CN108149229A - 一种用于纳米薄膜沉积的液相基板火焰合成装置和方法 - Google Patents
一种用于纳米薄膜沉积的液相基板火焰合成装置和方法 Download PDFInfo
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Abstract
一种用于纳米薄膜沉积的液相基板火焰合成装置和方法,属于纳米及超细材料制备领域。该装置包括燃烧系统和液相基板沉积系统。该方法是通过火焰合成方法生长的纳米颗粒在液体表面进行沉积,液面的柔性使得颗粒沉积过程在二维方向进行,进而使得生长的单个颗粒可及时分散开来,降低了颗粒的团聚程度,形成单分散性较好,薄膜厚度可控,密度均匀的纳米薄膜,通过升降台将附着板升起,使得薄膜在表面张力作用下附着在多孔板上,将纳米膜置于烘箱烘干,即可得到致密薄膜。本发明不仅可以使得制备的纳米材料粒径分布更加均匀,还可以提高材料制备效率,适用于大规模生产各种氧化物薄膜,如二氧化钛、氧化铝以及氧化铜等薄膜材料。
Description
技术领域
本发明涉及一种用于纳米薄膜沉积的液相基板火焰合成装置和方法,属于超细材料制备技术领域。
背景技术
新材料的研究和创新将是未来科学研究的重要课题,其中纳米材料由于其特殊的物理和化学性能一直是科学研究的热点。纳米薄膜及纳米颗粒功能材料如纳米光学薄膜和纳米气敏薄膜超高比表面积和显著的量子特性,表现出常规材料所不具备的特殊性能,例如纳米厚度的信息存储薄膜具有超高密度功能,这类集成器件具有惊人的信息处理能力。
纳米薄膜的制备方法由粒子束溅射沉积、化学气相沉积(CVD)和电化学沉积等,但目前的薄膜沉积技术受技术本身限制很难合成20nm以下的纳米颗粒,进而使得薄膜的量子特性无法进一步体现;而火焰合成技术能够合成20nm以下的超细颗粒,且工艺简单易于工业放大等优点;目前火焰合成技术均使用固相基板,江苏大学CN103708439A利用传送固相基板沉积碳纳米管;清华大学CN103464064A使用弱旋流滞止火焰合成装置采用固体滞止板沉积纳米颗粒。纳米颗粒在沉积到基板时由于颗粒不能及时分散开发生团聚并形成的薄膜孔隙率较高,使得该方法制备的薄膜分布不均进而限制其使用性能,且随制备速率的增加团聚现象越发明显。
发明内容
本发明的目的是提供一种用于纳米薄膜沉积的液相基板火焰合成装置和方法,使其不仅可以提高薄膜制备效率,而且还可以避免颗粒团聚制备粒径分布更加均匀的薄膜。
本发明的技术方案如下:
一种用于纳米薄膜沉积的液相基板火焰合成装置,该装置包括燃烧系统和液相基板沉积装置;燃烧系统包括依次连接的燃烧供气瓶、超声雾化装置和燃烧器喷嘴;所述的液相基板沉积系统包括沉积液、薄膜附着系统和液面恒定连通器;薄膜附着系统包括薄膜附着板、精密升降台、支撑杆;薄膜附着板通过支撑杆设置在精密升降台上;液面恒定连通器包括通过连通器连通的液相沉积槽(10)与液面恒定槽,其中,薄膜附着板通过精密升降台在液相沉积槽内垂直方向上移动。
优选的,沉积液为水溶液。
优选的,液面恒定槽设有循环冷却液入口与循环冷却液出口,用于调整液面恒定槽液面恒定及液体温度。
优选的,液相基板沉积系统距离燃烧器喷嘴的距离在1-5cm范围内可调。
优选的,薄膜附着板材质为玻璃、二氧化硅、铝、铜或不锈钢。
优选的,薄膜附着板尺寸为6-20倍的燃烧器喷嘴直径,薄膜附着板的上气孔直径为1-3μm。
一种用于纳米薄膜沉积的液相基板火焰合成方法,方法包括如下步骤:
(1)燃烧系统生成燃料预混气在燃烧器喷嘴下方发生燃烧反应,形成稳定于液相基板上方的滞止火焰面,反应温度为1000-1650℃;
(2)前驱液经过燃烧系统的超声雾化装置雾化经载气形成气溶胶送入火焰场,经过火焰场成核、生长成纳米颗粒,纳米颗粒在热泳作用下沉积到沉积液表面,使颗粒单分散;
(3)使用精密升降台将薄膜附着板抬起,纳米薄膜在表面张力的作用下附着在薄膜附着板上,取出后50-80℃真空条件下烘干10-20min制得纳米薄膜。
优选的,沉积液的温度控制在60-100℃。
优选的,燃烧系统生成燃料预混气气流速度为0.5-5.0m/s,当量比为0.5-2.5。
优选的,超声雾化装置超声频率在1.7-2.4MHZ。
本发明相对于现有技术具有显著优点如下:
1、本发明通过平面滞止火焰与液相基板相结合制备的组成纳米薄膜的纳米颗粒粒径分布极窄;
2、合成的纳米薄膜孔隙率极小的均匀薄膜。
附图说明
图1为本发明提供的用于纳米薄膜沉积的液相基板火焰合成装置的结构示意图;
图2为液相基板系统结构示意图;
图3为连接杆与沉积槽连接处剖面图;
1、氧气瓶;2、氮气瓶;3、超声雾化装置;4、称量装置;5、液相基板系统;6、燃烧器喷嘴;7、燃料气瓶;8、沉积液;9、薄膜附着板;10、液相沉积槽;11、支撑杆;12、精密升降台;13、连通器;14、液面恒定槽;15、循环冷却液出口;16、循环冷却液入口。
图4为本发明制备的二氧化钛薄膜TEM形貌图;
图5为本发明制备的氧化铝薄膜TEM形貌图;
图6为本发明制备的氧化铜薄膜TEM形貌图。
具体实施方式
下面结合附图对本发明的装置结构、工艺方法和具体实施方式做进一步说明。雾化装置以及供气瓶;图2为本发明提供的一种液相基板沉积系统,包括
图1为本发明提供的一种用于纳米薄膜沉积的液相基板火焰合成装置,包括燃烧系统和薄膜沉积装置,该装置含有燃烧系统和液相基板沉积装置;燃烧系统包括依次连接的燃烧供气瓶、超声雾化装置3和燃烧器喷嘴6。
图2为液相基板沉积系统,所述的液相基板沉积系统包括沉积液8、薄膜附着系统和液面恒定连通器13;薄膜附着系统包括薄膜附着板9、精密升降台12、支撑杆11;薄膜附着板通过支撑杆设置在精密升降台上;液面恒定连通器包括通过连通器连通的沉积槽10与液面恒定槽14,其中,薄膜附着板通过精密升降台在液相沉积槽内垂直方向上移动。
本发明的工艺过程如下:
燃料预混气燃烧产生的平面火焰稳定在沉积液8上方3-4mm的位置,经超声雾化器3雾化后的前驱液经氮气载气经过火焰面颗粒成核、生长,在热泳作用下沉积到液面上方,液面柔性使得所合成的纳米颗粒在气流横向速度和热泳横向速度的作用下迅速分散,随着颗粒的沉积形成薄膜,薄膜厚度通过气流速度和燃料当量比控制。将薄膜附着板9升起,使得薄膜在表面张力作用下附着在薄膜附着板上,经真空烘干处理后即可得到质地均匀的纳米薄膜。
本发明的液相基板火焰合成装置可合成:氧化铝、二氧化钛,氧化钇,氧化铋,氧化铜,氧化铁,碲化铋,碲化锑,硒化铋,硒化锑等。
实施例1:合成二氧化钛纳米薄膜
将四异丙醇钛加入到超声雾化器3经过超声产生前驱液气雾,气雾经过氮气载气形成气溶胶;乙烯、前驱体气溶胶和氮气氧气混合气体,当量比0.45,送入燃烧器喷嘴6,经燃烧反应形成稳定在沉积液8上方3mm位置的火焰面,火焰温度控制在1600℃。
前驱液在火焰中发生分解、成核和生长形成纳米颗粒,颗粒在热泳作用下沉积到沉积液8上,颗粒迅速分散,避免颗粒的团聚,随着颗粒的不断沉积形成单分散性较好,分布均匀的纳米薄膜,此后将薄膜附着板9升起,使得薄膜在表面张力作用下附着在薄膜附着板上,经50℃真空环境干燥10min即可得到致密薄膜。
实施例2:合成氧化铝纳米薄膜
将浓度为4.2%的氯化铝溶液加入到超声雾化器3经过超声产生前驱液气雾,气雾经过氮气载气形成气溶胶;乙烯、前驱体气溶胶和氮气氧气混合气体,当量比0.45,送入燃烧器,经燃烧反应形成稳定在沉积液8上方3mm位置的火焰面,火焰温度控制在1600℃。
前驱液在火焰中发生分解、成核和生长形成纳米颗粒,颗粒在热泳作用下沉积到沉积液上,颗粒迅速分散,避免颗粒的团聚,随着颗粒的不断沉积形成单分散性较好,分布均匀的纳米薄膜,此后将薄膜附着板升起,使得薄膜在表面张力作用下附着在薄膜附着板上,经50℃真空环境干燥10min即可得到致密薄膜。。
实施例3:合成氧化铜纳米薄膜
将浓度为3.8%的氯化铜溶液加入到超声雾化器3经过超声产生前驱液气雾,气雾经过氮气载气形成气溶胶;乙烯、前驱体气溶胶和氮气氧气混合气体,当量比0.45,送入燃烧器喷嘴6,经燃烧反应形成稳定在沉积液8上方3mm位置的火焰面,火焰温度控制在1600℃。
前驱液在火焰中发生分解、成核和生长形成纳米颗粒,颗粒在热泳作用下沉积到液面上,颗粒迅速分散,避免颗粒的团聚,随着颗粒的不断沉积形成单分散性较好,分布均匀的纳米薄膜,此后将薄膜附着板9升起,使得薄膜在表面张力作用下附着在薄膜附着板上,经50℃真空环境干燥10min即可得到致密薄膜。
Claims (10)
1.一种用于纳米薄膜沉积的液相基板火焰合成装置,其特征在于,该装置包括燃烧系统和液相基板沉积装置;燃烧系统包括依次连接的燃烧供气瓶、超声雾化装置(3)和燃烧器喷嘴(6);所述的液相基板沉积系统包括沉积液(8)、薄膜附着系统和液面恒定连通器(13);薄膜附着系统包括薄膜附着板(9)、精密升降台(12)、支撑杆(11);薄膜附着板(9)通过支撑杆(11)设置在精密升降台(12)上;液面恒定连通器包括通过连通器(13)连通的液相沉积槽(10)与液面恒定槽(14),其中,薄膜附着板(9)通过精密升降台(12)在液相沉积槽(10)内垂直方向上移动。
2.根据权利要求1所述的用于纳米薄膜沉积的液相基板火焰合成装置,其特征在于,所述的沉积液(8)为水溶液。
3.根据权利要求1所述的用于纳米薄膜沉积的液相基板火焰合成装置,其特征在于:液面恒定槽(14)设有循环冷却液入口(16)与循环冷却液出口(15),用于调整液面恒定槽(14)液面恒定及液体温度。
4.根据权利要求1所述的用于纳米薄膜沉积的液相基板火焰合成装置,其特征在于,所述的液相基板沉积系统距离燃烧器喷嘴(6)的距离在1-5cm范围内可调。
5.根据权利要求1所述的用于纳米薄膜沉积的液相基板火焰合成装置,其特征在于,薄膜附着板(9)材质为玻璃、二氧化硅、铝、铜或不锈钢。
6.根据权利要求1或5所述的用于纳米薄膜沉积的液相基板火焰合成装置,所述的薄膜附着板(9)尺寸为6-20倍的燃烧器喷嘴(6)直径,薄膜附着板(9)的上气孔直径为1-3μm。
7.一种用于纳米薄膜沉积的液相基板火焰合成方法,其特征在于,所述的方法包括如下步骤:
(1)燃烧系统生成燃料预混气在燃烧器喷嘴(6)下方发生燃烧反应,形成稳定于液相基板(5)上方的滞止火焰面,反应温度为1000-1650℃;
(2)前驱液经过燃烧系统的超声雾化装置(3)雾化经载气形成气溶胶送入火焰场,经过火焰场成核、生长成纳米颗粒,纳米颗粒在热泳作用下沉积到沉积液表面,使颗粒单分散;
(3)使用精密升降台(12)将薄膜附着板(9)抬起,纳米薄膜在表面张力的作用下附着在薄膜附着板(9)上,取出后50-80℃真空条件下烘干10-20min制得纳米薄膜。
8.根据权利要求7所述的用于纳米薄膜沉积的液相基板火焰合成方法,其特征在于,沉积液(8)的温度控制在60-100℃。
9.根据权利要求7所述的用于纳米薄膜沉积的液相基板火焰合成方法,其特征在于,燃烧系统生成燃料预混气气流速度为0.5-5.0m/s,当量比为0.5-2.5。
10.根据权利要求7所述的用于纳米薄膜沉积的液相基板火焰合成方法,其特征在于,超声雾化装置(3)超声频率在1.7-2.4MHZ。
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