CN105070643B - A kind of preparation method of amorphous conductive carbon film - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 18
- 230000008020 evaporation Effects 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000007740 vapor deposition Methods 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 229910021417 amorphous silicon Inorganic materials 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000008021 deposition Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 33
- 229910003481 amorphous carbon Inorganic materials 0.000 description 13
- 239000002245 particle Substances 0.000 description 9
- 238000000089 atomic force micrograph Methods 0.000 description 5
- 238000012876 topography Methods 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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Abstract
Description
技术领域technical field
本发明属于微电子薄膜材料技术领域,具体涉及一种非晶导电碳膜的制备方法。The invention belongs to the technical field of microelectronic thin film materials, and in particular relates to a preparation method of an amorphous conductive carbon film.
背景技术Background technique
随着半导体工业的发展,缩小器件的尺寸成为了半导体工业继续推进的重点与难点,因此,进一步缩小器件尺寸的纳电子学就受到了科学界的广泛重视;碳材料作为纳电子器件的主流材料,其频率范围、电和散热等性能优异。With the development of the semiconductor industry, reducing the size of devices has become the focus and difficulty of the semiconductor industry. Therefore, nanoelectronics, which further reduces the size of devices, has received extensive attention from the scientific community; carbon materials are the mainstream materials for nanoelectronic devices. , and its frequency range, electrical and thermal properties are excellent.
目前,石墨烯、氧化石墨烯、碳纳米管是常见的碳材料;非晶碳薄膜是一种用于纳电子器件制备的新型碳材料,因其具有较好的物理、化学性能而备受关注;然而在实际生产中,非晶碳薄膜的制备存在工艺复杂、工艺参数不易控制,且制备过程中需要使用昂贵的仪器设备,生产成本高等问题。At present, graphene, graphene oxide, and carbon nanotubes are common carbon materials; amorphous carbon film is a new type of carbon material used in the preparation of nanoelectronic devices, and has attracted much attention because of its good physical and chemical properties. However, in actual production, the preparation of amorphous carbon thin films has complex processes, difficult control of process parameters, and the need to use expensive instruments and equipment in the preparation process, resulting in high production costs.
发明内容Contents of the invention
本发明的目的是提供一种非晶导电碳膜的制备方法,解决了现有非晶碳薄膜制备过程中工艺复杂、工艺参数不易控制,且需要使用昂贵的仪器设备、生产成本高的问题。The purpose of the present invention is to provide a method for preparing an amorphous carbon film, which solves the problems of complex process, difficult control of process parameters, expensive equipment and high production cost in the preparation process of the existing amorphous carbon film.
本发明所采用的技术方案是,一种非晶导电碳膜的制备方法,采用蒸镀仪进行制备,具体过程为:The technical scheme adopted in the present invention is, a kind of preparation method of amorphous conductive carbon film, adopts evaporation apparatus to prepare, and specific process is:
步骤1,在室温下,将碳绳固定在蒸发源上,随后将清洗后的基板放在基片托片上固定;Step 1, at room temperature, fix the carbon rope on the evaporation source, and then place the cleaned substrate on the substrate holder and fix it;
步骤2,打开蒸镀仪电源,调节蒸镀仪的电流至40~50A,进行蒸镀,碳绳断裂后,停止蒸镀,冷却后,即得非晶导电碳膜。Step 2, turn on the power of the vapor deposition apparatus, adjust the current of the vapor deposition apparatus to 40-50A, conduct vapor deposition, stop the vapor deposition after the carbon rope breaks, and obtain an amorphous conductive carbon film after cooling.
本发明的特征还在于,The present invention is also characterized in that,
步骤1中,碳绳由纯度99%、直径为2毫米的石墨纤维制成,碳绳长度为1厘米。In step 1, the carbon rope is made of graphite fibers with a purity of 99% and a diameter of 2 mm, and the length of the carbon rope is 1 cm.
步骤1中,基板为非晶硅基板、Pt导电基板或FTO导电基板中的一种。In step 1, the substrate is one of an amorphous silicon substrate, a Pt conductive substrate or an FTO conductive substrate.
步骤1中,基板的清洗过程为:将基板放入丙酮中超声清洗3~8min,随后放入无水乙醇中超声清洗3~8min,最后用去离子水冲洗2~3次。In step 1, the cleaning process of the substrate is as follows: put the substrate in acetone for ultrasonic cleaning for 3-8 minutes, then put it in absolute ethanol for ultrasonic cleaning for 3-8 minutes, and finally rinse it with deionized water for 2-3 times.
步骤2中,蒸镀环境为:在空气气氛条件下,真空度为1×10-2Pa;或Ar气氛条件下,真空度为5×10-2Pa;或N2气氛条件下,真空度为5×10-2Pa。In step 2, the evaporation environment is: under air atmosphere conditions, the vacuum degree is 1×10 -2 Pa; or under Ar atmosphere conditions, the vacuum degree is 5×10 -2 Pa; or under N 2 atmosphere conditions, the vacuum degree is is 5×10 -2 Pa.
本发明的有益效果是,利用蒸镀仪进行非晶导电碳膜的制备,不需要复杂、昂贵的设备,且制备工艺简便、工艺参数易于控制,能大大地降低生产成本;此外,本发明方法可在不同的基板以及不同的沉积气氛下制备出薄膜质量较好的非晶导电碳膜。The beneficial effects of the present invention are that the preparation of the amorphous conductive carbon film by using a vapor deposition apparatus does not require complex and expensive equipment, and the preparation process is simple, the process parameters are easy to control, and the production cost can be greatly reduced; in addition, the method of the present invention The amorphous conductive carbon film with better film quality can be prepared under different substrates and different deposition atmospheres.
附图说明Description of drawings
图1是实施例1制备得到的非晶导电碳膜的原子力显微镜微观形貌图;Fig. 1 is the atomic force microscope microscopic topography figure of the amorphous conductive carbon film that embodiment 1 prepares;
图2是实施例2制备得到的非晶导电碳膜的原子力显微镜微观形貌图;Fig. 2 is the atomic force microscope microscopic topography figure of the amorphous conductive carbon film that embodiment 2 prepares;
图3是实施例3制备得到的非晶导电碳膜的原子力显微镜微观形貌图;Fig. 3 is the atomic force microscope microscopic topography figure of the amorphous conductive carbon film that embodiment 3 prepares;
图4是实施例4制备得到的非晶导电碳膜的原子力显微镜微观形貌图;Fig. 4 is the atomic force microscope microscopic topography figure of the amorphous conductive carbon film that embodiment 4 prepares;
图5是实施例5制备得到的非晶导电碳膜的原子力显微镜微观形貌图。FIG. 5 is an atomic force microscope microscopic topography diagram of the amorphous conductive carbon film prepared in Example 5. FIG.
具体实施方式detailed description
下面结合附图和具体实施方式对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.
实施例1Example 1
步骤1,在室温下,将长度为1厘米的碳绳固定在蒸发源上,随后将清洗后的非晶硅基板放在基片托片上固定;其中,碳绳由纯度99%、直径为2毫米的石墨纤维制成;基板的清洗过程为:将基板放入丙酮中超声清洗3min,随后放入无水乙醇中超声清洗3min,最后用去离子水冲洗2次。Step 1, at room temperature, fix a carbon rope with a length of 1 cm on the evaporation source, and then place the cleaned amorphous silicon substrate on a substrate holder; wherein, the carbon rope is made of a purity of 99% and a diameter of 2 The cleaning process of the substrate is as follows: put the substrate in acetone for ultrasonic cleaning for 3 minutes, then put it in absolute ethanol for ultrasonic cleaning for 3 minutes, and finally rinse it twice with deionized water.
步骤2,打开蒸镀仪电源,调节蒸镀仪的电流至40A,在空气气氛条件下,真空度为1×10-2Pa的环境中进行蒸镀,碳绳断裂后,停止蒸镀,冷却后,即得厚度为220nm的非晶导电碳膜。Step 2, turn on the power of the vapor deposition apparatus, adjust the current of the vapor deposition apparatus to 40A, conduct vapor deposition in an environment with a vacuum of 1×10 -2 Pa under air atmosphere conditions, and stop vapor deposition after the carbon rope breaks, and cool down After that, an amorphous conductive carbon film with a thickness of 220 nm was obtained.
本实施例所得非晶导电碳膜原子力显微镜图像如图1所示,从图中可以看出所制备的非晶碳膜表面是由大量尺寸不同的微粒构成,表面平整,表面质量较高;微粒的尺寸约为在10nm,高度在5nm左右;经过软件的分析样品的表面均方根粗糙度(RMS)为0.380nm。The atomic force microscope image of the amorphous conductive carbon film obtained in this embodiment is shown in Figure 1. It can be seen from the figure that the prepared amorphous carbon film surface is composed of a large number of particles with different sizes, the surface is flat, and the surface quality is high; The size is about 10nm, and the height is about 5nm; the surface root mean square roughness (RMS) of the sample analyzed by the software is 0.380nm.
实施例2Example 2
步骤1,在室温下,将长度为1厘米的碳绳固定在蒸发源上,随后将清洗后的Pt导电基板放在基片托片上固定;其中,碳绳由纯度99%、直径为2毫米的石墨纤维制成;基板的清洗过程为:将基板放入丙酮中超声清洗5min,随后放入无水乙醇中超声清洗5min,最后用去离子水冲洗3次。Step 1, at room temperature, fix a carbon rope with a length of 1 cm on the evaporation source, and then place the cleaned Pt conductive substrate on the substrate holder and fix it; wherein, the carbon rope has a purity of 99% and a diameter of 2 mm Made of graphite fibers; the cleaning process of the substrate is as follows: put the substrate in acetone for 5 minutes for ultrasonic cleaning, then put it in absolute ethanol for 5 minutes, and finally rinse it with deionized water for 3 times.
步骤2,打开蒸镀仪电源,调节蒸镀仪的电流至40A,在空气气氛条件下,真空度为1×10-2Pa的环境中进行蒸镀,碳绳断裂后,停止蒸镀,冷却后,即得厚度为200nm的非晶导电碳膜。Step 2, turn on the power of the vapor deposition apparatus, adjust the current of the vapor deposition apparatus to 40A, conduct vapor deposition in an environment with a vacuum of 1×10 -2 Pa under air atmosphere conditions, and stop vapor deposition after the carbon rope breaks, and cool down After that, an amorphous conductive carbon film with a thickness of 200 nm was obtained.
本实施例所得非晶导电碳膜原子力显微镜图像如图2所示,从图中可以看出,所制备的非晶碳膜表面是由大量尺寸不同的微粒构成,表面平整,表面质量较高。微粒的尺寸在100nm之间,高度在10nm左右;非晶碳膜样品的表面均方根粗糙度(RMS)为1.645nm。The atomic force microscope image of the amorphous conductive carbon film obtained in this example is shown in Figure 2. It can be seen from the figure that the surface of the prepared amorphous carbon film is composed of a large number of particles of different sizes, and the surface is smooth and of high surface quality. The particle size is between 100nm and the height is about 10nm; the surface root mean square roughness (RMS) of the amorphous carbon film sample is 1.645nm.
实施例3Example 3
步骤1,在室温下,将长度为1厘米的碳绳固定在蒸发源上,随后将清洗后的FTO导电基板放在基片托片上固定;其中,碳绳由纯度99%、直径为2毫米的石墨纤维制成;基板的清洗过程为:将FTO导电基板放入丙酮中超声清洗8min,随后放入无水乙醇中超声清洗8min,最后用去离子水冲洗3次。Step 1, at room temperature, fix a carbon rope with a length of 1 cm on the evaporation source, and then place the cleaned FTO conductive substrate on the substrate holder and fix it; wherein, the carbon rope has a purity of 99% and a diameter of 2 mm Made of graphite fibers; the cleaning process of the substrate is as follows: put the FTO conductive substrate in acetone for 8 minutes, then put it in absolute ethanol for 8 minutes, and finally rinse it with deionized water for 3 times.
步骤2,打开蒸镀仪电源,调节蒸镀仪的电流至50A,在空气气氛条件下,真空度为1×10-2Pa的环境中进行蒸镀,碳绳断裂后,停止蒸镀,冷却后,即得厚度为210nm的非晶导电碳膜。Step 2, turn on the power of the vapor deposition apparatus, adjust the current of the vapor deposition apparatus to 50A, conduct vapor deposition in an environment with a vacuum of 1×10 -2 Pa under air atmosphere conditions, and stop the vapor deposition after the carbon rope breaks, and cool down After that, an amorphous conductive carbon film with a thickness of 210 nm was obtained.
本实施例所得非晶导电碳膜原子力显微镜图像如图3所示,从图中可以看出,所制备的非晶碳膜表面是由大量尺寸不同的微粒构成,表面平整,表面质量较高。微粒的尺寸在200nm之间,高度在60nm左右。非晶碳膜样品的表面均方根粗糙度(RMS)为2.213nm。The atomic force microscope image of the amorphous conductive carbon film obtained in this example is shown in Figure 3. It can be seen from the figure that the surface of the prepared amorphous carbon film is composed of a large number of particles of different sizes, the surface is smooth, and the surface quality is high. The particle size is between 200nm and the height is around 60nm. The surface root mean square roughness (RMS) of the amorphous carbon film sample is 2.213nm.
实施例4Example 4
步骤1,在室温下,将长度为1厘米的碳绳固定在蒸发源上,随后将清洗后的非晶硅基板放在基片托片上固定;其中,碳绳由纯度99%、直径为2毫米的石墨纤维制成;基板的清洗过程为:将非晶硅基板放入丙酮中超声清洗5min,随后放入无水乙醇中超声清洗5min,最后用去离子水冲洗3次。Step 1, at room temperature, fix a carbon rope with a length of 1 cm on the evaporation source, and then place the cleaned amorphous silicon substrate on a substrate holder; wherein, the carbon rope is made of a purity of 99% and a diameter of 2 The cleaning process of the substrate is as follows: put the amorphous silicon substrate in acetone for 5 minutes for ultrasonic cleaning, then put it in absolute ethanol for 5 minutes, and finally rinse it with deionized water for 3 times.
步骤2,打开蒸镀仪电源,调节蒸镀仪的电流至50A,Ar气氛条件下,真空度为5×10-2Pa环境中进行蒸镀,碳绳断裂后,停止蒸镀,冷却后,即得厚度为190nm的非晶导电碳膜。Step 2, turn on the power supply of the vapor deposition apparatus, adjust the current of the vapor deposition apparatus to 50A, conduct vapor deposition in an environment with an Ar atmosphere and a vacuum of 5×10 -2 Pa, stop the vapor deposition after the carbon rope is broken, and cool down, That is, an amorphous conductive carbon film with a thickness of 190 nm was obtained.
本实施例所得非晶导电碳膜原子力显微镜图像如图4所示,从图中可以看出,所制备的非晶碳膜表面是由大量尺寸不同的微粒构成,表面平整,表面质量较高。微粒的尺寸在100nm,高度在10nm左右。非晶碳膜样品的表面均方根粗糙度(RMS)为1.706nm。The atomic force microscope image of the amorphous conductive carbon film obtained in this example is shown in Figure 4. It can be seen from the figure that the surface of the prepared amorphous carbon film is composed of a large number of particles of different sizes, and the surface is smooth and of high surface quality. The particle size is 100nm and the height is about 10nm. The surface root mean square roughness (RMS) of the amorphous carbon film sample is 1.706nm.
实施例5Example 5
步骤1,在室温下,将长度为1厘米的碳绳固定在蒸发源上,随后将清洗后的非晶硅基板放在基片托片上固定;其中,碳绳由纯度99%、直径为2毫米的石墨纤维制成;基板的清洗过程为:将基板放入丙酮中超声清洗4min,随后放入无水乙醇中超声清洗4min,最后用去离子水冲洗2次。Step 1, at room temperature, fix a carbon rope with a length of 1 cm on the evaporation source, and then place the cleaned amorphous silicon substrate on a substrate holder; wherein, the carbon rope is made of a purity of 99% and a diameter of 2 The cleaning process of the substrate is as follows: put the substrate into acetone for ultrasonic cleaning for 4 minutes, then put it into absolute ethanol for ultrasonic cleaning for 4 minutes, and finally rinse it twice with deionized water.
步骤2,打开蒸镀仪电源,调节蒸镀仪的电流至40A,在N2气氛条件下,真空度为5×10-2Pa环境中进行蒸镀,碳绳断裂后,停止蒸镀,冷却后,即得厚度为200nm的非晶导电碳膜。Step 2, turn on the power of the vapor deposition apparatus, adjust the current of the vapor deposition apparatus to 40A, conduct vapor deposition in an environment with a vacuum degree of 5×10 -2 Pa under the condition of N2 atmosphere, stop the vapor deposition after the carbon rope breaks, and cool down After that, an amorphous conductive carbon film with a thickness of 200 nm was obtained.
本实施例所得非晶导电碳膜原子力显微镜图像如图5所示,从图中可以看出,所制备的非晶碳膜表面是由大量尺寸不同的微粒构成,表面平整,表面质量较高。微粒的尺寸在100nm左右,高度在50nm左右。非晶碳膜样品的表面均方根粗糙度(RMS)为1.843nm。The atomic force microscope image of the amorphous conductive carbon film obtained in this example is shown in Figure 5. It can be seen from the figure that the surface of the prepared amorphous carbon film is composed of a large number of particles of different sizes, and the surface is smooth and of high surface quality. The particle size is about 100nm and the height is about 50nm. The surface root mean square roughness (RMS) of the amorphous carbon film sample is 1.843nm.
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