纳米氧化锌制备及胺酯类聚合物合成、掺杂性质研究
摘要
本研究运用回流反应装置制备得到ZnCO_3前驱体,在683K灼烧得到白色ZnO颗粒。通过对回流反应时间、分散剂种类与产品粒度之间关系的实验确定了最佳的反应时间为10h,样品粒径小,粒度较均匀。比较了不同种类分散剂的分散效果,较好的分散剂种类为非离子型分散剂-甘油。经激光粒度仪、扫描电镜等方法测定,其粒径为25nm左右。
用醇类与胺类物质合成得到了具有较强粘性的胺酯类聚合物。通过研究氧化剂加入量、固化时间与产品粘度之间的关系,得到了最佳氧化剂加入量及固化时间。最好的氧化剂为浓度0.6g/L的NH_4HSO_4溶液,固化时间3h。固化后此种聚合物粘度最高可达到2703mpa.s。
用共混法将纳米ZnO掺杂粒子掺杂入此胺酯类聚合物中,运用电化学工作站对其导电特性进行研究表明,其电导率最高可达到4.35×10~(-3)S/m,氧化锌掺杂比为12%。小于12wt%时,随掺入量增加电导率增加,掺入量大于12wt%时,掺入量增加电导率反而下降。为提高导电聚合物的电导率,将锡族化合物-SnCl_2、SnO_2为ZnO的掺杂微粒,对其进行改性,通过实验确定这两种聚合物的电导率分别为:2.16×10~(-2)S/m,6.25×10~(-2)S/m。针对ZnO的半导体特性,本研究对掺杂聚合物的光电转换特性进行了初步研究,研究结果表明三种掺杂聚合物在相同入射光强条件下的最大光生电流分别为8.9mA、13.6mA、20.7mA, ZnO/SnO_2掺杂聚合物光电转化性能较优。
In the paper, nano ZnO with about 25nm diameter has been prepared by the circumfluence reaction. The experiments were carried out in order to determine the optimum conditions such as reaction time and the type of dispersant. The results show that the best reaction time is 10h and the type of non-ionic dispersant is better. The UV adsorption behavior of the nano ZnO has also been studied.The alcohol and amine were used to synthesize a polymer with high glutinosity. The concentration of oxidant, time of solidification and the glutinosity of the viscoid have been determined as 0.6g/L, 3h and 2703mpa.s, respectively.The polymer was doped with nano ZnO by the means of co-mix treatment. The experiments of electrochemistry reveal that the conductivity of the polymer doped by ZnO is 435×10~-3S/m and the doped ratio, 12wt%. When the ratio is lower than it, the conductivity increases with the doped contents, while higher than 12wt%, in reverse, there occurs decrease. In order to improve the conductivity, SnCl_2 and SnO_2 were chosen to mix with nano ZnO, and the mixtures were doped into the polymer to form two types of co-doped ones. Their conductivity are 2.16×10~-2S/m, 6.25×10~-5S/m, respectively. A set of experiments of photoelectric effects for the doped polymers has been carried out. The results show the highest currents caused by light are 8.9mA, 13.6mA and 20.7mA, respectively, for three kinds of the different doped polymers that are with nano-ZnO individual, mixed with SnCl_2 as well as with SnO_2. The doped with ZnO mixed with SnO_2 among them is the best.
用醇类与胺类物质合成得到了具有较强粘性的胺酯类聚合物。通过研究氧化剂加入量、固化时间与产品粘度之间的关系,得到了最佳氧化剂加入量及固化时间。最好的氧化剂为浓度0.6g/L的NH_4HSO_4溶液,固化时间3h。固化后此种聚合物粘度最高可达到2703mpa.s。
用共混法将纳米ZnO掺杂粒子掺杂入此胺酯类聚合物中,运用电化学工作站对其导电特性进行研究表明,其电导率最高可达到4.35×10~(-3)S/m,氧化锌掺杂比为12%。小于12wt%时,随掺入量增加电导率增加,掺入量大于12wt%时,掺入量增加电导率反而下降。为提高导电聚合物的电导率,将锡族化合物-SnCl_2、SnO_2为ZnO的掺杂微粒,对其进行改性,通过实验确定这两种聚合物的电导率分别为:2.16×10~(-2)S/m,6.25×10~(-2)S/m。针对ZnO的半导体特性,本研究对掺杂聚合物的光电转换特性进行了初步研究,研究结果表明三种掺杂聚合物在相同入射光强条件下的最大光生电流分别为8.9mA、13.6mA、20.7mA, ZnO/SnO_2掺杂聚合物光电转化性能较优。
In the paper, nano ZnO with about 25nm diameter has been prepared by the circumfluence reaction. The experiments were carried out in order to determine the optimum conditions such as reaction time and the type of dispersant. The results show that the best reaction time is 10h and the type of non-ionic dispersant is better. The UV adsorption behavior of the nano ZnO has also been studied.The alcohol and amine were used to synthesize a polymer with high glutinosity. The concentration of oxidant, time of solidification and the glutinosity of the viscoid have been determined as 0.6g/L, 3h and 2703mpa.s, respectively.The polymer was doped with nano ZnO by the means of co-mix treatment. The experiments of electrochemistry reveal that the conductivity of the polymer doped by ZnO is 435×10~-3S/m and the doped ratio, 12wt%. When the ratio is lower than it, the conductivity increases with the doped contents, while higher than 12wt%, in reverse, there occurs decrease. In order to improve the conductivity, SnCl_2 and SnO_2 were chosen to mix with nano ZnO, and the mixtures were doped into the polymer to form two types of co-doped ones. Their conductivity are 2.16×10~-2S/m, 6.25×10~-5S/m, respectively. A set of experiments of photoelectric effects for the doped polymers has been carried out. The results show the highest currents caused by light are 8.9mA, 13.6mA and 20.7mA, respectively, for three kinds of the different doped polymers that are with nano-ZnO individual, mixed with SnCl_2 as well as with SnO_2. The doped with ZnO mixed with SnO_2 among them is the best.
引文
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