CN102820867A - Method for producing titanium dioxide doped copper phthalocyanine sensitive membrane of acoustic surface wave sensor - Google Patents

Method for producing titanium dioxide doped copper phthalocyanine sensitive membrane of acoustic surface wave sensor Download PDF

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CN102820867A
CN102820867A CN201110155259XA CN201110155259A CN102820867A CN 102820867 A CN102820867 A CN 102820867A CN 201110155259X A CN201110155259X A CN 201110155259XA CN 201110155259 A CN201110155259 A CN 201110155259A CN 102820867 A CN102820867 A CN 102820867A
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cupc
tio2
sensitive
doped
copper phthalocyanine
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李冬梅
汪幸
刘明
周文
侯成诚
闫学锋
谢常青
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中国科学院微电子研究所
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Abstract

The invention discloses a method for producing a titanium dioxide (TiO2) doped copper phthalocyanine (CuPc) sensitive membrane of an acoustic surface wave sensor. The method includes that TiO2 doped CuPc is used as a sensitive material and subjected to mixing and pressing to form a TiO2 and CuPc mixed material, and the TiO2 and CuPc mixed material is subjected to evaporation by electron beams and then photoresist stripping to form the TiO2 doped CuPc sensitive membrane. According to the method for producing the TiO2 doped CuPc sensitive membrane of the acoustic surface wave sensor, TiO2 is added into CuPc to produce the polymerized sensitive membrane, so that the possibility that a phthalocyanine material is used for detecting a nitrogen dioxide (NO2) gas at a normal temperature is achieved, and compared with sensors with pure CuPc sensitive membranes, the sensor with the TiO2 doped CuPc sensitive membrane is greatly improved in selectivity, sensitivity and detection qualities when the lower-concentration NO2 gas is detected.

Description

一种制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法 A method of making a surface acoustic wave sensor method doped titanium oxide film of copper phthalocyanine sensitive

技术领域 FIELD

[0001] 本发明涉及声表面波气体传感器技术领域,特别涉及一种通过电子束蒸发二氧化钛(TiO2)与酞菁铜(CuPc)混合材料制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法。 [0001] The present invention relates to a surface acoustic wave gas sensor technology, and particularly, to a by electron beam evaporation of titanium dioxide (TiO2) and copper phthalocyanine (CuPc) mixing SAW sensor material doped titanium dioxide film of copper phthalocyanine sensitive .

背景技术 Background technique

[0002] 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, NH3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。 [0002] Since the 1980s, a surface acoustic wave (SAW) gas sensor development work gradually on the rise, the current can be detected H2S, NO2, SO2, NH3 and other gases, using technology developed into a surface acoustic wave sensor may be directly output digital signal, which has unique advantages. SAW气体传感器与其他类型的传感器相比有很多优良的特性,具有体积小、重量轻、精度高、分辨率高、抗干扰能力强、灵敏度高、有效检测范围线性好等众多特点。 Compared with SAW gas sensors have many other types of sensors excellent properties, a small size, light weight, high precision, high resolution, anti-interference ability, high sensitivity, good linearity effective detection range and other characteristics.

[0003] SAff气体传感器的基本工作原理是通过SAW气体传感器表面所覆盖的敏感膜对待侧气体的吸附引起SAW传感器电导率和质量的变化,从而引起SAW振荡器的振荡频率的改变,以此来实现对气体的监控和测量。 [0003] The basic operating principle of the gas sensor SAff side gas adsorption treatment by SAW gas sensors sensitive membrane covered surface causes a change in the electrical conductivity and quality of the SAW sensor so as to cause a change in the oscillation frequency of the SAW oscillator, in order to achieve the monitoring and measurement of gases. 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。 Therefore, in order to produce high-quality and sensitivity of the surface acoustic wave sensor device, wherein the design and production of a particular critical portion of the sensitive film.

[0004] 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S02、NO2等有毒有害的气体,现场实时监测的大气污染物的体积分数往往低至10_6甚至10_9的水平,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。 [0004] As technology continues to improve the socio-economic and people's living standards, people living on the pollution of the environment more and more attention, industrial production and combustion of mineral often produce large amounts of S02, NO2 and other toxic gases, on-site real-time monitoring volume fraction of air pollutants often even low levels 10_6 10_9, which requires the sensor to monitor pollutant gases have sufficient sensitivity and selectivity.

[0005] 在声表面波传感器领域酞菁材料主要的用于检测NO2,单独的CuPc作为敏感薄膜材料制作出的SAW器件选择性低,工作温度高,适用价值不高。 [0005] Phthalocyanine material SAW sensor for detecting the main areas NO2, produce low single CuPc film material as the SAW device is selectively sensitive, high operating temperatures, practical value is not high. 选择特性和高温不仅影响传感器测量的稳定效果,而且会带来额外的功率损耗等问题,所以能够制作出在常温下快速,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。 Selection characteristics and affects not only the temperature measured by the sensor stabilizing effect, but causes additional problems such as power loss, it is possible to produce a rapid, sensitive detection of low concentrations of the gas sensor is particularly important at room temperature, to which the film production put forward higher requirements.

[0006] 因为CuPc作为几种常见的检测NO2气体传感器中的敏感膜材料,在高温下对低浓度的NO2气体响应比较大,灵敏度较高。 [0006] For the detection of several common as CuPc NO2 gas sensor sensitive film material at a high temperature gas of low concentration of NO2 in response to relatively large, high sensitivity. TiO2是一种弱η型金属氧化物半导体,作为气敏传感器有着更高的反应灵敏度、以及更快的响应时间,已有比较广泛的应用。 TiO2 is a weak η-type metal oxide semiconductor, as the reaction gas sensor has a higher sensitivity and faster response time, has been widely used. 将CuPc掺杂TiO2通过聚合制作出的敏感膜能够使得纯的CuPc对NO2气体有着更大的响应,以期望在常温下做到对低浓度NO2气体进行高质量、灵敏和精确的检测。 The CuPc doped TiO2 prepared by polymerizing a sensitive membrane such that pure CuPc can have a greater response to NO2 gas, to achieve a desired low concentration of NO2 at room temperature for high-quality, sensitive and accurate detection.

发明内容 SUMMARY

[0007]( 一)要解决的技术问题 [0007] (a) To solve technical problems

[0008] 有鉴于此,本发明的主要目的在于提供一种制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法,以实现在常温下对低浓度NO2气体进行高质量、灵敏和精确的检测。 [0008] In view of this, the main object of the present invention is to provide a method for fabricating a surface acoustic wave sensor titania-doped copper phthalocyanine sensitive film, in order to achieve high-quality low-concentration NO2 gas at normal temperature, sensitivity and precision detection.

[0009] ( 二)技术方案 [0009] (ii) Technical Solution

[0010] 为达到上述目的,本发明提供了一种制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法,该方法是由TiO2掺杂CuPc作为敏感材料,通过混合和压制形成TiO2与CuPc混合材料,电子束蒸发该TiO2与CuPc混合材料,并剥离光刻胶形成二氧化钛掺杂酞菁铜敏感膜。 [0010] To achieve the above object, the present invention provides a method of making a surface acoustic wave sensor titania-doped copper phthalocyanine sensitive film, which is doped TiO2 as CuPc sensitive material is formed by mixing TiO2 and pressing the CuPc mixed material, the electron beam evaporation CuPc mixed with TiO2 material, and forming a titanium dioxide sensitive stripping the photoresist film is doped copper phthalocyanine.

[0011] 上述方案中,所述通过混合和压制形成TiO2与CuPc混合材料,包括:将质量比I : I的TiO2与CuPc在常温下进行混合,制作TiO2与CuPc混合材料;以及用机器将TiO2与CuPc混合材料压制成型。 [0011] In the above embodiment, the TiO2 formed by mixing and pressing with CuPc hybrid material, comprising: a mass ratio of I: I CuPc is mixed with the TiO2 at ordinary temperature, production of TiO2 with mixing CuPc material; and by machine TiO2 and press molding the mixed material CuPc.

[0012] 上述方案中,所述电子束蒸发该TiO2与CuPc混合材料,并剥离光刻胶形成二氧化钛掺杂酞菁铜敏感膜,包括:在基片上涂光刻胶;在光刻胶上电子束蒸发压制好的TiO2与CuPc混合材料,将块状TiO2与CuPc混合材料当作电子束蒸发的祀材进行蒸发;以及将基片泡在化学试剂中使得光刻胶溶解,从而剥离光刻胶,形成二氧化钛掺杂酞菁铜敏感膜。 [0012] In the above embodiment, the electron beam evaporation CuPc mixed with the TiO2 material, and stripping the photoresist is formed of copper phthalocyanine-doped titanium oxide sensitive film, comprising: coating a photoresist on a substrate; electrons on the resist TiO2 and good press beam evaporation CuPc mixed material, the bulk material mixing CuPc and TiO2 as electron beam evaporation sacrificial material is evaporated; and the substrate is soaked in a chemical agent such that the photoresist is dissolved, thereby stripping the photoresist , forming a titanium dioxide sensitive film is doped copper phthalocyanine.

[0013](三)有益效果[0014] 本发明提供的这种制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法,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通过电子束蒸发TiO2与CuPc的混合材料制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜。 Method [0013] (c) Advantageous Effects [0014] The present invention provides such a surface acoustic wave sensor made of copper phthalocyanine-doped titanium oxide sensitive film, the manufacturing process is a surface acoustic wave gas sensor, in dual delay line type on a delay line oscillator by electron beam evaporation and TiO2 mixed CuPc material SAW sensor titania-doped copper phthalocyanine sensitive membrane. 本发明通过将TiO2加入CuPc中制作聚合敏感膜,使得常温下使用酞菁材料去检测NO2气体变为可能,而且具有该二氧化钛掺杂酞菁铜敏感膜的传感器与单纯CuPc敏感膜的传感器相比,检测低浓度NO2气体时在选择性、灵敏度和检测质量均有大幅的提高。 TiO2 added to the present invention by the polymerization prepared CuPc sensitive film, so that normal use of the phthalocyanine material and NO2 becomes possible to detect, with a sensor and the copper phthalocyanine-doped titanium oxide film sensor sensitive and simple as compared to the sensitive film CuPc , selective, have significantly improved sensitivity and detection by mass detect low concentrations of NO2 gas.

附图说明 BRIEF DESCRIPTION

[0015] 图I为本发明制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法流程图; [0015] Figure I of the present production method of the surface acoustic wave sensor titania-doped copper phthalocyanine sensitive film flowchart invention;

[0016]图2为本发明制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的工艺流程图; [0016] FIG surface acoustic wave sensor 2 made of copper phthalocyanine-doped titanium oxide film sensitive to the process flow diagram of the present invention;

[0017] 图2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为光刻胶,5为敏感膜。 In [0017] FIG. 2: 1 is a piezoelectric substrate (piezoelectric single crystal or thin film), 2 to the IDT interdigital transducer (Au or Pt),. 3 is a metal film (Au or Pt, etc.) on the propagation path, 4 is a photoresist film 5 as a sensitive.

具体实施方式 Detailed ways

[0018] 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。 [0018] To make the objectives, technical solutions, and advantages of the present invention will become more apparent hereinafter in conjunction with specific embodiments, and with reference to the accompanying drawings, the present invention is described in further detail.

[0019] 本发明提供的这种制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法,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通过电子束蒸发TiO2与CuPc的混合材料制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜。 Method [0019] The present invention provides such a surface acoustic wave sensor made of copper phthalocyanine-doped titanium oxide sensitive film, the manufacturing process is a surface acoustic wave gas sensor, a delay in the delay line oscillator by double TiO2 electron-beam evaporation and mixing of CuPc material SAW sensor titania-doped copper phthalocyanine sensitive membrane. 该二氧化钛掺杂酞菁铜敏感膜是由Ti02掺杂CuPc作为敏感材料,并通过混合、压制、电子束蒸发和剥离光刻胶而形成。 The titania-doped copper phthalocyanine sensitive film is made of Ti02 doped CuPc as sensitive material, and by mixing, pressing, electron beam evaporation and stripping the photoresist is formed.

[0020] 如图I所示,图I为本发明制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法流程图。 [0020] FIG. I shown in FIG. I SAW sensor-based method of making titania-doped copper phthalocyanine sensitive film flowchart invention. 该方法是由TiO2掺杂CuPc作为敏感材料,通过混合和压制形成TiO2与CuPc混合材料,电子束蒸发该TiO2与CuPc混合材料,并剥离光刻胶形成二氧化钛掺杂酞菁铜敏感膜。 This method is sensitive material as TiO2 doped CuPc, formed by mixing CuPc and pressing a mixed material of TiO2, TiO2 electron-beam evaporation of the CuPc and the mixed material, and forming a titanium dioxide sensitive stripping the photoresist film is doped copper phthalocyanine. .

[0021] 本发明制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的具体工艺如图2所示,包括: [0021] Production acoustic wave sensor of the present invention, copper phthalocyanine-doped titanium oxide film is particularly sensitive to the process shown in Figure 2, comprising:

[0022] 步骤I :将I克左右质量比I : I的TiO2与CuPc在常温下进行混合,制作TiO2与CuPc的混合材料; [0022] Step I: The mass ratio of about I g I: I CuPc is mixed with the TiO2 at room temperature to prepare a mixed material of CuPc and TiO2;

[0023] 步骤2 :用机器将TiO2与CuPc的混合材料压制成型; [0023] Step 2: The TiO2 CuPc and the mixed material by press molding machine;

[0024] 步骤3 :在基片上涂光刻胶; [0024] Step 3: coating a photoresist on a substrate;

[0025] 步骤4 :在光刻胶上电子束蒸发压制好的TiO2与CuPc混合材料,将块状TiO2与CuPc混合材料当作电子束蒸发的靶材进行蒸发。 [0025] Step 4: e-beam evaporated over the photoresist with press TiO2 good mixing CuPc material, CuPc the bulk mixed material and TiO2 as electron beam evaporation target evaporated.

[0026] 步骤5 :将基片泡在化学试剂中使得光刻胶溶解,从而剥离光刻胶,形成二氧化钛掺杂酞菁铜敏感膜。 [0026] Step 5: The substrate is soaked in a chemical agent such that the photoresist is dissolved, thereby stripping the photoresist, forming a titanium dioxide sensitive film is doped copper phthalocyanine.

[0027] 本发明是在双延迟线型振荡器的一条延迟线上通过电子束蒸发TiO2与CuPc的混合材料,并剥离光刻胶而形成二氧化钛掺杂酞菁铜敏感膜,作为制作检测NO2气体的声表面波气体传感器敏感膜。 [0027] The present invention is a delay in the delay line oscillator bis evaporation material mixed with TiO2 CuPc by an electron beam, and the photoresist stripped to form a copper phthalocyanine-doped titanium oxide film is sensitive, detecting as a producer and NO2 the surface acoustic wave gas sensor sensitive membrane. [0028] 实施例 [0028] Example

[0029] 一种制作声表面波传感器二氧化钛掺杂酞菁铜敏感膜的方法,该方法包括:将I克左右质量比I : I的TiO2与CuPc在常温下进行混合,制作TiO2与CuPc的混合材料,然后用机器将TiO2与CuPc的混合材料压制成型,将压制成型的混合材料经过电子束蒸发沉积大约50nm至200nm左右的薄膜,再在丙酮或乙醇溶液剥离光刻胶,常温下真空烘干后即可形成二氧化钛掺杂酞菁铜敏感膜。 [0029] A surface acoustic wave sensor making titania-doped copper phthalocyanine sensitive film, the method comprising: a mass ratio of about I g I: I CuPc is mixed with the TiO2 at ordinary temperature, production of TiO2 with mixing of CuPc film material, then the machine with the TiO2 mixed material CuPc press molding, press molding the mixed material through electron beam evaporation deposition of about 50nm to about 200nm, and then in stripping the photoresist solution of acetone or ethanol, vacuum dried at room temperature after the titania-doped copper phthalocyanine sensitive film can be formed.

[0030] 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。 Specific Example [0030] above, the objectives, technical solutions, and beneficial effects of the present invention will be further described in detail, it should be understood that the above descriptions are merely embodiments of the present invention, but not intended to limit the present invention, within the spirit and principle of the present invention, any modifications, equivalent replacements, improvements, etc., should be included within the scope of the present invention.

Claims (3)

1. ー种制作声表面波传感器ニ氧化钛掺杂酞菁铜敏感膜的方法,其特征在于,该方法是由TiO2掺杂CuPc作为敏感材料,通过混合和压制形成TiO2与CuPc混合材料,电子束蒸发该TiO2与CuPc混合材料,并剥离光刻胶形成ニ氧化钛掺杂酞菁铜敏感膜。 A method of fabricating a surface acoustic wave sensor ー ni sensitive copper phthalocyanine-doped titanium oxide film, characterized in that the method is sensitive material as CuPc doped TiO2, TiO2 CuPc and the mixed material formed by mixing and pressing, electronic the CuPc beam evaporation and TiO2 mixed material, and stripping the photoresist sensitive film is formed a copper phthalocyanine-doped Ni oxide.
2.根据权利要求I所述的制作声表面波传感器ニ氧化钛掺杂酞菁铜敏感膜的方法,其特征在于,所述通过混合和压制形成TiO2与CuPc混合材料,包括: 将质量比I : I的TiO2与CuPc在常温下进行混合,制作TiO2与CuPc混合材料;以及用机器将TiO2与CuPc混合材料压制成型。 2. The method of claim I SAW sensor making titania-doped Ni-sensitive film of copper phthalocyanine as claimed in claim, wherein said TiO2 is formed with a mixed material obtained by mixing CuPc and pressing, comprising: a mass ratio of I : I CuPc of TiO2 with mixing carried out at room temperature to prepare TiO2 with mixing CuPc material; and TiO2 by machine mixed material compression-molded with CuPc.
3.根据权利要求I所述的制作声表面波传感器ニ氧化钛掺杂酞菁铜敏感膜的方法,其特征在于,所述电子束蒸发该TiO2与CuPc混合材料,并剥离光刻胶形成ニ氧化钛掺杂酞菁铜敏感膜,包括: 在基片上涂光刻胶; 在光刻胶上电子束蒸发压制好的TiO2与CuPc混合材料,将块状TiO2与CuPc混合材料当作电子束蒸发的靶材进行蒸发;以及将基片泡在化学试剂中使得光刻胶溶解,从而剥离光刻胶,形成ニ氧化钛掺杂酞菁铜敏感膜。 The surface acoustic wave sensor prepared according to method I Ni-doped titanium oxide of copper phthalocyanine as claimed in claim sensitive membrane, wherein said electron beam evaporation CuPc mixed with the TiO2 material, and stripping the photoresist forming Ni copper phthalocyanine-doped titanium oxide sensitive film, comprising: coating a photoresist on a substrate; electron beam evaporation on the resist compression better material mixing CuPc and TiO2, TiO2 and the bulk mixed material as CuPc electron beam evaporation the target was evaporated; and the sensitive film of copper phthalocyanine-doped Ni oxide substrate is soaked in the chemical reagents such that the photoresist is dissolved, thereby stripping the photoresist, is formed.
CN201110155259XA 2011-06-10 2011-06-10 Method for producing titanium dioxide doped copper phthalocyanine sensitive membrane of acoustic surface wave sensor CN102820867A (en)

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