CN104599947A - 氧化锆绝缘薄膜及其制备方法 - Google Patents
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Abstract
一种氧化锆绝缘薄膜及其制备方法,通过将乙酰丙酮锆溶于二甲基甲酰胺中,并添加乙醇胺、油酸作为稳定剂混合制成前驱体溶液,通过将前驱体溶液涂覆在衬底上经退火处理制成氧化锆绝缘薄膜。本发明制备得到的氧化锆绝缘薄膜,厚度为5~25nm,介电常数为10~23,在1MV/cm下漏电流小于1E‐9A/cm2,4MV/cm下漏电流小于1E‐8A/cm2。
Description
技术领域
本发明涉及的是一种半导体器件制备领域的技术,具体是一种应用于TFT(Thin‐FilmTransistor,薄膜晶体管)器件、MIM(metal insulator metal,金属、绝缘层、金属夹心结构)器件或AMOLED(Active MatrixOrganic Light Emitting Diode,有源矩阵有机发光二极管)器件的氧化锆绝缘薄膜及其制备方法。
背景技术
现有绝缘薄膜多采用化学气相沉积、磁控溅射等真空镀膜方法,这种生产工艺要求真空条件、特定的靶材及气体环境,且设备的生产与维护成本较高;也有部分文献资料采用溶液法制备绝缘薄膜,但大多需要高温退火,这限制了绝缘薄膜的应用范围。为解决这一问题,本专利公开了一种溶液法制备绝缘薄膜的方法,该方法用旋涂机将前驱物溶液旋涂到衬底上,然后通过加热退火或紫外光照射退火的方法制得绝缘薄膜,在大气环境中即可完成操作,制备工艺温度低、简单、可控、成本低,制得的氧化锆绝缘薄膜性能优良。
经过对现有技术的检索发现:中国专利文献号CN102709176A公开(公告)日2012.10.03,公开了一种MIM型电容中绝缘体二氧化硅薄膜的制备方法,包括提供衬底;利用次大气压化学气相沉积法在衬底上沉积二氧化硅薄膜;对沉积形成的二氧化硅薄膜进行紫外光照射;取出衬底。但由于利用化学气相沉积二氧化硅薄膜,需要真空条件,以及特定的靶材与气体环境,对生产设备要求高。此外,该技术制备的二氧化硅绝缘薄膜,虽经紫外光照射工艺处理降低了氢含量、提高了薄膜密度,但二氧化硅本身的性质仍限制了薄膜的性能。
中国专利文献号CN104009093A公开(公告)日2014.08.27,公开了一种高k介电层水性氧化铟薄膜晶体管的制备方法,先将乙酰丙酮锆溶于二甲基甲酰胺中,同时加入与乙酰丙酮锆等摩尔量的乙醇胺作为稳定剂形成前驱体溶液;再在清洗后的低阻硅衬底上旋涂前驱体溶液得到样品,将样品放到高压汞灯下进行紫外光照处理得到光退火后的样品;然后将光退火后的样品进行退火得到薄膜样品;然后在得到的薄膜样品表面旋涂In2O3水性溶液得到In2O3沟道层;最后在In2O3沟道层上面制备源、漏电极,即得到薄膜晶体管;但该技术经过紫外光照处理后得到的样品,还需要进行300℃的加热退火,这增加了工艺步骤,提高了工艺温度,限制了工艺的应用范围。
发明内容
本发明针对现有技术存在的上述不足,提出一种氧化锆绝缘薄膜及其制备方法,采用溶液法制备氧化锆绝缘薄膜,通过控制旋涂转速和时间来调节薄膜厚度,然后将旋涂好的样品经过加热退火或紫外光照射退火制得氧化锆薄膜,该工艺制得的薄膜厚度范围为5~25nm,介电常数范围为10~23。本发明无需加热,只需光照处理即可制得性能良好的绝缘薄膜。
本发明是通过以下技术方案实现的:
本发明涉及一种氧化锆绝缘薄膜的制备方法,通过将乙酰丙酮锆溶于二甲基甲酰胺中,并添加乙醇胺、油酸作为稳定剂混合制成前驱体溶液,通过将前驱体溶液涂覆在衬底上经退火处理制成氧化锆绝缘薄膜。
所述的前驱体溶液中:100~500mg乙酰丙酮锆,1~5mL二甲基酰胺,1~5mL乙醇胺,0.1~1mL油酸。
所述的混合是指:将前驱体溶液充分搅拌,优选在50~80℃下搅拌1~3小时。
所述的涂覆优选但不限于采用旋转涂覆方式实现,旋涂速度为2000~5000rpm,旋涂时间:30~60秒。
所述的退火处理包括但不限于加热退火或紫外光照射退火,其中:加热退火温度为300~600℃,加热时间1~3小时;紫外光照退火的波长为200~400nm,光强为30~300mW/cm2,照射时间30~90分钟。
本发明通过上述方法制备得到的氧化锆绝缘薄膜,其厚度范围为5~25nm,介电常数范围为10~23。
本发明涉及上述氧化锆绝缘薄膜的应用,将其用于制备MIM或TFT器件,也可用于制备AMOLED中的介质层。
技术效果
与传统的二氧化硅绝缘薄膜,氧化锆绝缘薄膜有更好的绝缘性能,一般二氧化硅绝缘层在1MV/cm下漏电流约为1E‐7A/cm2,4MV/cm下漏电流约为1E‐5A/cm2,而采取本发明制作的氧化锆绝缘薄膜在1MV/cm下漏电流小于1E‐9A/cm2,4MV/cm下漏电流小于1E‐8A/cm2。
附图说明
图1和图2为本发明氧化锆薄膜AFM图。
图3为实施例中漏电流检测示意图。
图4为实施例中XPS分析图谱。
具体实施方式
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
本实施例采用以下操作步骤:
1)将乙酰丙酮锆溶于二甲基甲酰胺中,并添加乙醇胺、油酸作为稳定剂混合制成前驱体溶液;
2)将1寸硅片清洗干净,在硅片上旋涂乙酰丙酮锆前驱体溶液,旋涂速度2000rpm,旋涂时间30秒;
3)将样品放置到高压汞灯下进行紫外光照射45分钟制得氧化锆薄膜;
如图1所示,为本实施例制备得到的氧化锆薄膜AFM图,如图1、图2所示,本发明制取的薄膜表面平整,无孔洞无裂纹,表面粗糙度只有0.638。
如图4所示,为本实施例制备得到的产物的XPS分析图谱,薄膜经退火处理后,杂质元素很少,基本只有氧和锆元素,还有少量的C元素。
实施例2
本实施例采用以下操作步骤:
1)按照与实施例1相同的方式配制乙酰丙酮锆的前驱体溶液;
2)将1寸玻璃清洗干净,在1寸玻璃上热蒸镀70nm铝电极;
3)在铝上面旋涂乙酰丙酮锆前驱体溶液,旋涂速度2000rpm,旋涂时间30秒;
4)将样品放置到高压汞灯下进行紫外光照射45分钟制得氧化锆薄膜;
5)在氧化锆薄膜上面通过shadow mask热蒸镀70nm铝电极,铝电极的尺寸为1mm×0.2mm。
如图3所示,本实施例制备得到的氧化锆绝缘薄膜在1MV/cm下漏电流小于1E‐9A/cm2,4MV/cm下漏电流小于1E‐8A/cm2。
Claims (7)
1.一种氧化锆绝缘薄膜的制备方法,其特征在于,通过将乙酰丙酮锆溶于二甲基甲酰胺中,并添加乙醇胺、油酸作为稳定剂混合制成前驱体溶液,通过将前驱体溶液涂覆在衬底上经退火处理制成氧化锆绝缘薄膜。
2.根据权利要求1所述的方法,其特征是,所述的前驱体溶液中:100~500mg乙酰丙酮锆,1~5mL二甲基酰胺,1~5mL乙醇胺,0.1~1mL油酸。
3.根据权利要求1所述的方法,其特征是,所述的混合是指:将前驱体溶液充分搅拌,具体为50~80℃下搅拌1~3小时。
4.根据权利要求1所述的方法,其特征是,所述的涂覆采用旋转涂覆方式实现,旋涂速度为2000~5000rpm,旋涂时间:30~60秒。
5.根据权利要求1所述的方法,其特征是,所述的退火处理包括加热退火或紫外光照射退火,其中:加热退火温度为300~600℃,加热时间1~3小时;紫外光照退火的波长为200~400nm,光强为30~300mW/cm2,照射时间30~90分钟。
6.一种根据上述任一权利要求所述方法制备得到的氧化锆绝缘薄膜,其特征在于,厚度为5~25nm,介电常数为10~23,在1MV/cm下漏电流小于1E‐9A/cm2,4MV/cm下漏电流小于1E‐8A/cm2。
7.一种根据上述任一权利要求中所述的氧化锆绝缘薄膜的应用,其特征在于,将其用于制备MIM或TFT器件,也可以用做AMOLED器件中的介质层。
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104945962A (zh) * | 2015-05-13 | 2015-09-30 | 上海交通大学 | 金属氧化物保护膜及其制备方法 |
CN106431397A (zh) * | 2016-09-14 | 2017-02-22 | 齐鲁工业大学 | 一种高介电氧化锆薄膜的低温溶液制备方法 |
CN107902694A (zh) * | 2017-11-30 | 2018-04-13 | 齐鲁工业大学 | 一种快速制备氧化锆薄膜的低温液相方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20040222476A1 (en) * | 2002-01-17 | 2004-11-11 | Micron Technology, Inc. | Highly reliable amorphous high-k gate dielectric ZrOxNy |
CN1986725A (zh) * | 2006-12-14 | 2007-06-27 | 上海交通大学 | CdSe量子点的制备方法 |
CN101787522A (zh) * | 2010-04-02 | 2010-07-28 | 南京大学 | 一种超高密度有序的磁性纳米颗粒复合薄膜的制备方法 |
CN102716745A (zh) * | 2011-03-29 | 2012-10-10 | 中国科学院大连化学物理研究所 | 蛋黄-蛋壳型有机-无机杂化氧化硅纳米球的制备方法 |
CN103928350A (zh) * | 2014-04-24 | 2014-07-16 | 青岛大学 | 一种双沟道层薄膜晶体管的制备方法 |
-
2014
- 2014-12-24 CN CN201410836235.4A patent/CN104599947A/zh active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20040222476A1 (en) * | 2002-01-17 | 2004-11-11 | Micron Technology, Inc. | Highly reliable amorphous high-k gate dielectric ZrOxNy |
CN1986725A (zh) * | 2006-12-14 | 2007-06-27 | 上海交通大学 | CdSe量子点的制备方法 |
CN101787522A (zh) * | 2010-04-02 | 2010-07-28 | 南京大学 | 一种超高密度有序的磁性纳米颗粒复合薄膜的制备方法 |
CN102716745A (zh) * | 2011-03-29 | 2012-10-10 | 中国科学院大连化学物理研究所 | 蛋黄-蛋壳型有机-无机杂化氧化硅纳米球的制备方法 |
CN103928350A (zh) * | 2014-04-24 | 2014-07-16 | 青岛大学 | 一种双沟道层薄膜晶体管的制备方法 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104945962A (zh) * | 2015-05-13 | 2015-09-30 | 上海交通大学 | 金属氧化物保护膜及其制备方法 |
CN106431397A (zh) * | 2016-09-14 | 2017-02-22 | 齐鲁工业大学 | 一种高介电氧化锆薄膜的低温溶液制备方法 |
CN107902694A (zh) * | 2017-11-30 | 2018-04-13 | 齐鲁工业大学 | 一种快速制备氧化锆薄膜的低温液相方法 |
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Application publication date: 20150506 |