CN109616525A - 一种溶液法制备锆铝氧化物绝缘层薄膜及叠层结构的方法 - Google Patents
一种溶液法制备锆铝氧化物绝缘层薄膜及叠层结构的方法 Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 41
- HVXCTUSYKCFNMG-UHFFFAOYSA-N aluminum oxygen(2-) zirconium(4+) Chemical compound [O-2].[Zr+4].[Al+3] HVXCTUSYKCFNMG-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 31
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- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 5
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- 230000015556 catabolic process Effects 0.000 abstract description 8
- SWCIQHXIXUMHKA-UHFFFAOYSA-N aluminum;trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SWCIQHXIXUMHKA-UHFFFAOYSA-N 0.000 abstract description 5
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- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 229910002651 NO3 Inorganic materials 0.000 description 11
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 description 7
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- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 4
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- 159000000013 aluminium salts Chemical class 0.000 description 4
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 4
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- 229910007875 ZrAlO Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 229910052593 corundum Inorganic materials 0.000 description 1
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- GGDKOXQCDTUUIG-UHFFFAOYSA-N dialuminum;oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zr+4] GGDKOXQCDTUUIG-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 238000006116 polymerization reaction Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于薄膜晶体管技术领域,公开了一种溶液法制备锆铝氧化物绝缘层薄膜及叠层结构的方法。所述方法包括如下步骤:将五水合硝酸锆和九水合硝酸铝溶于乙二醇单甲醚中,搅拌老化得到前驱体溶液;在ITO玻璃衬底上旋涂所得的前驱体溶液,然后在300~500℃退火处理1~2h,得到锆铝氧化物绝缘层薄膜。在所得锆铝氧化物绝缘层薄膜上通过磁控溅射镀圆形Al电极,得到MIM叠层结构。本发明提高绝缘薄膜的物理化学性能,如漏电流密度从6.71×10‑5A/cm2降低为3.8×10‑7A/cm2,禁带宽度从5.0eV提升为5.8eV,禁带宽度的增大将有利于提高击穿电压。
Description
技术领域
本发明属于薄膜晶体管技术领域,具体涉及一种溶液法制备锆铝氧化物绝缘层薄膜及叠层结构的方法。
背景技术
薄膜晶体管(Thin Film Transistor,简称TFT),是一种用途广泛的半导体器件,其最重要的用途是在显示器中用于驱动液晶排列变化、以及驱动OLED像素发光。TFT中绝缘层能起到存储电容和防止信号串扰等作用,既影响TFT器件的转移性能,又影响其稳定性和寿命。
近年来,金属氧化物绝缘薄膜因其性能优异,具有稳定性好和均匀性好等优点,引起了越来越多研究者的关注。然而,一元氧化物都有各自的优缺点,ZrO2有高的相对介电常数(~27)、较宽的禁带(~5eV)、较好的电学稳定性和界面态密度,但漏电高和击穿电场低;Al2O3的禁带宽度大(~8eV),从而使得其击穿电场较高且漏电流较低,但相对的其介电常数(~9)比其他高介电常数氧化物要低。因此,如何将多种金属氧化物进行复合,从而做到取长补短,制备性能更优异的绝缘薄膜是个亟待解决的问题。
发明内容
针对以上现有技术存在的缺点和不足之处,本发明的首要目的在于提供一种溶液法制备锆铝氧化物绝缘层薄膜的方法。
本发明的再一目的在于提供一种溶液法制备锆铝氧化物绝缘层薄膜叠层结构的方法。
本发明目的通过以下技术方案实现:
一种溶液法制备锆铝氧化物绝缘层薄膜的方法,包括如下制备步骤:
(1)将Zr(NO3)4·5H2O(五水合硝酸锆)和Al(NO3)3·9H2O(九水合硝酸铝)溶于乙二醇单甲醚(2-MOE)中,搅拌老化得到前驱体溶液;
(2)在ITO玻璃衬底上旋涂步骤(1)所得的前驱体溶液,然后在300~500℃退火处理1~2h,得到锆铝氧化物绝缘层薄膜。
优选地,步骤(1)中所述前驱体溶液中Zr(NO3)4·5H2O的浓度为0.1~0.3mol/L,Al(NO3)3·9H2O的浓度为0.1~0.3mol/L。
优选地,步骤(2)中所述旋涂的工艺条件为:转速4000~6000rpm,匀胶次数1~5次,匀胶时间30~40s,每次匀胶之间退火温度350℃,时间3~5min。
一种溶液法制备锆铝氧化物绝缘层薄膜叠层结构的方法,在所得锆铝氧化物绝缘层薄膜上通过磁控溅射镀圆形Al电极,得到MIM(ITO/ZrAlOx/Al)叠层结构。
本发明的原理为:将Zr(NO3)4·5H2O(五水合硝酸锆)和Al(NO3)3·9H2O(九水合硝酸铝)溶于乙二醇单甲醚中可以得到含锆盐和铝盐的前驱体溶液,将溶液旋涂、热退火处理后,溶液发生水解和聚合等反应形成锆铝氧化物薄膜。
与现有技术相比,本发明具有如下优点及有益效果:
本发明通过将Zr(NO3)4·5H2O(五水合硝酸锆)和Al(NO3)3·9H2O(九水合硝酸铝)混合溶于乙二醇单甲醚中,得到含锆盐和铝盐的前驱体溶液。利用锆盐和铝盐混合的前驱体溶液可以制备得到锆铝氧化物薄膜,从而能够整合氧化锆和氧化铝的优势,提高绝缘薄膜的物理化学性能,如漏电流密度从6.71×10-5A/cm2降低为3.8×10-7A/cm2,禁带宽度从5.0eV提升为5.8eV,同时禁带宽度的增大将有利于提高击穿电压。
附图说明
图1是实施例1所得锆铝氧化物绝缘层薄膜的漏电流密度曲线图。
图2是实施例2所得锆铝氧化物绝缘层薄膜的漏电流密度曲线图。
图3是实施例1所得锆铝氧化物绝缘层薄膜的介电常数曲线图。
图4是实施例2所得锆铝氧化物绝缘层薄膜的介电常数曲线图。
图5是实施例1所得锆铝氧化物绝缘层薄膜的禁带宽度拟合图。
图6是实施例2所得锆铝氧化物绝缘层薄膜的禁带宽度拟合图。
具体实施方式
下面结合实施例及附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例1
(1)前驱体配制:将1.288g Zr(NO3)4·5H2O(五水合硝酸锆)和0.3751gAl(NO3)3·9H2O(九水合硝酸铝)溶于10ml乙二醇单甲醚(2-MOE)中,搅拌老化得到含锆盐0.3mol/L和铝盐0.1mol/L的前驱体溶液。
(2)衬底制备:在玻璃基板表面沉积一层150n。m的ITO电极,清洗烘干,得到ITO玻璃衬底。
(3)在ITO玻璃衬底按所选工艺参数旋涂步骤(1)所得的前驱体溶液,旋涂转速5000rpm,匀胶时间40s,匀胶次数2次,每次匀胶之间退火温度350℃,时间4min,然后在350℃退火处理1h,得到锆铝氧化物绝缘层薄膜。
(4)在步骤(3)的氧化锆绝缘层薄膜上通过磁控溅射镀100nm的圆形Al电极,制备MIM(ITO/ZrAlOx/Al)叠层结构。
本实施例所得锆铝氧化物绝缘层薄膜的漏电流测试结果如图1所示。
本实施例所得锆铝氧化物绝缘层薄膜的介电常数测试结果如图3所示。
本实施例所得锆铝氧化物绝缘层薄膜的禁带宽度测试结果如图5所示。
测试结果表明本实施例制备的锆铝氧化物绝缘层薄膜具有较好的绝缘性能,其漏电流密度为3.8×10-7A/cm2,相比纯的氧化锆绝缘薄膜(漏电流密度为6.71×10-5A/cm2)有较大的提高,介电常数约为25,禁带宽度为5.63eV,禁带宽度的增大有利于提高击穿电压。相比纯的氧化锆绝缘薄膜,锆铝氧化物绝缘层薄膜可以在保持较高介电常数的前提下提高禁带宽度,从而降低漏电流密度、提高击穿电压。
实施例2
(1)前驱体配制:将0.4293g Zr(NO3)4·5H2O(五水合硝酸锆)和1.1253gAl(NO3)3·9H2O(九水合硝酸铝)溶于10ml乙二醇单甲醚(2-MOE)中,搅拌老化得到含锆盐0.1mol/L和铝盐0.3mol/L的前驱体溶液。
(2)衬底制备:在玻璃基板表面沉积一层150nm的ITO电极,清洗烘干,得到ITO玻璃衬底。
(3)在ITO玻璃衬底按所选工艺参数旋涂步骤(1)所得的前驱体溶液,旋涂转速5000rpm,匀胶时间40s,匀胶次数2次,每次匀胶之间退火温度350℃,时间4min,然后在200℃退火处理1h,得到锆铝氧化物绝缘层薄膜。
(4)在步骤(3)的氧化锆绝缘层薄膜上通过磁控溅射镀100nm的圆形Al电极,制备MIM(ITO/ZrO2/Al)叠层结构。
本实施例所得锆铝氧化物绝缘层薄膜的漏电流测试结果如图2所示。
本实施例所得锆铝氧化物绝缘层薄膜的介电常数测试结果如图4所示。
本实施例所得锆铝氧化物绝缘层薄膜的禁带宽度测试结果如图6所示。测试结果表明本实施例制备的锆铝氧化物绝缘层薄膜具有较好的绝缘性能,其漏电流密度为3.0×10-7A/cm2,相比纯的氧化锆绝缘薄膜(漏电流密度为6.71×10-5A/cm2)有较大的提高,介电常数约为21,禁带宽度为5.84eV,禁带宽度的增大有利于提高击穿电压。相比纯的氧化锆绝缘薄膜,锆铝氧化物绝缘层薄膜可以在保持较高介电常数的前提下提高禁带宽度,从而降低漏电流密度、提高击穿电压。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (5)
1.一种溶液法制备锆铝氧化物绝缘层薄膜的方法,其特征在于,包括如下制备步骤:
(1)将Zr(NO3)4·5H2O和Al(NO3)3·9H2O溶于乙二醇单甲醚中,搅拌老化得到前驱体溶液;
(2)在ITO玻璃衬底上旋涂步骤(1)所得的前驱体溶液,然后在300~500℃退火处理1~2h,得到锆铝氧化物绝缘层薄膜。
2.根据权利要求1所述的溶液法制备锆铝氧化物绝缘层薄膜的方法,其特征在于,步骤(1)中所述前驱体溶液中Zr(NO3)4·5H2O的浓度为0.1~0.3mol/L。
3.根据权利要求1或2所述的溶液法制备锆铝氧化物绝缘层薄膜的方法,其特征在于,步骤(1)中所述前驱体溶液中Al(NO3)3·9H2O的浓度为0.1~0.3mol/L。
4.根据权利要求3所述的溶液法制备锆铝氧化物绝缘层薄膜的方法,其特征在于,步骤(2)中所述旋涂的工艺条件为:转速4000~6000rpm,匀胶次数1~5次,匀胶时间30~40s,每次匀胶之间退火温度350℃,时间3~5min。
5.一种溶液法制备锆铝氧化物绝缘层薄膜叠层结构的方法,其特征在于,在权利要求1~4任一项所述溶液法制得的锆铝氧化物绝缘层薄膜上通过磁控溅射镀圆形Al电极,得到MIM叠层结构。
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