CN106252224A - 一种氧化镁介电薄膜的低温液相制备方法 - Google Patents
一种氧化镁介电薄膜的低温液相制备方法 Download PDFInfo
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 6
- 239000011777 magnesium Substances 0.000 claims abstract description 6
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- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
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- 235000011285 magnesium acetate Nutrition 0.000 claims description 3
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- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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- XSETZKVZGUWPFM-UHFFFAOYSA-N magnesium;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Mg+2].[Ti+4] XSETZKVZGUWPFM-UHFFFAOYSA-N 0.000 description 2
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- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- 229910019438 Mg(OC2H5)2 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 229910003068 Ti(C4H9O)4 Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000000280 densification Methods 0.000 description 1
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Abstract
本发明属于新材料及半导体领域，特别涉及一种氧化镁介电薄膜的低温液相制备方法。包括如下步骤：称取可溶性的镁盐，量取溶剂，配置浓度为0.01‑0.5摩尔/升的氧化镁前驱体溶液，经过0.1‑3小时的磁力搅拌和超声分散形成澄清透明的氧化镁前驱体溶液；制备氧化镁薄膜：将氧化镁前驱体溶液涂覆到清洗好的衬底上形成氧化镁前驱体薄膜，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，根据氧化镁薄膜的厚度要求可多次涂覆前驱体氧化镁溶液并退火处理，即得到氧化镁介电薄膜。本发明所得氧化镁薄膜介电性能高，在晶体管、电容器等微电子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，特别涉及一种氧化镁介电薄膜的低温液相制备方法，氧化镁薄膜在晶体管、电容器等微电子领域有重要应用前景。
背景技术
随着集成电路的飞速发展，作为硅基集成电路核心器件金属-氧化物-场效应晶体管(Metal-Oxide-Semiconductor Field Effect Transistor， MOSFET)的特征尺寸正以摩尔定律速度缩小。然而，当传统栅介质层氧化硅的厚度减小到原子尺寸时，由于量子隧穿效应的影响，氧化硅将失去介电性 能，以至将严重影响器件的稳定性和可靠性。因此需要寻找新型高介电常数(K)材料来替代氧化硅作栅介质，能够在保持和增大栅极电容的同时，使介质层仍保持足够的物理厚度来限制隧穿效应的影响。 氧化镁因为有着许多优异的性质，例如电绝缘性、化学惰性、机械稳定性、高温稳定性、热传导性和高效二次电子发射等，而广泛应用在如光学薄膜、以及高临界温 度的超导缓冲层、大面积平板、等离子显示器件、高K绝缘层介质材料等诸多领域。氧化镁因化学惰性，禁带宽度为7.8 eV，本征材料介电常数为9.8，被选作高K介质材料，可以用在MOSFET中取代氧化硅作为新的绝缘层介质。
目前制备氧化镁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氧化镁薄膜。然而，这些气相方法通常需要真空环境，增加了设备的复杂及成本的提高。近年来，液相方法日益引起了广泛的关注和迅速的发展，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镁薄膜的研究报道有许多。例如，公开号为CN105489486A的中国发明专利公开了一种基于超薄氧化镁高k介电层薄膜晶体管的制备方法：采用溶胶-凝胶法、UV光处理和热退火相结合的方式制备超薄氧化镁栅介电层。公开号为CN103489766A的中国发明专利公开了一种氧化镁钛高介电常数薄膜的制备方法：以乙二醇单甲醚为溶剂，浓盐酸为稳定剂，将Mg(OC2H5)2、Ti(C4H9O)4溶解其中，形成澄清稳定的前驱体溶液；将前驱体溶液旋转涂覆于玻璃基板上，经预热处理及后续高温热处理得到氧化镁钛薄膜。公开号为CN101274821B的发明专利公开了一种氧化镁薄膜的制备方法：在基板上涂布、并在干燥后烧成氧化镁微粒子分散液。公开号为CN100447305C的中国发明专利公开了一种溶胶－凝胶技术制备氧化镁防蚀保护薄膜的方法，以无机镁盐为出发原料，在常温常压下、运用成本较低的原料、简便可行的工艺条件，制备适用于不同易腐蚀金属基材的溶胶薄膜。虽然液相法可以制备较高性能的氧化镁薄膜，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，形成致密无针孔的氧化镁薄膜。因此，寻找一种新的低温液相技术制备技术，对于氧化镁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氧化镁介电薄膜的低温液相制备方法，实现氧化镁的简易高效制备，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高介电性能的氧化镁薄膜。
本发明的技术方案，具体包括以下步骤：
(1) 制备前驱体溶液：称取可溶性的镁盐，量取溶剂，配置浓度为0.01-0.5摩尔/升的氧化镁前驱体溶液，经过0.1-3小时的磁力搅拌和超声分散形成澄清透明的氧化镁前驱体溶液；
( 2) 制备氧化镁薄膜：将氧化镁前驱体溶液涂覆到清洗好的衬底上形成氧化镁前驱体薄膜，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，根据氧化镁薄膜的厚度要求可多次涂覆氧化镁前驱体溶液并退火处理，即得到氧化镁介电薄膜。
本发明所述制备方法的步骤(1)中，所述的可溶性的镁盐为硝酸镁、氯化镁、硫酸镁或乙酸镁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150-300 ℃。
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，所制备的氧化镁薄膜介电性能高，有望在晶体管、电容器等微电子器件中得到应用。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为实施例之一的氧化镁薄膜的电容-频率曲线；
附图2是实施例之一的氧化镁薄膜的漏电流密度-偏压曲线。
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1.28 g硝酸镁，量取10毫升乙醇溶液，配置浓度为0.5摩尔/升的氧化镁前驱体溶液，经过3小时的磁力搅拌和超声分散形成澄清透明的氧化镁前驱体溶液。将氧化镁前驱体溶液涂覆到清洗好的衬底上形成氧化镁前驱体薄膜，进行50 ℃的预热处理，然后经过900W、5分钟和300 ℃的光波退火，即得到氧化镁介电薄膜。
实施例2：
称取0.021 g乙酸镁，量取10毫升乙二醇甲醚溶液，配置浓度为0.01摩尔/升的氧化镁前驱体溶液，经过0.1小时的磁力搅拌和超声分散形成澄清透明的氧化镁前驱体溶液。将氧化镁前驱体溶液涂覆到清洗好的衬底上形成氧化镁前驱体薄膜，进行150 ℃的预热处理，然后经过100W、120分钟和150 ℃的光波退火，即得到氧化镁介电薄膜。
实施例3：
称取0.048 g氯化镁，量取5毫升水溶液，配置浓度为0.1摩尔/升的氧化镁前驱体溶液，经过1小时的磁力搅拌和超声分散形成澄清透明的氧化镁前驱体溶液。将氧化镁前驱体溶液涂覆到清洗好的衬底上形成氧化镁前驱体薄膜，进行90 ℃的预热处理，然后经过500W、20分钟和250 ℃的光波退火，即得到氧化镁介电薄膜。
实施例4：
称取0.26 g硝酸镁，量取20毫升乙二醇溶液，配置浓度为0.05摩尔/升的氧化镁前驱体溶液，经过2小时的磁力搅拌和超声分散形成澄清透明的氧化镁前驱体溶液。将氧化镁前驱体溶液涂覆到清洗好的衬底上形成氧化镁前驱体薄膜，进行120 ℃的预热处理，然后经过300W、60分钟和200 ℃的光波退火，即得到氧化镁介电薄膜。
实施例5：
称取0.9 g硫酸镁，量取15毫升二甲基甲酰胺溶液，配置浓度为0.5摩尔/升的氧化镁前驱体溶液，经过3小时的磁力搅拌和超声分散形成澄清透明的氧化镁前驱体溶液。将氧化镁前驱体溶液涂覆到清洗好的衬底上形成氧化镁前驱体薄膜，进行70 ℃的预热处理，然后经过700W、30分钟和280 ℃的光波退火，即得到氧化镁介电薄膜。
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 (7)
1.一种氧化镁介电薄膜的低温液相制备方法，其特征在于包括如下步骤：
(1) 制备氧化镁前驱体溶液：称取可溶性的镁盐，量取溶剂，配置浓度为0.01-0.5摩尔/升的氧化镁前驱体溶液，经过0.1-3小时的磁力搅拌和超声分散形成澄清透明的氧化镁前驱体溶液；
(2) 制备氧化镁薄膜：将氧化镁前驱体溶液涂覆到清洗好的衬底上形成氧化镁前驱体薄膜，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，根据氧化镁薄膜的厚度要求可多次涂覆前驱体氧化镁溶液并退火处理，即得到氧化镁介电薄膜；
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所述的一种氧化镁介电薄膜的低温液相制备方法，其特征在于：所述的可溶性的镁盐为硝酸镁、氯化镁、硫酸镁或乙酸镁中的一种或两种以上。
3.根据权利要求1所述的一种氧化镁介电薄膜的低温液相制备方法，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。
4.根据权利要求1所述的一种氧化镁介电薄膜的低温液相制备方法，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。
5.根据权利要求1所述的一种氧化镁介电薄膜的低温液相制备方法，其特征在于：所述的光波退火的功率为100-900 W。
6.根据权利要求1所述的一种氧化镁介电薄膜的低温液相制备方法，其特征在于：所述的光波退火的时间为5-120分钟。
7.根据权利要求1所述的一种氧化镁介电薄膜的低温液相制备方法，其特征在于：所述的光波退火过程中的温度为150-300 ℃。
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| US5361720A (en) * | 1988-04-22 | 1994-11-08 | British Technology Group Ltd. | Epitaxial deposition |
| CN1252779A (zh) * | 1997-04-14 | 2000-05-10 | 塞姆特里克斯公司 | 在用于等离子体显示面板的玻璃衬底上形成氧化镁膜的方法 |
| CN1900362A (zh) * | 2006-07-14 | 2007-01-24 | 西南大学 | 用溶胶－凝胶技术制备氧化镁防蚀保护薄膜的方法 |
| CN105489486A (zh) * | 2016-01-18 | 2016-04-13 | 青岛大学 | 一种基于超薄氧化镁高k介电层薄膜晶体管的制备方法 |
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| US5361720A (en) * | 1988-04-22 | 1994-11-08 | British Technology Group Ltd. | Epitaxial deposition |
| CN1252779A (zh) * | 1997-04-14 | 2000-05-10 | 塞姆特里克斯公司 | 在用于等离子体显示面板的玻璃衬底上形成氧化镁膜的方法 |
| CN1900362A (zh) * | 2006-07-14 | 2007-01-24 | 西南大学 | 用溶胶－凝胶技术制备氧化镁防蚀保护薄膜的方法 |
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