【摘要】：二氧化鈦粒子,是一種非常重要的功能材料。因其具有較高的折射率和優(yōu)異的光學(xué)特性,有望以二氧化鈦膠體微球?yàn)榻M裝原料,制備近紅外和可見光波段的高質(zhì)量光子晶體。單分散二氧化鈦微球的合成是制備膠體光子晶體的基礎(chǔ)。本論文在溶膠-凝膠法的基礎(chǔ)上,以鈦酸四丁酯為原料,合成了單分散亞微米和窄分散納米二氧化鈦粒子,并通過離心自組裝法制備了高質(zhì)量的光子晶體,具體內(nèi)容如下:在乙醇體系中加入KCl水溶液,其中KCl作為穩(wěn)定劑,成功合成出粒徑范圍為100~465nm的單分散亞微米二氧化鈦微球,并制備了多分散指數(shù)在0.05~0.25之間的窄分散納米級二氧化鈦粒子,研究了不同反應(yīng)時(shí)間(0~8h)、KCl濃度(4.06×10~(-4)~1.74×10~(-3)mol/L)、水鈦摩爾比(4.05~9.45)、反應(yīng)溫度(15~40℃)等因素對二氧化鈦微球的粒徑尺寸及粒徑分布的影響規(guī)律。結(jié)果表明:KCl的加入能夠有效抑制粒子聚沉現(xiàn)象的發(fā)生;采用適當(dāng)?shù)姆磻?yīng)條件可以得到不同粒徑的二氧化鈦粒子。以丙酮-乙醇或二甲基亞砜(DMSO)-乙醇混合溶劑為反應(yīng)介質(zhì),KCl作為穩(wěn)定劑,合成了粒徑范圍為100~480nm的單分散二氧化鈦規(guī)則微球。實(shí)驗(yàn)發(fā)現(xiàn):隨著KCl濃度(4.06×10~(-4)~1.45×10~(-3)mol/L)的增大,微球的粒徑依次減小,單分散性保持良好;丙酮或DMSO的含量增加,導(dǎo)致微球的粒徑變大,單分散性變差,DMSO的影響程度尤為明顯�；旌先軇┓閱畏稚單⒚锥趸佉�(guī)則微球的制備提供了一種思路。采用兩步法,先在常溫下生成沉淀,然后80℃回流膠溶,通過調(diào)控鈦酸四丁酯的用量和回流體系中pH值的大小,成功實(shí)現(xiàn)水溶性良好的納米二氧化鈦粒子的合成,確定了最小尺寸納米粒子的合成條件:回流體系中pH值為1.5,鈦酸四丁酯濃度為0.5mol/L。分別以預(yù)先合成的145nm,179nm,200nm和230nm單分散二氧化鈦微球?yàn)樽越M裝原料,利用離心法在2500rpm,3500rpm和4500rpm轉(zhuǎn)速下制備出大面積的三維膠體光子晶體,使用掃描電子顯微鏡和紫外-可見分光光度計(jì)表征,結(jié)果表明:離心法工藝操作簡單,制備周期短;制備的膠體光子晶體具有明顯的光子帶隙,隨著顆粒增大,禁帶位置紅移;離心轉(zhuǎn)速會影響膠體光子晶體的質(zhì)量,根據(jù)微球的大小選擇合適的轉(zhuǎn)速至關(guān)重要。這為光子晶體在光學(xué)器件中的應(yīng)用提供了實(shí)驗(yàn)依據(jù)和有效指導(dǎo)。
[Abstract]:Titanium dioxide particles are very important functional materials. Due to its high refractive index and excellent optical properties, it is expected to prepare high quality photonic crystals with near infrared and visible light bands using titanium dioxide colloidal microspheres as the assembly material. The synthesis of monodisperse titanium dioxide microspheres is the basis for the preparation of colloidal photonic crystals. Based on the sol-gel method, monodisperse submicron and narrow dispersed nano-TiO _ 2 particles were synthesized from tetrabutyl titanate, and high quality photonic crystals were prepared by centrifugal self-assembly method. The main contents are as follows: the monodisperse submicron TIO _ 2 microspheres with the particle size range of 100~465nm were successfully synthesized by adding KCl aqueous solution and KCl as stabilizer in ethanol system. Narrow dispersed nanometer TIO _ 2 particles with polydispersity index of 0.05 ~ 0.25 were prepared. The effects of different reaction time (0 ~ 8 h), KCl concentration (4.06 脳 10 ~ (-4) ~ 1.74 脳 10 ~ (-3) mol/L), molar ratio of water to titanium (4.05 ~ 9.45) and reaction temperature (1540 鈩，

本文編號：2286617