CN102375030A - A kind of method for making semiconductor thin film material - Google Patents
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- 239000010409 thin film Substances 0.000 title abstract description 9
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 29
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Abstract
本发明公开了一种制作半导体薄膜材料的方法，该方法是在声表面波气体传感器的制造过程中，在双延迟线型振荡器的一条延迟线上滴涂三乙醇胺与碳纳米管的混合溶液，并真空烘干而形成敏感膜的。本发明通过将研磨的碳纳米管加入三乙醇胺中配制聚合敏感膜，与纯的三乙醇胺传感器相比，三乙醇胺/碳纳米管传感器灵敏度、稳定性和检测质量都有很大的提高。
The invention discloses a method for manufacturing a semiconductor thin film material. The method is to drop-coat a mixed solution of triethanolamine and carbon nanotubes on one delay line of a double-delay line oscillator during the manufacturing process of a surface acoustic wave gas sensor , and vacuum drying to form a sensitive film. In the invention, the polymerized sensitive film is prepared by adding ground carbon nanotubes into triethanolamine. Compared with pure triethanolamine sensors, the sensitivity, stability and detection quality of the triethanolamine/carbon nanotube sensors are greatly improved.
Description
技术领域 technical field
本发明涉及声表面波气体传感器器件技术领域，特别涉及一种通过在三乙醇胺中掺杂研磨的碳纳米管制作半导体薄膜材料的方法。The invention relates to the technical field of surface acoustic wave gas sensor devices, in particular to a method for manufacturing semiconductor thin film materials by doping and grinding carbon nanotubes in triethanolamine.
背景技术 Background technique
从80年代开始，声表面波(SAW)气体传感器的研制工作逐渐兴起，目前可以检测H2S、NO2、SO2和H2等多种气体，运用声表面波技术研制成的传感器可以直接输出数字信号，因而具有得天独厚的优越性。Since the 1980s, the development of surface acoustic wave (SAW) gas sensors has gradually risen. At present, various gases such as H 2 S, NO 2 , SO 2 and H 2 can be detected. The sensor developed by using surface acoustic wave technology can directly Output digital signal, so it has unique advantages.
SAW气体传感器与其它种类的气体传感器相比有一些明显的优势，比如气体测量的灵敏度高、精度高、分辨率高、抗干扰能力强、有效检测范围大，而且SAW气体传感器可与逻辑器件结合在一起实现微型化、集成化和智能化。Compared with other types of gas sensors, SAW gas sensors have some obvious advantages, such as high sensitivity, high precision, high resolution, strong anti-interference ability, and large effective detection range of gas measurement, and SAW gas sensors can be combined with logic devices Miniaturization, integration and intelligence together.
在声表面波气体传感器中，除了延迟线之外，其最关键的部件就是气敏覆盖薄膜。SAW气体传感器在延迟线的SAW传播路径上覆盖一层选择性吸附薄膜，薄膜只对所需敏感的气体有吸附作用。薄膜对气体的吸附可导致振荡器频率的变化，由精确测量频率变化可测得气体浓度。因此要想制作出高灵敏度和质量的声表面波传感器器件，其中敏感膜的设计与制作部分特别的关键。In the surface acoustic wave gas sensor, in addition to the delay line, the most critical component is the gas-sensitive cover film. The SAW gas sensor is covered with a selective adsorption film on the SAW propagation path of the delay line, and the film only has the adsorption effect on the required sensitive gas. The adsorption of gas by the film can lead to a change in the frequency of the oscillator, and the gas concentration can be measured by accurately measuring the frequency change. Therefore, in order to manufacture high-sensitivity and high-quality surface acoustic wave sensor devices, the design and manufacture of the sensitive film are particularly critical.
但是，随着社会经济技术和人们生活水平的不断提高，人们对生活环境的污染越来越重视，工业生产和矿物质的燃烧往往产生大量的SO2、NO2等有毒有害的气体，我国居民区大气中SO2的最高允许浓度为0.5mg/m3，这就要求监测污染气体的传感器要有足够的灵敏度和选择性。However, with the continuous improvement of social economy technology and people's living standards, people pay more and more attention to the pollution of the living environment. Industrial production and mineral combustion often produce a large amount of toxic and harmful gases such as SO 2 and NO 2 . The maximum allowable concentration of SO 2 in the atmosphere of the region is 0.5mg/m 3 , which requires that the sensors for monitoring polluted gases have sufficient sensitivity and selectivity.
通过文献的调研我们知道现如今国内主要以三乙醇胺作为检测SO2气体传感器的敏感材料，虽然这些传感器在一定程度上可以检测SO2气体，但是三乙醇胺作为敏感材料制作的敏感膜非常的不稳定，这种不稳定的效果非常影响传感器的测量的选择性和灵敏度。Through literature research, we know that triethanolamine is mainly used as a sensitive material for detecting SO 2 gas sensors in China. Although these sensors can detect SO 2 gas to a certain extent, the sensitive film made of triethanolamine as a sensitive material is very unstable. , this destabilizing effect greatly affects the selectivity and sensitivity of the sensor's measurements.
所以能够制作出在常温下既稳定，又能够快速、灵敏的检测低浓度的气体传感器显得特别的重要，这也给膜的制作提出了更高的要求。Therefore, it is particularly important to be able to produce a gas sensor that is stable at room temperature and can quickly and sensitively detect low concentrations, which also puts forward higher requirements for the production of membranes.
发明内容 Contents of the invention
(一)要解决的技术问题(1) Technical problems to be solved
有鉴于此，本发明的主要目的在于提供一种通过在三乙醇胺中掺杂研磨的碳纳米管制作半导体薄膜材料的方法。In view of this, the main purpose of the present invention is to provide a method for manufacturing semiconductor thin film materials by doping ground carbon nanotubes in triethanolamine.
(二)技术方案(2) Technical solution
为达到上述目的，本发明提供了一种制作半导体薄膜材料的方法，该方法是在声表面波气体传感器的制造过程中，在双延迟线型振荡器的一条延迟线上滴涂三乙醇胺与碳纳米管的混合溶液，并真空烘干而形成敏感膜的。In order to achieve the above object, the present invention provides a method for making semiconductor thin film material, the method is in the manufacturing process of the surface acoustic wave gas sensor, drop-coating triethanolamine and carbon on a delay line of the double delay line oscillator The mixed solution of nanotubes is dried in vacuum to form a sensitive film.
上述方案中，所述在双延迟线型振荡器的一条延迟线上滴涂三乙醇胺与碳纳米管的混合溶液之前，进一步包括：配制三乙醇胺与碳纳米管的混合溶液。In the above scheme, before dripping the mixed solution of triethanolamine and carbon nanotubes on one delay line of the double delay line oscillator, it further includes: preparing the mixed solution of triethanolamine and carbon nanotubes.
上述方案中，所述配制三乙醇胺与碳纳米管的混合溶液，具体包括：研磨碳纳米管10至30分钟，将研磨好的10至200mg碳纳米管加入到50至100ml的三乙醇胺溶液中，并在常温下超声波振荡60分钟，形成三乙醇胺与碳纳米管的混合溶液。In the above scheme, the preparation of the mixed solution of triethanolamine and carbon nanotubes specifically includes: grinding the carbon nanotubes for 10 to 30 minutes, adding 10 to 200 mg of the ground carbon nanotubes to 50 to 100 ml of the triethanolamine solution, And ultrasonically oscillate for 60 minutes at normal temperature to form a mixed solution of triethanolamine and carbon nanotubes.
上述方案中，所述滴涂三乙醇胺与碳纳米管的混合溶液，是在双延迟线型振荡器的一条延迟线的敏感区域滴涂10至50μl的混合溶液。In the above scheme, the drop-coating of the mixed solution of triethanolamine and carbon nanotubes is to drop-coat 10 to 50 μl of the mixed solution on the sensitive area of one delay line of the double delay line oscillator.
上述方案中，所述真空烘干，是在真空环境下干燥至少2个小时。In the above scheme, the vacuum drying is drying in a vacuum environment for at least 2 hours.
(三)有益效果(3) Beneficial effects
本发明的有益效果在于：通过将研磨的碳纳米管加入三乙醇胺中配制聚合敏感膜，与纯的三乙醇胺传感器相比，三乙醇胺/碳纳米管传感器灵敏度、稳定性和检测质量都有很大的提高。The beneficial effects of the present invention are: by adding the ground carbon nanotubes into triethanolamine to prepare a polymerized sensitive film, compared with the pure triethanolamine sensor, the triethanolamine/carbon nanotube sensor has great sensitivity, stability and detection quality. improvement.
附图说明Description of drawings
图1为依照本发明制作半导体薄膜材料的工艺流程图；Fig. 1 is a process flow chart of making semiconductor thin film material according to the present invention;
其中，1为压电基体(压电单晶或薄膜)，2为叉指换能器IDT(Au或Pt)，3为传播路径上的金属薄膜(Au或Pt等)4化学敏感膜。Among them, 1 is the piezoelectric substrate (piezoelectric single crystal or thin film), 2 is the interdigital transducer IDT (Au or Pt), 3 is the metal film (Au or Pt, etc.) on the propagation path, and 4 is the chemically sensitive film.
具体实施方式 Detailed ways
为使本发明的目的、技术方案和优点更加清楚明白，以下结合具体实施例，并参照附图，对本发明进一步详细说明。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with specific embodiments and with reference to the accompanying drawings.
三乙醇胺在常温下对低浓度的SO2气体响应比较大，灵敏度较高。碳纳米管有着特殊的管状，网状结构，具有很大比表面积，稳定性非常高，将研磨的碳纳米管加入三乙醇胺中一起溶解，通过聚合制作出的敏感膜能够使得三乙醇胺更好的吸附气体，而且使得三乙醇胺的稳定性有很大的提高。Triethanolamine has a relatively large response to low-concentration SO 2 gas at room temperature and has a high sensitivity. Carbon nanotubes have a special tubular and network structure, have a large specific surface area, and are very stable. The ground carbon nanotubes are dissolved in triethanolamine, and the sensitive film produced by polymerization can make triethanolamine better. It absorbs gas and greatly improves the stability of triethanolamine.
本发明提供的制作半导体薄膜材料的方法，是在声表面波气体传感器的制造过程中，在双延迟线型振荡器的一条延迟线上滴涂三乙醇胺与碳纳米管的混合溶液，并真空烘干而形成敏感膜的。The method for making semiconductor thin film materials provided by the present invention is to drip-coat a mixed solution of triethanolamine and carbon nanotubes on a delay line of a double delay line oscillator during the manufacture of a surface acoustic wave gas sensor, and vacuum bake dry to form a sensitive film.
在双延迟线型振荡器的一条延迟线上滴涂三乙醇胺与碳纳米管的混合溶液之前，进一步包括：配制三乙醇胺与碳纳米管的混合溶液，具体包括：研磨碳纳米管10至30分钟，将研磨好的10至200mg碳纳米管加入到50至100ml的三乙醇胺溶液中，并在常温下超声波振荡60分钟，形成三乙醇胺与碳纳米管的混合溶液。Before drip-coating the mixed solution of triethanolamine and carbon nanotubes on a delay line of a double delay line oscillator, it further includes: preparing a mixed solution of triethanolamine and carbon nanotubes, specifically including: grinding carbon nanotubes for 10 to 30 minutes , adding 10 to 200 mg of ground carbon nanotubes into 50 to 100 ml of triethanolamine solution, and ultrasonically oscillating at room temperature for 60 minutes to form a mixed solution of triethanolamine and carbon nanotubes.
如图1所示，图1为依照本发明制作半导体薄膜材料的工艺流程图，具体包括以下步骤：As shown in Figure 1, Figure 1 is a process flow diagram for making semiconductor thin film materials according to the present invention, specifically comprising the following steps:
步骤1：在常温下制作三乙醇胺与碳纳米管的混合溶液；具体包括：研磨碳纳米管10至30分钟，将研磨好的10至200mg碳纳米管加入到50至100ml的三乙醇胺溶液中，形成三乙醇胺与碳纳米管的混合溶液；Step 1: Make a mixed solution of triethanolamine and carbon nanotubes at room temperature; specifically include: grinding carbon nanotubes for 10 to 30 minutes, adding 10 to 200 mg of carbon nanotubes that have been ground to 50 to 100 ml of triethanolamine solution, Form a mixed solution of triethanolamine and carbon nanotubes;
步骤2：采用超声振荡器在常温下对三乙醇胺与碳纳米管的混合溶液超声振荡1个小时；Step 2: Using an ultrasonic oscillator to ultrasonically oscillate the mixed solution of triethanolamine and carbon nanotubes at room temperature for 1 hour;
步骤3：在常温下用微量移液器在双延迟线型振荡器的一条延迟线的敏感区域滴涂大约10至50μl左右三乙醇胺与碳纳米管的混合溶液；Step 3: Use a micropipette to drop and apply about 10 to 50 μl of a mixed solution of triethanolamine and carbon nanotubes on the sensitive area of a delay line of a double delay line oscillator at room temperature;
步骤4：真空干燥：在60℃左右的真空干燥箱中干燥至少两个小时。Step 4: Vacuum drying: Dry in a vacuum oven at around 60°C for at least two hours.
以上所述的具体实施例，对本发明的目的、技术方案和有益效果进行了进一步详细说明，所应理解的是，以上所述仅为本发明的具体实施例而已，并不用于限制本发明，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The specific embodiments described above have further described the purpose, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above descriptions are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.
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Cited By (2)
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| CN109187737A (en) * | 2018-08-03 | 2019-01-11 | 郑州智谷工业技术有限公司 | A kind of carbon monoxide transducer and its density calculating method based on SAW device |
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Application publication date: 20120314 |