials have different structure, such as nanowires, nanorod, nanobelt, nanotube and so on. All of these kinds of materials have shown quite different character, such as quantum size effect, macroscopic quantum tunneling effect, coulomb blocked effect, small size effect, surface effect and so on. New kind research fields have been explored for scientist.
The silicon nanotubes (SiNTs) have been synthesized by hydrothermal method with pure water. The pH value of solution which is one of important parameters of hydrothermal have not been considered. So we study the affection of pH value to the structure and morphology of nano materials mainly. The viscosity, grain size and ζ potential of precursor in solution have been studied in different pH value condition. The dispersion was better when pH value was3-6than the others. In acid environment, the silicon nanowires (SiNWs) have been synthesized. The typical experimental condition is470℃in temperature,8MPa in pressure, and4hours in reaction time. The average diameter of SiNWs with amorphous outside is80nm. The special SiNWs which would be deformed under high power electron beam illumination were composed of disposed nano particles by TEM image. The space between the nano particles is amorphous SiO. The SiNWs growth mechanism have two stage. The fist is nucleation stage, in which the size of crystal nucleus have been influence by pH value of solution. The precursor would dissolve to form silicate aggregation. When the temperature rised, the silicate aggregation would hydrolyze to form crystal nucleus. The Si-O bond located on the crystal nucleus would be broken and transform to Si-H bond, which ensure the growth of SiNWs continually. The second stage is growth stage of SiNWs, which fellow the oxide-assisted growth mechanism. The silicon would separate out from nucleus with temperature rising., The crystal silicon would separate out in direction which the diffusibility of oxygen atom was lower. The SiNTs would synthesized in neutral solution, as the SiNWs would synthesize in acid solution. The key parameter is pH value of solution in the transformation, which play an important role in nucleation and growth stage of crystal silicon nano materials. The simulation method have been used to study the mechanism of silicon nano materials growth. The nanotubes without Si-H bond on surface tend to collapse. The Si-H bond play an important role in stability of silicon nano material.
In alkalescence solution, the production of experiment is silica nanospheres. The typical experiment parameter:pH is9, temperature is350℃, pressure is14MPa, soaking time is4hours. The nanosphere is smooth in surface, uniform in diameter and high purity. The diameter of nanosphere increase with the pH value of solution and temperature, and that decrease with the pressure. The photoluminescence spectrum of silica nanosphere shown that there are obviously peak located in411nm. The PL character of silica nanospheres still good when the sample place for long time. The Si-OH bond and Si-O-Si bond located on the surface of nanosphere synthesized by infra-red spectrum.
The silicate monomer would increase in the alkalescence form the result of experiment with high pH value. The silicate monomer would hydrolyze to form the nucleation central, at the same time the OH-ion enter the central to form the Si-OH bond. The Si-OH bond would link each other to form Si-O-Si bond, and then the silica nanospheres generated at last. The amount of defect exist on the nanosphere surface because that the OH-take up the location of O2-, which induce the amorphous structure of nanospheres.
The amorphous silica nanowires have been synthesize in neutral and alkalescence solution. The silica naowires locate on the top of reaction kettle. The diameter distribution rang are wide. The TEM image of sample shown that the nanowires are amorphous. The diameter of silica nanowires would increase with the pH value.
The Ni(OH)2nanosheets have been synthesized by hydrothermal. The typical experiment condition:pH value was7, temperature was470℃and the pressure is9MPa. The thickness of Ni(OH)2nanosheets is about30nm, the diameter is about150nm. The temperature was higher than200℃is necessary condition of growth Ni(OH)2nanosheet. The aggregation of Ni(OH)2nanosheets have trend to dissolve when the temperature rise. The size of crystalline grain of Ni(OH)2nanosheets show a trend of first increase and then decrease with the pH value.
In summary, the Si-H bond play an important role in growth proceeding. The pH value in solution is a crucial factor in synthesized silicon nano materials. The production is SiNWs in acid solution, and amorphous silica nanospheres in alkalescence solution. We discuss the growth mechanism of silicon nano materials in different experiment condition including temperature, pressure, reaction time and all. The Si-O bond on the surface of crystal nucleus were replaced by Si-H or Si-OH bond. The Si-H bond had advantage of stability of silicon crystal, which indicated that production is SiNWs in acid solution and amorphous nanospheres in alkalescence solution. The controllable silicon nano materials have been synthesized initially, which lay the foundation of silicon nano materials synthesis by hydrothermal method.
引文
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