CN106094445A - Method for manufacturing nano-scale metal structure with large height-width ratio - Google Patents
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Abstract
本发明提供一种大高宽比纳米级金属结构的制作方法，所述方法包括：利用电子束蒸发金属材料，以在特定参数的单晶硅衬底上金属薄膜图案；将表面形成有金属薄膜图案的单晶硅衬底浸在混合液中进行催化腐蚀一段时间，以在单晶硅衬底上形成大高宽比的深硅槽；以深硅槽底部的金属薄膜为导电电镀种子层，将具有深硅槽的单晶硅衬底浸在电镀液中进行电镀，以增加金属薄膜的厚度至指定高度，以形成指定高宽比的金属结构；将形成有指定高宽比的金属结构的单晶硅衬底浸在混合液中进行各向同性湿法腐蚀一段时间，以去除所述金属结构之间的单晶硅。本发明的制作方法制作的纳米级金属结构的高宽比大。
The invention provides a method for manufacturing a nanoscale metal structure with a large aspect ratio. The method includes: using an electron beam to evaporate a metal material to form a metal thin film pattern on a single crystal silicon substrate with specific parameters; forming a metal thin film on the surface The patterned single crystal silicon substrate is immersed in the mixed solution for catalytic etching for a period of time to form a deep silicon groove with a large aspect ratio on the single crystal silicon substrate; the metal film at the bottom of the deep silicon groove is used as a conductive electroplating seed layer, and the A single crystal silicon substrate with a deep silicon groove is immersed in an electroplating solution for electroplating to increase the thickness of the metal film to a specified height to form a metal structure with a specified aspect ratio; a single metal structure with a specified aspect ratio will be formed The crystalline silicon substrate is immersed in the mixed solution for isotropic wet etching for a period of time to remove the single crystal silicon between the metal structures. The nanoscale metal structure produced by the production method of the invention has a large aspect ratio.
Description
技术领域technical field
本发明涉及纳米加工技术领域，尤其涉及一种大高宽比纳米级金属结构的制作方法。The invention relates to the technical field of nano-processing, in particular to a method for manufacturing a nanoscale metal structure with a large aspect ratio.
背景技术Background technique
对于高精度X射线波段的位相型衍射光学元件，为了获得所需要的位相，必须制作大高宽比纳米级金属结构。目前，在纳米加工技术中，主要是是利用多层胶工艺和干法刻蚀工艺来制作大高宽比纳米级金属结构，即利用比较厚的光刻胶作为掩模，通过干法刻蚀工艺来进行深硅刻蚀。For phase-type diffractive optical elements in the high-precision X-ray band, in order to obtain the required phase, it is necessary to fabricate a nanoscale metal structure with a large aspect ratio. At present, in nanofabrication technology, it is mainly to use multi-layer glue technology and dry etching technology to make nanoscale metal structures with large aspect ratio, that is, to use relatively thick photoresist as a mask, and dry etching process for deep silicon etch.
在实现本发明的过程中，发明人发现现有技术中至少存在如下技术问题：In the process of realizing the present invention, the inventor found that there are at least the following technical problems in the prior art:
由于光刻胶的各向同性刻蚀，其横向刻蚀精度很难控制，使得比较厚的光刻胶在显影时容易出现由于显影液张力引起的图形倒塌问题；同时后续干法刻蚀时所形成的金属结构也存在线宽陡直度差的问题。由于上述原因使得制作的纳米级金属结构的高宽比有限，即其高宽比很难大于10。Due to the isotropic etching of the photoresist, its lateral etching accuracy is difficult to control, so that relatively thick photoresists are prone to pattern collapse caused by the tension of the developer during development; at the same time, the subsequent dry etching The formed metal structure also has the problem of poor line width steepness. Due to the above reasons, the fabricated nanoscale metal structure has a limited aspect ratio, that is, its aspect ratio is hardly greater than 10.
发明内容Contents of the invention
为了解决上述技术问题，本发明提供一种大高宽比纳米级金属结构的制作方法，能够在避免光刻胶显影时出现的图形倒塌问题和干法刻蚀深度硅时出现的线宽陡直度差的问题，且其制作的纳米级金属结构的高宽比大。In order to solve the above technical problems, the present invention provides a method for fabricating a nanoscale metal structure with a large aspect ratio, which can avoid the problem of pattern collapse during photoresist development and the steep line width that occurs during dry etching of deep silicon. The problem of poor density, and the aspect ratio of the nanoscale metal structure produced by it is large.
本发明提供一种大高宽比纳米级金属结构的制作方法，包括：The invention provides a method for manufacturing a nanoscale metal structure with a large aspect ratio, comprising:
在特定参数的单晶硅衬底上旋涂光刻胶，并对所述光刻胶进行电子束曝光与显影，以在所述光刻胶中形成光栅掩模槽；Spin-coating a photoresist on a single crystal silicon substrate with specific parameters, and subjecting the photoresist to electron beam exposure and development to form grating mask grooves in the photoresist;
利用电子束蒸发金属材料，以在所述光栅掩模槽中形成金属薄膜；Evaporating a metal material with an electron beam to form a metal thin film in the groove of the grating mask;
去除所述单晶硅衬底上残留的光刻胶，以在所述单晶硅衬底表面形成金属薄膜图案；removing the remaining photoresist on the single crystal silicon substrate to form a metal thin film pattern on the surface of the single crystal silicon substrate;
以所述金属薄膜作为催化剂，将表面形成有金属薄膜图案的单晶硅衬底浸在由氢氟酸、双氧水和去离子水组成的混合液中进行催化腐蚀一段时间，以在所述单晶硅衬底上形成大高宽比的深硅槽，；Using the metal thin film as a catalyst, immerse the single crystal silicon substrate with the metal thin film pattern formed on the surface in a mixed solution composed of hydrofluoric acid, hydrogen peroxide and deionized water for a period of time to catalyze and corrode the single crystal silicon substrate. A deep silicon trench with a large aspect ratio is formed on the silicon substrate;
以所述深硅槽底部的所述金属薄膜为导电电镀种子层，将具有深硅槽的单晶硅衬底浸在电镀液中进行电镀，以增加所述金属薄膜的厚度至指定高度，以形成指定高宽比的金属结构；Using the metal thin film at the bottom of the deep silicon groove as a conductive electroplating seed layer, the single crystal silicon substrate with the deep silicon groove is immersed in an electroplating solution for electroplating, so as to increase the thickness of the metal thin film to a specified height, so as to Form a metal structure with a specified aspect ratio;
将形成有指定高宽比的金属结构的单晶硅衬底浸在由氢氟酸、硝酸和醋酸组成的混合液中进行各向同性湿法腐蚀一段时间，以去除所述金属结构之间的单晶硅；A single crystal silicon substrate formed with a metal structure with a specified aspect ratio is immersed in a mixed solution of hydrofluoric acid, nitric acid and acetic acid for isotropic wet etching for a period of time to remove the metal structure monocrystalline silicon;
所述特定参数包括单晶硅的晶向、掺杂类型和电阻率。The specific parameters include the crystallographic orientation, doping type and resistivity of the single crystal silicon.
本发明实施例提供的大高宽比纳米级金属结构的制作方法，与现有技术相比，其只需要将极薄的金属薄膜图案化就可以在单晶硅上形成大高宽比的金属结构，从而不存在光刻胶很厚时出现的由于显影液张力引起的图形倒塌问题和干法刻蚀深度硅时出现的线宽陡直度差的问题；而且应用本发明的制作方法制作的纳米级金属结构的高宽比大。Compared with the prior art, the method for fabricating a nanoscale metal structure with a large aspect ratio provided by the embodiment of the present invention only needs to pattern an extremely thin metal film to form a metal structure with a large aspect ratio on a single crystal silicon. structure, so that there is no problem of pattern collapse caused by the tension of the developer solution when the photoresist is very thick and the problem of poor line width steepness that occurs when the depth of silicon is dry etched; and the production method of the present invention is used to produce The aspect ratio of the nanoscale metal structure is large.
附图说明Description of drawings
图1为本发明大高宽比纳米级金属结构的制作方法的流程图；Fig. 1 is the flow chart of the manufacturing method of the nano-scale metal structure with large aspect ratio of the present invention;
图2为上述实施例中的所述金属薄膜图案的示意图。FIG. 2 is a schematic diagram of the metal thin film pattern in the above embodiment.
具体实施方式detailed description
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments It is only some embodiments of the present invention, but not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
如图1所示，本发明提供一种大高宽比纳米级金属结构的制作方法，所述方法包括：As shown in Figure 1, the present invention provides a method for fabricating a nanoscale metal structure with a large aspect ratio, the method comprising:
步骤1)在特定参数的单晶硅衬底上旋涂光刻胶，并对所述光刻胶进行电子束曝光与显影，以在所述光刻胶中形成光栅掩模槽。Step 1) Spin-coat photoresist on a single crystal silicon substrate with specific parameters, and perform electron beam exposure and development on the photoresist, so as to form grating mask grooves in the photoresist.
其中，所述特定参数包括单晶硅的晶向、掺杂类型和电阻率，具体地，所述单晶硅的晶向为<100>，所述单晶硅为P型掺杂，所述单晶硅的电阻率大于10cm。Wherein, the specific parameters include the crystal orientation, doping type and resistivity of the single crystal silicon, specifically, the crystal orientation of the single crystal silicon is <100>, the single crystal silicon is P-type doped, and the The resistivity of single crystal silicon is greater than 10 cm.
其中，所述光刻胶为PMMA光刻胶，所述PMMA光刻胶的厚度为200nm。Wherein, the photoresist is PMMA photoresist, and the thickness of the PMMA photoresist is 200nm.
步骤2)利用电子束蒸发金属材料，以在所述光栅掩模槽中形成金属薄膜。Step 2) Evaporating the metal material by using an electron beam to form a metal thin film in the groove of the grating mask.
其中，所述金属材料为金、铂金或者银，所述金属薄膜的厚度为10nm～50nm。Wherein, the metal material is gold, platinum or silver, and the thickness of the metal thin film is 10nm-50nm.
步骤3)去除所述单晶硅衬底上残留的光刻胶，以在所述单晶硅衬底表面形成金属薄膜图案。Step 3) removing the remaining photoresist on the single crystal silicon substrate to form a metal thin film pattern on the surface of the single crystal silicon substrate.
其中，所述金属薄膜图案的特征尺寸为10nm～3μm。Wherein, the characteristic size of the metal thin film pattern is 10 nm˜3 μm.
步骤4)以所述金属薄膜作为催化剂，将表面形成有金属薄膜图案的单晶硅衬底浸在由氢氟酸、双氧水和去离子水组成的混合液中进行催化腐蚀一段时间，以在所述单晶硅衬底上形成大高宽比的深硅槽。Step 4) using the metal thin film as a catalyst, immersing the single crystal silicon substrate with the metal thin film pattern formed on the surface in a mixed solution composed of hydrofluoric acid, hydrogen peroxide and deionized water for a period of time to catalyze corrosion on the A deep silicon groove with a large aspect ratio is formed on the single crystal silicon substrate.
其中，所述氢氟酸、双氧水和去离子水混合的摩尔比例为5.9：0.3：48。Wherein, the molar ratio of hydrofluoric acid, hydrogen peroxide and deionized water is 5.9:0.3:48.
步骤5)以所述深硅槽底部的所述金属薄膜为导电电镀种子层，将具有深硅槽的单晶硅衬底浸在电镀液中进行电镀，以增加所述金属薄膜的厚度至指定高度，以形成指定高宽比的金属结构。Step 5) using the metal thin film at the bottom of the deep silicon groove as a conductive electroplating seed layer, immersing the single crystal silicon substrate with the deep silicon groove in an electroplating solution for electroplating, so as to increase the thickness of the metal thin film to a specified height to form metal structures with a specified aspect ratio.
其中，所述氢氟酸、硝酸和醋酸混合的摩尔比例为23：4：1。Wherein, the molar ratio of hydrofluoric acid, nitric acid and acetic acid mixed is 23:4:1.
步骤6)将形成有指定高宽比的金属结构的单晶硅衬底浸在由氢氟酸、硝酸和醋酸组成的混合液中进行各向同性湿法腐蚀一段时间，以去除所述金属结构之间的单晶硅。Step 6) Dip the monocrystalline silicon substrate with a metal structure with a specified aspect ratio in a mixed solution of hydrofluoric acid, nitric acid and acetic acid for isotropic wet etching for a period of time to remove the metal structure between single crystal silicon.
本发明实施例提供的大高宽比纳米级金属结构的制作方法，与现有技术相比，其只需要将极薄的金属薄膜图案化就可以在单晶硅上形成大高宽比的金属结构，从而不存在光刻胶很厚时出现的由于显影液张力引起的图形倒塌问题和干法刻蚀深度硅时出现的线宽陡直度差的问题；而且应用本发明的制作方法制作的纳米级金属结构的高宽比大。Compared with the prior art, the method for fabricating a nanoscale metal structure with a large aspect ratio provided by the embodiment of the present invention only needs to pattern an extremely thin metal film to form a metal structure with a large aspect ratio on a single crystal silicon. structure, so that there is no problem of pattern collapse caused by the tension of the developer solution when the photoresist is very thick and the problem of poor line width steepness that occurs when the depth of silicon is dry etched; and the production method of the present invention is used to produce The aspect ratio of the nanoscale metal structure is large.
下面通过一个具体的例子对本发明做进一步详细说明。The present invention will be further described in detail through a specific example below.
步骤1)在单晶硅衬底上旋涂一层厚度为200nm的PMMA光刻胶，并对所述PMMA光刻胶进行电子束曝光与显影，以在所述PMMA光刻胶中形成光栅掩模槽。Step 1) Spin coating a layer of PMMA photoresist with a thickness of 200nm on the single crystal silicon substrate, and carry out electron beam exposure and development to the PMMA photoresist, to form a grating mask in the PMMA photoresist Die groove.
其中，所述单晶硅的晶向为<100>，所述单晶硅为P型掺杂，所述单晶硅的电阻率大于10cm。Wherein, the crystal orientation of the single crystal silicon is <100>, the single crystal silicon is P-type doped, and the resistivity of the single crystal silicon is greater than 10 cm.
步骤2)利用电子束蒸发金材料，以在所述光栅掩模槽中形成厚度为20nm金薄膜。Step 2) Evaporate the gold material by electron beam to form a gold film with a thickness of 20nm in the groove of the grating mask.
步骤3)去除所述单晶硅衬底上残留的PMMA光刻胶，以在所述单晶硅衬底表面形成金薄膜图案，如图2所示，所述金薄膜图案由周期排列的多个正方形组成。Step 3) remove the residual PMMA photoresist on the single crystal silicon substrate to form a gold thin film pattern on the surface of the single crystal silicon substrate, as shown in Figure 2, the gold thin film pattern consists of periodically arranged multiple composed of squares.
其中，所述金薄膜图案的特征尺寸为200nm，即每个正方形的边长为200nm。Wherein, the characteristic size of the gold thin film pattern is 200nm, that is, the side length of each square is 200nm.
步骤4)以所述金薄膜作为催化剂，将表面形成有属薄膜图案的单晶硅衬底浸在由氢氟酸、双氧水和去离子水组成的混合液中进行催化腐蚀10分钟，以在所述单晶硅衬底上形成高宽比为100:1的深硅槽。Step 4) Using the gold thin film as a catalyst, immerse the single crystal silicon substrate with the metal thin film pattern formed on the surface in a mixed solution composed of hydrofluoric acid, hydrogen peroxide and deionized water for 10 minutes to perform catalytic corrosion on the A deep silicon trench with an aspect ratio of 100:1 is formed on the single crystal silicon substrate.
其中，所述氢氟酸、双氧水和去离子水混合的摩尔比例为5.9：0.3：48。Wherein, the molar ratio of hydrofluoric acid, hydrogen peroxide and deionized water is 5.9:0.3:48.
步骤5)以所述深硅槽底部的所述金薄膜为导电电镀种子层，将具有深硅槽的单晶硅衬底浸在金电镀液中进行电镀，以增加所述金薄膜的厚度至指定高度，以形成高宽比为100:1的金结构。Step 5) using the gold thin film at the bottom of the deep silicon groove as a conductive electroplating seed layer, immersing the single crystal silicon substrate with the deep silicon groove in a gold electroplating solution for electroplating, so as to increase the thickness of the gold thin film to Specify the height to form gold structures with an aspect ratio of 100:1.
其中，所述氢氟酸、硝酸和醋酸混合的摩尔比例为23：4：1。Wherein, the molar ratio of hydrofluoric acid, nitric acid and acetic acid mixed is 23:4:1.
步骤6)将形成有高宽比为100:1的金结构的单晶硅衬底浸在由氢氟酸、硝酸和醋酸组成的混合液中进行各向同性湿法腐蚀3分钟，以去除所述金结构之间的单晶硅。Step 6) Dip the monocrystalline silicon substrate formed with a gold structure with an aspect ratio of 100:1 in a mixture of hydrofluoric acid, nitric acid and acetic acid for isotropic wet etching for 3 minutes to remove all Single crystal silicon between the gold structures.
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求的保护范围为准。The above is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Anyone skilled in the art can easily think of changes or substitutions within the technical scope disclosed in the present invention. All should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be determined by the protection scope of the claims.
Claims (7)
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| CN110286432A (en) * | 2019-06-25 | 2019-09-27 | 安徽工程大学 | Preparation method of X-ray gold transmission grating |
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