La-Yb共掺杂二氧化锡纳米粉体的制备、表征与性能研究

发布时间：2018-01-28 13:39

  本文关键词： 纳米材料 化学共沉淀法 La-Yb共掺杂 LaxYbySn(1-x-y)O2 掺杂二氧化锡 隔热涂层　出处：《深圳大学》2015年硕士论文　论文类型：学位论文

【摘要】：现代建筑广泛采用大面积玻璃窗及豪华气派的玻璃幕墙,采暖和制冷造成很大的能源消耗,同时也带来了“光污染”,影响了人们的生活。近年来,越来越多的人开始重视“绿色环保,节能减排”。目前主要通过镀膜和贴膜来达到建筑玻璃门窗、车窗隔热和节能减排的目的,但是效果不太理想,且成本较高,使用寿命短。一种以掺杂二氧化锡为代表的新型的无机-有机复合的多组分材料慢慢被广泛应用于隔热玻璃涂料。本文的研究内容主要是:通过掺杂元素镧和镱来改变二氧化锡在不同波长区域的光学性能,希望能获得既能满足可见光透过率,同时具有良好阻隔近红外线的隔热涂料。以La Cl3·7H2O、Yb(NO3)3·6H2O、Sn Cl4·5H2O为原料,氨水为沉淀剂,PEG-600作分散剂,采用化学共沉淀法制备了镧镱共掺杂二氧化锡纳米粉体。考察了反应温度、反应时间、反应p H值、煅烧温度、煅烧时间、镧和镱的掺杂量等因素的影响,运用差热-热重分析(TG-DTA),X射线衍射仪(XRD)、扫描电镜(SEM)等仪器对粉体的结构、形貌及纳米化程度等进行表征。优化得到共沉淀法制备镧镱共掺杂二氧化锡纳米粉体的最佳工艺条件如下:反应温度为60℃,反应时间为3h,PEG-600为分散剂,滴定终点p H值为9,镧的掺杂量x=0.05,镱的掺杂量y=0.1,煅烧温度为800℃,煅烧保温时间为3h。分析测试结果表明,镧和镱的掺杂没有改变二氧化锡的物相,仍为四方相金红石结构,粉体呈球形,颗粒大小和分布都较均匀,平均粒径在40nm左右,分散性良好,只有轻微团聚现象。通过机械研磨-超声分散法制备La0.05Yb0.1Sn0.85O2浆料,通过沉降实验讨论了分散介质、硅烷偶联剂的种类、分散剂的种类及含量等因素对浆料稳定性的影响。实验结果表明:当超声分散时间为20min,用去离子水为分散介质,KH560为硅烷偶联剂、3%的CTAB为分散剂,p H为6时,所制备的La0.05Yb0.1Sn0.85O2浆料的分散稳定性最好,沉降速率最慢,一周时间内浆料只沉降了4%左右;超声波处理对浆料的分散性影响很大,SEM、TEM测试结果表明,浆料中纳米颗粒分散均匀,粒径大小均匀,粒径在20nm左右,只有较少团聚现象。最后,用水性丙烯酸树脂和La0.05Yb0.1Sn0.85O2浆料通过共混法制得隔热涂料,然后涂覆在载玻片基底上制得隔热涂层,并对涂层进行了紫外-可见-近红外光谱及物理性能的测试表征,讨论了镧和镱的掺杂量、不同浆料用量及涂层厚度等对紫外可见近红外光透过率的影响。实验结果表明:当镧的掺杂量x=0.05、镱的掺杂量y=0.1,浆料用量为35%,涂层厚度为3层时,涂层的隔热性能最佳,红外阻隔率达到80%-90%,且对可见过的透过率在80%以上,达到了建筑涂膜隔热玻璃标准(GB/T 29501-2013);涂层的硬度为3H,附着力为1级,耐水性良好(浸泡24h无起泡)。
[Abstract]:Large area glass windows and luxurious glass curtain wall are widely used in modern buildings. Heating and cooling cause a great deal of energy consumption, but also bring "light pollution", which has affected people's lives in recent years. More and more people begin to pay attention to "green environmental protection, energy conservation and emission reduction". At present, mainly through coating and film to achieve the purpose of building glass doors and windows, car windows insulation and energy conservation, but the effect is not very good. And the cost is high. A new type of inorganic-organic composite multicomponent material, represented by doped tin dioxide, has been widely used in insulating glass coatings. The main contents of this paper are as follows:. By doping lanthanum and ytterbium, the optical properties of tin dioxide in different wavelength regions were changed. It is hoped that the thermal insulation coating can satisfy the visible light transmittance and have a good barrier to near infrared ray. La Cl3 路7H _ 2O _ 3 路6H _ 2O is used in this paper. Sn Cl4 路5H 2O was used as raw material and ammonia water as precipitator PEG-600 as dispersant. Lanthanum and ytterbium co-doped tin dioxide nano-powders were prepared by chemical co-precipitation method. The reaction temperature was investigated. The factors such as reaction time, pH value, calcination temperature, calcination time, doping amount of lanthanum and ytterbium were studied by differential thermogravimetric analysis (TG-DTAC) X-ray diffractometer (XRD). Scanning electron microscopy (SEM) and other instruments on the structure of the powder. The optimum conditions for preparing lanthanum ytterbium co-doped tin dioxide nanoparticles by co-precipitation were obtained as follows: reaction temperature 60 鈩，

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