WO2020108140A1 - 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 PDF

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WO2020108140A1
WO2020108140A1 PCT/CN2019/111352 CN2019111352W WO2020108140A1 WO 2020108140 A1 WO2020108140 A1 WO 2020108140A1 CN 2019111352 W CN2019111352 W CN 2019111352W WO 2020108140 A1 WO2020108140 A1 WO 2020108140A1
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insulating layer
oxide insulating
zirconium
aluminum oxide
layer film
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宁洪龙
周尚雄
姚日晖
蔡炜
朱镇南
梁志豪
张观广
张旭
梁宏富
彭俊彪
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South China University of Technology SCUT
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D30/00—Field-effect transistors [FET]
    • H10D30/60—Insulated-gate field-effect transistors [IGFET]
    • H10D30/67—Thin-film transistors [TFT]
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D30/00—Field-effect transistors [FET]
    • H10D30/01—Manufacture or treatment
    • H10D30/021—Manufacture or treatment of FETs having insulated gates [IGFET]
    • H10D30/031—Manufacture or treatment of FETs having insulated gates [IGFET] of thin-film transistors [TFT]
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/63—Formation of materials, e.g. in the shape of layers or pillars of insulating materials characterised by the formation processes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/69—Inorganic materials
    • H10P14/692—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses
    • H10P14/6938—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides
    • H10P14/6939—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal
    • H10P14/69391—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal the material containing aluminium, e.g. Al2O3
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
    • H10P14/69—Inorganic materials
    • H10P14/692—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses
    • H10P14/6938—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides
    • H10P14/6939—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal
    • H10P14/69395—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal the material containing zirconium, e.g. ZrO2

Definitions

  • the invention belongs to the technical field of thin film transistors, and particularly relates to a method for preparing a zirconium aluminum oxide insulating layer film and a stacked structure by a solution method.
  • Thin film transistor Thin Film Transistor, TFT for short
  • TFT Thin Film Transistor
  • the insulating layer in the TFT can play the role of storage capacitance and prevent signal crosstalk, which not only affects the transfer performance of the TFT device, but also affects its stability and life.
  • ZrO 2 has a high relative dielectric constant ( ⁇ 27), a wide band gap ( ⁇ 5eV), good electrical stability and interface state density, but high leakage current Low breakdown electric field
  • Al 2 O 3 has a large band gap ( ⁇ 8eV), which makes its breakdown electric field higher and leakage current lower, but its relative dielectric constant ( ⁇ 9) is higher than other high dielectrics Constant oxides are lower. Therefore, how to combine multiple metal oxides to make up for each other's strengths and weaknesses and prepare an insulating film with better performance is an urgent problem to be solved.
  • the primary object of the present invention is to provide a solution method for preparing a zirconium aluminum oxide insulating layer film.
  • Still another object of the present invention is to provide a method for preparing a zirconium aluminum oxide insulating layer film laminated structure by a solution method.
  • a method for preparing a zirconium aluminum oxide insulating layer film by a solution method includes the following preparation steps:
  • step (2) The precursor solution obtained in step (1) is spin-coated on an ITO glass substrate, and then annealed at 300 to 500°C for 1 to 2 hours to obtain a zirconium aluminum oxide insulating layer thin film.
  • the concentration of Zr(NO 3 ) 4 ⁇ 5H 2 O in the precursor solution in step (1) is 0.1-0.3 mol/L
  • the concentration of Al(NO 3 ) 3 ⁇ 9H 2 O is 0.1-0.3 mol/L.
  • the process conditions of the spin coating in step (2) are: rotation speed 4000-6000rpm, homogenization times 1-5 times, homogenization time 30-40s, annealing temperature 350 °C, time 3 ⁇ 5min.
  • a method for preparing a laminated structure of a zirconium aluminum oxide insulating layer film by a solution method a circular Al electrode is plated on the obtained zirconium aluminum oxide insulating layer film by magnetron sputtering to obtain a MIM (ITO/ZrAlO x /Al) stack Layer structure.
  • the principle of the present invention is: dissolving Zr(NO 3 ) 4 ⁇ 5H 2 O (zirconium nitrate pentahydrate) and Al(NO 3 ) 3 ⁇ 9H 2 O (aluminum nitrate nonahydrate) in ethylene glycol monomethyl ether A precursor solution containing a zirconium salt and an aluminum salt is obtained. After the solution is spin-coated and thermally annealed, the solution undergoes hydrolysis and polymerization reactions to form a zirconium aluminum oxide film.
  • the present invention has the following advantages and beneficial effects:
  • Zr(NO 3 ) 4 .5H 2 O zirconium nitrate pentahydrate
  • Al(NO 3 ) 3 .9H 2 O aluminum nitrate nonahydrate
  • a zirconium aluminum oxide film can be prepared by using a mixed precursor solution of zirconium salt and aluminum salt, which can integrate the advantages of zirconium oxide and aluminum oxide and improve the physical and chemical properties of the insulating film, such as leakage current density from 6.71 ⁇ 10 -5 A /cm 2 is reduced to 3.8 ⁇ 10 -7 A/cm 2 , the width of the band gap is increased from 5.0 eV to 5.8 eV, and the increase of the width of the band gap will help to improve the breakdown voltage.
  • FIG. 1 is a graph showing the leakage current density of the zirconium aluminum oxide insulating layer film obtained in Example 1.
  • FIG. 2 is a graph showing the leakage current density of the zirconium aluminum oxide insulating layer film obtained in Example 2.
  • FIG. 3 is a graph of the dielectric constant of the zirconium aluminum oxide insulating layer film obtained in Example 1.
  • FIG. 4 is a graph of the dielectric constant of the zirconium aluminum oxide insulating layer film obtained in Example 2.
  • FIG. 5 is a fitting diagram of the band gap of the zirconium aluminum oxide insulating layer film obtained in Example 1.
  • FIG. 5 is a fitting diagram of the band gap of the zirconium aluminum oxide insulating layer film obtained in Example 1.
  • FIG. 6 is a fitting diagram of the band gap of the zirconium aluminum oxide insulating layer film obtained in Example 2.
  • FIG. 6 is a fitting diagram of the band gap of the zirconium aluminum oxide insulating layer film obtained in Example 2.
  • Precursor preparation dissolve 1.288g Zr(NO 3 ) 4 ⁇ 5H 2 O (zirconium nitrate pentahydrate) and 0.3751g Al(NO 3 ) 3 ⁇ 9H 2 O (aluminum nitrate nonahydrate) in 10 ml of ethylene dichloride In alcohol monomethyl ether (2-MOE), stirring and aging to obtain a precursor solution containing 0.3 mol/L of zirconium salt and 0.1 mol/L of aluminum salt.
  • 2-MOE alcohol monomethyl ether
  • Substrate preparation deposit a layer of 150n on the surface of the glass substrate. m ITO electrode, washed and dried to obtain ITO glass substrate.
  • a 100-nm circular Al electrode was plated on the zirconia insulating layer film of step (3) by magnetron sputtering to prepare a MIM (ITO/ZrAlO x /Al) laminated structure.
  • the leakage current test result of the zirconium aluminum oxide insulating layer film obtained in this embodiment is shown in FIG. 1.
  • the dielectric constant test result of the zirconium aluminum oxide insulating layer film obtained in this embodiment is shown in FIG. 3.
  • the test results show that the zirconium aluminum oxide insulating layer film prepared in this example has good insulation performance, and its leakage current density is 3.8 ⁇ 10 -7 A/cm 2 , compared with the pure zirconium oxide insulating film (leakage current density is 6.71 ⁇ 10 -5 A/cm 2 ) has a large improvement, the dielectric constant is about 25, the band gap width is 5.63eV, the increase of the band gap width is conducive to increase the breakdown voltage. Compared with pure zirconia insulating films, zirconium aluminum oxide insulating film can increase the band gap width while maintaining a high dielectric constant, thereby reducing leakage current density and increasing breakdown voltage.
  • Precursor preparation dissolve 0.4293g Zr(NO 3 ) 4 ⁇ 5H 2 O (zirconium nitrate pentahydrate) and 1.1253g Al(NO 3 ) 3 ⁇ 9H 2 O (aluminum nitrate nonahydrate) in 10 ml ethylenedioxide In alcohol monomethyl ether (2-MOE), the solution of the precursor containing 0.1 mol/L of zirconium salt and 0.3 mol/L of aluminum salt was obtained by stirring and aging.
  • 2-MOE alcohol monomethyl ether
  • Substrate preparation deposit a layer of 150nm ITO electrode on the surface of the glass substrate, wash and dry to obtain an ITO glass substrate.
  • a 100-nm circular Al electrode was plated on the zirconia insulating layer film of step (3) by magnetron sputtering to prepare a MIM (ITO/ZrO 2 /Al) laminated structure.
  • the leakage current test result of the zirconium aluminum oxide insulating layer film obtained in this embodiment is shown in FIG. 2.
  • the dielectric constant test result of the zirconium aluminum oxide insulating layer film obtained in this embodiment is shown in FIG. 4.
  • the test result of the forbidden band width of the zirconium aluminum oxide insulating layer film obtained in this embodiment is shown in FIG. 6.
  • the test results show that the zirconium aluminum oxide insulation layer film prepared in this example has good insulation performance, and its leakage current density is 3.0 ⁇ 10 -7 A/cm 2 , which is higher than that of pure zirconium oxide insulation film (leakage current density is 6.71 ⁇ 10 -5 A/cm 2 ) has a great improvement, the dielectric constant is about 21, the band gap width is 5.84eV, the increase of the band gap width is conducive to improving the breakdown voltage.
  • zirconium aluminum oxide insulating film can increase the band gap width while maintaining a high dielectric constant, thereby reducing leakage current density and increasing breakdown voltage.

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Abstract

薄膜晶体管技术领域，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，所述方法能够提高绝缘薄膜的物理化学性能，如漏电流密度从6.71×10 -5A/cm 2降低为3.8×10 -7A/cm 2，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

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 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，ZrO 2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；Al 2O 3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(NO 3) 4·5H 2O(五水合硝酸锆)和Al(NO 3) 3·9H 2O(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(NO 3) 4·5H 2O的浓度为0.1～0.3mol/L，Al(NO 3) 3·9H 2O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/ZrAlO x/Al)叠层结构。
本发明的原理为：将Zr(NO 3) 4·5H 2O(五水合硝酸锆)和Al(NO 3) 3·9H 2O(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(NO 3) 4·5H 2O(五水合硝酸锆)和Al(NO 3) 3·9H 2O(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/cm 2降低为3.8×10 -7A/cm 2，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(NO 3) 4·5H 2O(五水合硝酸锆)和0.3751g Al(NO 3) 3·9H 2O(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/ZrAlO x/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/cm 2，相比纯的氧化锆绝缘薄膜(漏电流密度为6.71×10 -5A/cm 2)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(NO 3) 4·5H 2O(五水合硝酸锆)和1.1253g Al(NO 3) 3·9H 2O(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/ZrO 2/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/cm 2，相比纯的氧化锆绝缘薄膜(漏电流密度为6.71×10 -5A/cm 2)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(NO 3) 4·5H 2O和Al(NO 3) 3·9H 2O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(NO 3) 4·5H 2O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(NO 3) 3·9H 2O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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