CN106373863A - 一种制备铟铝氧透明半导体薄膜的低温液相方法 - Google Patents
一种制备铟铝氧透明半导体薄膜的低温液相方法 Download PDFInfo
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
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- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02697—Forming conducting materials on a substrate
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- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明属于新材料及半导体领域,特别涉及一种制备铟铝氧透明半导体薄膜的低温液相方法。包括如下步骤:称取可溶性的铟盐、铝盐,量取溶剂,配置浓度为0.01‑0.5摩尔/升的铟铝氧前驱体溶液,经过0.1‑3小时的磁力搅拌和超声分散形成澄清透明的铟铝氧前驱体溶液;制备铟铝氧薄膜:将铟铝氧前驱体溶液涂覆到清洗好的衬底上形成铟铝氧前驱体薄膜,进行50‑150℃的预热处理,然后经过一定功率、时间和温度的光波退火,根据铟铝氧薄膜的厚度要求可多次涂覆前驱体铟铝氧溶液并退火处理,即得到铟铝氧透明半导体薄膜。本发明所得铟铝氧薄膜在晶体管、存储器、太阳能电池等信息能源领域有重要应用前景。通过本发明的工艺可以避免通常的高温溶液工艺、工艺周期长或昂贵设备等,成本低,适合工业化大规模生产。
Description
技术领域
本发明属于新材料及半导体领域,特别涉及一种制备铟铝氧透明半导体薄膜的低温液相方法,铟铝氧透明薄膜在晶体管、存储器、太阳能电池等信息能源领域有重要应用前景。
背景技术
在科学技术日新月异的今天,半导体材料的发展经历了第一代以锗、硅为代表的元素半导体,第二代以砷化镓、磷化铟为代表的化合物半导体,第三代半导体材料则以氮化镓、碳化硅、氧化锌等宽禁带半导体为代表,它们一般具有更高的击穿电场、热导率、电子饱和速率和更高的抗辐射能力,因而更适合于制作高温、高频及大功率器件,其中的In2O3和ZnO等宽禁带半导体氧化物材料都是重要的光电子信息材料,在透明导电氧化物方面有很多的应用。透明导电氧化物(transparent conductive oxide简称TCO)薄膜主要包括In、Sn、Zn和Ga的氧化物及其复合多元氧化物薄膜材料。在透明导电氧化物薄膜的不同应用领域,对透明导电氧化物薄膜的性能提出了不同的要求。目前应用较多的是单掺杂的薄膜,用途有些局限,性能比较单一。每一种透明导电氧化物材料都具有各自的特性,不可能满足所有的应用要求。为了开发适合特殊用途的TCO薄膜,一些研究小组将各种TCO材料进行组合,制各出一些具有新特点的TCO薄膜。多元TCO材料(如InGaZnO等)可以按各种比例组合、采用多种方法制成TCO薄膜,其性能与化学组分密切相关。InGaZnO薄膜可以同时具有其各组分氧化物的优点,它的化学稳定性与易刻蚀性及相关光电和结构等性质随组分的改变而改变。
目前制备铟铝氧薄膜的方法多种多样,主要包括气相法和液相法两大类。例如,磁控溅射、电子束蒸发、原子层沉积及化学气相沉积等方法都被用来制备铟铝氧薄膜。然而,这些气相方法通常需要真空环境,增加了设备的复杂性,提高了制备成本。近年来,液相方法日益引起了广泛的关注,例如溶胶-凝胶法、喷雾热解法等。近年来发展的液相法合成氧化铟基薄膜的研究报道有许多。例如,公开号为CN103779425A的中国发明专利公开了一种氧化铟基薄膜的制备方法,包括如下步骤:a)制备乙酰丙酮镓的乙醇溶液、乙酰丙酮锌水合物的乙醇溶液和乙酰丙酮铟的四氢呋喃溶液;b)将三种溶液进行混合并搅拌均匀,制得铟镓锌氧化物的前驱体溶液;c)将前驱体溶液沉积在基板材料上并进行退火处理,制得铟镓锌氧化物半导体薄膜。由上述发明专利可以看出,虽然液相法可以制备较高性能的氧化铟基薄膜,但液相法通常需要高温(高于400℃)退火,才能促使前驱体薄膜分解并致密化,形成致密的氧化铟基薄膜。因此,寻找一种新的低温液相制备技术,对于铟铝氧薄膜在各种领域的大规模应用是极为重要和迫切的。
发明内容
本发明的目的在于提供一种制备铟铝氧透明半导体薄膜的低温液相方法,实现铟铝氧透明半导体的简易高效制备,更易于大规模生产和应用。本发明的创新点主要在于:发展了新的低温光波方法高效合成铟铝氧透明半导体薄膜。
本发明的技术方案,具体包括以下步骤:
(1) 制备铟铝氧前驱体溶液:称取可溶性的铟盐、铝盐,量取溶剂,配置浓度为0.01-0.5摩尔/升的铟铝氧前驱体溶液,经过0.1-3小时的磁力搅拌和超声分散形成澄清透明的铟铝氧前驱体溶液;
(2) 制备铟铝氧薄膜:将铟铝氧前驱体溶液涂覆到清洗好的衬底上形成铟铝氧前驱体薄膜,进行50-150 ℃的预热处理,然后经过一定功率、时间和温度的光波退火,根据铟铝氧薄膜的厚度要求可多次涂覆前驱体铟铝氧溶液并退火处理,即得到铟铝氧透明半导体薄膜。
本发明所述制备方法的步骤(1)中,所述的可溶性的铟盐为硝酸铟、氯化铟、硫酸铟或乙酸铟中的一种或两种以上。
本发明所述制备方法的步骤(1)中,所述的可溶性的铝盐为硝酸铝、氯化铝、硫酸铝或乙酸铝中的一种或两种以上。
本发明所述制备方法的步骤(1)中,所述的溶剂为乙二醇甲醚、乙醇、水、乙二醇或二甲基甲酰胺中的一种或两种以上。
本发明所述制备方法的步骤(1)中,所述涂覆方法为旋转涂覆法、滴涂法、浸涂法、喷雾法或喷墨打印法。
本发明所述制备方法的步骤(1)中,所述的光波的生成仪器为用作厨具的光波炉或具有卤素灯管的加热仪器。
本发明所述制备方法的步骤(1)中,所述的光波退火的功率为100-900 W。
本发明所述制备方法的步骤(1)中,所述的光波退火的时间为5-120分钟。
本发明所述制备方法的步骤(1)中,所述的光波退火过程中的温度为100-300 ℃。
本发明的有益效果是:本发明工艺简单容易操作,原料廉价易得,所制备的铟铝氧透明半导体薄膜性能高,有望在晶体管、存储器、太阳能电池等器件中得到应用。通过本发明的工艺可以避免通常的高温溶液工艺、工艺周期长或昂贵设备等,成本低,适合工业化大规模生产。
附图说明
下面结合附图对本发明作进一步的说明。
附图1为实施例之一的铟铝氧透明半导体薄膜的扫描电镜图片。
具体实施方式
下面结合附图和具体实施例对本发明作进一步的说明。
实施例1:
称取0.022 g氯化铟,0.034 g硫酸铝,量取1毫升乙二醇甲醚溶液,配置浓度为0.1摩尔/升的铟铝氧前驱体溶液,经过3小时的磁力搅拌和超声分散形成澄清透明的铟铝氧前驱体溶液。将铟铝氧前驱体溶液涂覆到清洗好的衬底上形成铟铝氧前驱体薄膜,进行50 ℃的预热处理,然后经过300W、60分钟和200 ℃的光波退火,即得到铟铝氧透明半导体薄膜。
实施例2:
称取0.292 g乙酸铟,0.133 g氯化铝,量取5毫升乙醇溶液,配置浓度为0.2摩尔/升的铟铝氧前驱体溶液,经过0.1小时的磁力搅拌和超声分散形成澄清透明的铟铝氧前驱体溶液。将铟铝氧前驱体溶液涂覆到清洗好的衬底上形成铟铝氧前驱体薄膜,进行150 ℃的预热处理,然后经过700W、30分钟和280 ℃的光波退火,即得到铟铝氧透明半导体薄膜。
实施例3:
称取1.659 g氯化铟,1.53 g乙酸铝,量取15毫升水溶液,配置浓度为0.5摩尔/升的铟铝氧前驱体溶液,经过1小时的磁力搅拌和超声分散形成澄清透明的铟铝氧前驱体溶液。将铟铝氧前驱体溶液涂覆到清洗好的衬底上形成铟铝氧前驱体薄膜,进行90 ℃的预热处理,然后经过900W、5分钟和300 ℃的光波退火,即得到铟铝氧透明半导体薄膜。
实施例4:
称取0.3 g硝酸铟,0.2 g乙酸铝,量取20毫升乙二醇溶液,配置浓度为0.05摩尔/升的铟铝氧前驱体溶液,经过2小时的磁力搅拌和超声分散形成澄清透明的铟铝氧前驱体溶液。将铟铝氧前驱体溶液涂覆到清洗好的衬底上形成铟铝氧前驱体薄膜,进行120 ℃的预热处理,然后经过500W、20分钟和250 ℃的光波退火,即得到铟铝氧透明半导体薄膜。
实施例5:
称取1.46 g乙酸铟,0.665 g氯化铝,量取10毫升二甲基甲酰胺溶液,配置浓度为0.5摩尔/升的铟铝氧前驱体溶液,经过3小时的磁力搅拌和超声分散形成澄清透明的铟铝氧前驱体溶液。将铟铝氧前驱体溶液涂覆到清洗好的衬底上形成铟铝氧前驱体薄膜,进行70 ℃的预热处理,然后经过100W、120分钟和150 ℃的光波退火,即得到铟铝氧透明半导体薄膜。
上述实施例结合附图对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制。所属领域技术人员应该明白,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的对本发明的各种修改或变形,仍在本发明的保护范围以内。
Claims (8)
1.一种制备铟铝氧透明半导体薄膜的低温液相方法,其特征在于包括如下步骤:
(1) 制备铟铝氧前驱体溶液:称取可溶性的铟盐、铝盐,量取溶剂,配置浓度为0.01-0.5摩尔/升的铟铝氧前驱体溶液,经过0.1-3小时的磁力搅拌和超声分散形成澄清透明的铟铝氧前驱体溶液;
(2) 制备铟铝氧薄膜:将铟铝氧前驱体溶液涂覆到清洗好的衬底上形成铟铝氧前驱体薄膜,进行50-150 ℃的预热处理,然后经过一定功率、时间和温度的光波退火,根据铟铝氧薄膜的厚度要求可多次涂覆前驱体铟铝氧溶液并退火处理,即得到铟铝氧透明半导体薄膜;
所述的光波的生成仪器为用作厨具的光波炉或具有卤素灯管的加热仪器。
2.根据权利要求1所述的一种制备铟铝氧透明半导体薄膜的低温液相方法,其特征在于:所述的可溶性的铟盐为硝酸铟、氯化铟、硫酸铟或乙酸铟中的一种或两种以上。
3.根据权利要求1所述的一种制备铟铝氧透明半导体薄膜的低温液相方法,其特征在于:所述的可溶性的铝盐为硝酸铝、氯化铝、硫酸铝或乙酸铝中的一种或两种以上。
4.根据权利要求1所述的一种制备铟铝氧透明半导体薄膜的低温液相方法,其特征在于:所述的溶剂为乙二醇甲醚、乙醇、水、乙二醇或二甲基甲酰胺中的一种或两种以上。
5.根据权利要求1所述的一种制备铟铝氧透明半导体薄膜的低温液相方法,其特征在于:所述涂覆方法为旋转涂覆法、滴涂法、浸涂法、喷雾法或喷墨打印法。
6.根据权利要求1所述的一种制备铟铝氧透明半导体薄膜的低温液相方法,其特征在于:所述的光波退火的功率为100-900 W。
7.根据权利要求1所述的一种制备铟铝氧透明半导体薄膜的低温液相方法,其特征在于:所述的光波退火的时间为5-120分钟。
8.根据权利要求1所述的一种制备铟铝氧透明半导体薄膜的低温液相方法,其特征在于:所述的光波退火过程中的温度为100-300 ℃。
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US20130101867A1 (en) * | 2010-06-08 | 2013-04-25 | Sumitomo Metal Mining Co., Ltd. | Method of manufacturing metal oxide film, metal oxide film, element using the metal oxide film, substrate with metal oxide film, and device using the substrate with metal oxide film |
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