CN113235066A - 有机铂族金属化学气相沉积装置和方法 - Google Patents
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Abstract
有机铂族金属化学气相沉积装置和方法。该装置包括控温室以及位于控温室上方的真空沉积室。控温室中设置有:有机铂族金属升华器;载气盘管,设置有载气控制阀并与升华器的底部连通;以及反应气盘管,设置有反应气控制阀。主管道从升华器顶部延伸至真空沉积室底部以将二者相互连通,并设置有位于控温室中的主管道控制阀。反应气盘管与主管道控制阀上部的主管道部分连通。真空沉积室中设置有电加热体,电加热体的加热底面适于设置待沉积基底。根据本发明的CVD装置,在真空沉积室中利用电加热体对待沉积基底进行局部直接加热(冷壁沉积),并使得混合气体近距离直对待沉积基底,使得沉积精准高效。另外,在控温室中加热升华器时,还利用盘管对载气和反应气进行了同步加热,防止物料在管路中凝结堵塞,从而进一步提高了沉积效率。
Description
技术领域
本发明涉及化学气相沉积(CVD)技术,尤其涉及金属有机化学气相沉积(MOCVD)技术。
背景技术
与溅射和热蒸发等其他沉积技术相比,金属有机化学气相沉积具有操作温度低、工艺简单、价格低廉的优点,并允许通过适当选择有机金属前体和反应气体来控制薄膜性能。它一般包括三个步骤:(1)产生挥发性物质;(2)将挥发性物质输运到沉积区;(3)于基体上发生化学反应而生成固态产物。
铂族金属有机化合物气相沉积时使用的铂络合物通常需要采用氢作为还原剂,以避免不希望的产物进入涂层结构,而且对空气非常敏感,并且在某些情况下还存在毒性危险。另外,在化学气相沉积过程中需要精确控制温度,例如过高时会导致原料气在管壁沉积分解,造成贵金属原料损失。
发明内容
本发明的目的是提供一种改进的有机铂族金属化学气相沉积技术。
根据本发明的第一方面,提供了一种有机铂族金属CVD装置,包括控温室以及位于控温室上方的真空沉积室,其中控温室中设置有:
有机铂族金属升华器;
载气盘管,设置有载气控制阀并与升华器的底部连通;以及
反应气盘管,设置有反应气控制阀,
其中主管道从升华器顶部延伸至真空沉积室底部以将二者相互连通,并设置有位于控温室中的主管道控制阀,
反应气盘管与主管道控制阀上部的主管道部分连通,
真空沉积室中设置有电加热体,电加热体的加热底面适于设置待沉积基底。
根据本发明的CVD装置的优选实施例,真空沉积室位于控温室顶部,主管道在真空沉积室中的开口朝向电加热体的加热底面。主管道在真空沉积室中的开口与电加热体的加热底面上设置的待沉积基底优选间距1-3cm。
根据本发明的CVD装置的具体实施例,还可以包括位于真空沉积室外部用于对其进行抽真空的真空泵。
根据本发明的CVD装置的优选实施例,升华器还设置有气压计。
根据本发明的CVD装置,在真空沉积室中利用电加热体对待沉积基底进行局部直接加热(冷壁沉积),并使得混合气体近距离直对待沉积基底,使得沉积精准高效。另外,在控温室中加热升华器时,还利用盘管对载气和反应气进行了同步加热,防止物料在管路中凝结堵塞,从而进一步提高了沉积效率。
根据本发明的另一方面,还提供了一种有机铂族金属化学气相沉积方法,包括:
在控温室中分别提供升华器、载气盘管和反应气盘管;
提供位于控温室顶部上的真空沉积室;
在真空沉积室中提供电加热体;
提供从升华器顶部延伸至真空沉积室底部以将二者直接连通的主管道,并在主管道上提供主管道控制阀;
其中载气盘管设置有载气控制阀并与升华器的底部连通,反应气盘管设置有反应气控制阀并与主管道控制阀上部的主管道部分连通,主管道在真空沉积室中的开口朝向电加热体的加热底面,
在电加热体的加热底面设置待沉积基底;
在升华器中提供有机铂族金属;
提供用于对真空沉积室进行抽真空的真空泵;
关闭载气控制阀和反应气控制阀,打开主管道控制阀,打开真空泵进行抽真空操作;
关闭主管道控制阀;
将控温室加热至预定温度,以将有机铂族金属进行升华并分别预热载气盘管中的载气和反应气盘管中的反应气;
开启电加热体将待沉积基底加热至设定温度;
打开反应气控制阀,以将反应气通过主管道送入真空沉积室;
再分别打开载气控制阀和主管道控制阀,以通过载气将升华器中的有机铂族金属升华气体送入真空沉积室;
整个过程中保持真空泵开启直至真空沉积完成。
根据本发明的方法的优选实施方式,有机铂族金属为乙酰丙酮铂,载气为氮气,反应气为氧气。真空沉积过程中载气流量优选为50-300ml/min,反应气流量优选为20-150ml/min。
根据本发明的方法的优选实施方式,控温室加热至165℃~185℃的升华温度,待沉积基底加热至455℃~485℃。
根据本发明的方法的优选实施方式,真空沉积时间为5-30分钟。
根据本发明的金属化学气相沉积方法,由于采用了乙酰丙酮铂作为有机铂族金属,从而具有在空气中稳定性好、易升华、分解温度低、溶于有机溶剂等优点,并且沉积效果好,能有效提高铂族金属纯度及电学特性。另外,升华器与真空沉积室的同步真空预处理便捷地消除了金属对空气的敏感性。另外,真空泵在沉积过程中还同时起到了排出废气的作用。此外,控温室的整体加热方式还显著提高了沉积效率。
附图说明
图1为根据本发明的CVD装置的结构示意图;以及
图2和图4分别示出了根据本发明不同实施例的沉积薄膜的XRD图;以及
图3和图5分别示出了根据本发明不同实施例的沉积薄膜的SEM图。
具体实施方式
下面结合实施例和附图对本发明做进一步说明,本领域技术人员应该理解,实施例和附图只是为了更好地理解本发明,并不用于任何限制目的。
如图1所示,本发明的CVD装置总体包括控温室1以及位于控温室1顶部的真空沉积室9。真空沉积室9连接有真空泵10。
控温室1中设置有反应气盘管2、载气盘管3和升华器4。载气盘管3设置有载气控制阀①并与升华器4的底部连通。载气盘管3还配备有流量计M。主管道7从升华器4顶部延伸至真空沉积室9底部以将二者相互连通,并设置有位于控温室1中的主管道控制阀②。反应气盘管2设置有反应气控制阀③,并与主管道控制阀②上部或上游的主管道部分连通。反应气盘管2也配备有流量计M。升华器4还配备有泄压安全阀5和气压计6。
真空沉积室9中设置有圆柱体形状的电加热体8,电加热体8具有适于设置待沉积基底的加热底面。主管道7在真空沉积室9中的开口朝向电加热体8的加热底面,与电加热体的加热底面上设置的待沉积基底间距2cm。电加热体8与温控装置11相连。
下面简要描述根据本发明的CVD工艺。
首先,在电加热体8的加热底面设置待沉积基底;然后在升华器4中提供有机铂族金属;接下来关闭载气控制阀①和反应气控制阀③,打开主管道控制阀②,并打开真空泵进行抽真空操作;随后关闭主管道控制阀②;将控温室1加热至预定温度,以将有机铂族金属进行升华并分别预热载气盘管3中的载气和反应气盘管2中的反应气;通过温控装置11开启电加热体8将待沉积基底加热至设定温度;打开反应气控制阀③,以将反应气通过主管道7送入真空沉积室9;在升华器4的气压计6的读数达到预定值后,再分别打开载气控制阀①和主管道控制阀②,以通过载气将升华器4中的有机铂族金属升华气体送入真空沉积室9。整个过程中保持真空泵10开启直至真空沉积完成。
实施例1
用#400砂纸将钛箔表面氧化层打磨之后再用#1600砂纸将表面打磨光滑,然后置于乙醇当中超声处理15min去除表面灰尘及油污,后用蒸馏水洗涤烘干,与电加热体的加热底面贴紧。在升华器4中加入乙酰丙酮铂35.09mg,控温室1中的预定温度或升华温度为170℃,电加热体8的加热底面设定温度或沉积温度控制为460℃,氮气流量150ml/min,氧气流量50ml/min,沉积时间10min。所得薄膜产品XRD如图2所示,SEM如图3所示。
实施例2
用#400砂纸将钛箔表面氧化层打磨之后再用#1600砂纸将表面打磨光滑,然后置于乙醇当中超声处理15min去除表面灰尘及油污,后用蒸馏水洗涤烘干,与电加热体的加热底面贴紧。在升华器4中加入乙酰丙酮铂30.78mg,升华温度为180℃,沉积温度为480℃,氮气流量180ml/min,氧气流量30ml/min,沉积时间20min。所得产品XRD如图4所示,SEM如图5所示。
Claims (10)
1.一种有机铂族金属CVD装置,包括控温室以及位于控温室上方的真空沉积室,其中控温室中设置有:
有机铂族金属升华器;
载气盘管,设置有载气控制阀并与升华器的底部连通;以及
反应气盘管,设置有反应气控制阀,
其中主管道从升华器顶部延伸至真空沉积室底部以将二者相互连通,并设置有位于控温室中的主管道控制阀,
反应气盘管与主管道控制阀上部的主管道部分连通,
真空沉积室中设置有电加热体,电加热体的加热底面适于设置待沉积基底。
2.根据权利要求1的CVD装置,其中真空沉积室位于控温室顶部,主管道在真空沉积室中的开口朝向电加热体的加热底面。
3.根据权利要求2的CVD装置,其中主管道在真空沉积室中的开口与电加热体的加热底面上设置的待沉积基底间距1-3cm。
4.根据权利要求1的CVD装置,还包括位于真空沉积室外部用于对其进行抽真空的真空泵。
5.根据权利要求1的CVD装置,其中升华器还设置有气压计。
6.一种有机铂族金属化学气相沉积方法,包括:
在控温室中分别提供升华器、载气盘管和反应气盘管;
提供位于控温室顶部上的真空沉积室;
在真空沉积室中提供电加热体;
提供从升华器顶部延伸至真空沉积室底部以将二者直接连通的主管道,并在主管道上提供主管道控制阀;
其中载气盘管设置有载气控制阀并与升华器的底部连通,反应气盘管设置有反应气控制阀并与主管道控制阀上部的主管道部分连通,主管道在真空沉积室中的开口朝向电加热体的加热底面,
在电加热体的加热底面设置待沉积基底;
在升华器中提供有机铂族金属;
提供用于对真空沉积室进行抽真空的真空泵;
关闭载气控制阀和反应气控制阀,打开主管道控制阀,打开真空泵进行抽真空操作;
关闭主管道控制阀;
将控温室加热至预定温度,以将有机铂族金属进行升华并分别预热载气盘管中的载气和反应气盘管中的反应气;
开启电加热体将待沉积基底加热至设定温度;
打开反应气控制阀,以将反应气通过主管道送入真空沉积室;
再分别打开载气控制阀和主管道控制阀,以通过载气将升华器中的有机铂族金属升华气体送入真空沉积室;
整个过程中保持真空泵开启直至真空沉积完成。
7.根据权利要求6的方法,其中有机铂族金属为乙酰丙酮铂,载气为氮气,反应气为氧气。
8.根据权利要求7的方法,真空沉积过程中载气流量为50-300ml/min,反应气流量为20-150ml/min。
9.根据权利要求6的方法,其中控温室加热至165℃~185℃的升华温度,待沉积基底加热至455℃~485℃。
10.根据权利要求6的方法,其中真空沉积时间为5-30分钟。
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