CN111307911A - A kind of pH sensor and preparation method thereof - Google Patents
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Abstract
Description
技术领域technical field
本发明涉及一种pH传感器及其制备方法，属于传感器技术领域。The invention relates to a pH sensor and a preparation method thereof, belonging to the technical field of sensors.
背景技术Background technique
离子敏感场效应晶体管(Ion-Sensitive Field Effect Transistor，简称ISFET)作为检测生物化学信号的敏感器件，首先由荷兰科学家P.Bergveld于1970年 提出，并将其用于神经生理学的测量，从此揭开了生化传感器的一个新的研究 序幕，为电化学生化传感器的研究注入了新的活力，具有划时代的意义。Ion-Sensitive Field Effect Transistor (ISFET), as a sensitive device for detecting biochemical signals, was first proposed by Dutch scientist P. Bergveld in 1970 and used for neurophysiological measurements. It is a new prelude to the research of biochemical sensors, which injects new vitality into the research of electrochemical biochemical sensors, which is of epoch-making significance.
ISFET最基础的应用是用于pH值检测中，许多生物化学实验的分析都要基 于监测生化反应中的pH值的变化，但是想要取得相关技术的突破却如同要打赢 一场旷日持久的战争。例如，许多种类的细菌都需要在特定的培养皿中生长， 而它们在氧化或发酵条件下的数量达到足够多之前都是孤立存在的。目前，如 果需要检测由细菌产生的周围环境pH的变化，一般需要利用着色的pH指示剂， 在耗费大约24-36h的漫长等待中才能得到相关实验数据。因此，为提高相关检 测技术，微流体器件和微传感器等微检测技术的发展势在必行。The most basic application of ISFET is in pH value detection. The analysis of many biochemical experiments is based on monitoring the pH value changes in biochemical reactions. However, to achieve breakthroughs in related technologies is like winning a protracted war. . For example, many species of bacteria need to be grown in specific petri dishes and remain in isolation until they reach sufficient numbers under oxidative or fermentative conditions. At present, if it is necessary to detect the pH change of the surrounding environment produced by bacteria, it is generally necessary to use a colored pH indicator, and the relevant experimental data can only be obtained after a long wait of about 24-36 hours. Therefore, in order to improve the related detection technology, the development of micro-detection technologies such as microfluidic devices and micro-sensors is imperative.
近年来，借助金属-氧化物半导体场效应晶体管(Metal-Oxide-SemiconductorField Effect Transistor，简称MOSFET)的特有结构，经过创新性的独特设计， ISFET实现了具有较高灵敏度、高分辨率、短的响应时间等优异特性的新型生 化传感器。具有体积小、制造成本低、易于集成、无破坏性和可持久测量等优 点，并且通过对相应敏感材料的变更可满足各种特异性检测的要求，可广泛应 用于食品安全、生物医学、环境监测、军事航天、农业机械、工业控制以及司 法鉴定多个领域。In recent years, with the help of the unique structure of Metal-Oxide-Semiconductor Field Effect Transistor (MOSFET), through innovative and unique design, ISFET has achieved high sensitivity, high resolution and short response time. A new biochemical sensor with excellent properties such as time. It has the advantages of small size, low manufacturing cost, easy integration, non-destructive and durable measurement, and can meet the requirements of various specific detection by changing the corresponding sensitive materials, and can be widely used in food safety, biomedicine, environmental Monitoring, military aerospace, agricultural machinery, industrial control and forensic identification.
ISFET不同于传统使用离子选择电极的生化传感器，其具有更小的体积， 更快的检测速度，检测时需要的检测样本也更少，更适合进行实时而连续的系 统性监测。ISFET的基本器件结构与MOSFET非常相似，可看作去掉金属栅极 的MOSFET，其敏感薄膜淀积在栅介质层上并与电解溶液直接接触，溶液中某 些离子浓度的变化或者某些特异性行为会导致相应界面电势及电位分布的改 变，从而引起ISFET器件阈值电压的相应改变。这些变化可通过测量在相同源 漏电流下参考电极电位的变化情况，或者直接测量源漏电流的变化得到溶液中 离子浓度的改变量以及相关特异性行为的产生情况。Unlike traditional biochemical sensors using ion-selective electrodes, ISFET has a smaller volume, faster detection speed, and requires fewer detection samples during detection, making it more suitable for real-time and continuous systematic monitoring. The basic device structure of ISFET is very similar to that of MOSFET. It can be regarded as a MOSFET without the metal gate. Its sensitive film is deposited on the gate dielectric layer and is in direct contact with the electrolytic solution. The concentration of some ions in the solution changes or some specificity Behaviors lead to changes in the corresponding interface potential and potential distribution, which in turn lead to corresponding changes in the threshold voltage of the ISFET device. These changes can be obtained by measuring the change of the reference electrode potential under the same source-drain current, or by directly measuring the change of the source-drain current to obtain the change of the ion concentration in the solution and the generation of the related specific behavior.
对于ISFET来说，敏感层材料的选择直接决定着ISFET器件的检测灵敏度。For ISFET, the choice of sensitive layer material directly determines the detection sensitivity of the ISFET device.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于提供一种pH传感器，该传感器选择对氢离子具有一定特 异性和灵敏度的敏感材料，具有极高的灵敏特性。The purpose of the present invention is to provide a pH sensor, which selects sensitive materials with certain specificity and sensitivity to hydrogen ions, and has extremely high sensitivity characteristics.
本发明的另一目的在于提供一种所述传感器的制备方法。Another object of the present invention is to provide a preparation method of the sensor.
为实现上述目的，本发明采用以下技术方案：To achieve the above object, the present invention adopts the following technical solutions:
一种pH传感器，该传感器包括绝缘衬底材料、沉积在该绝缘衬底材料上的 MoS2薄膜、源电极、漏电极以及电介质材料；其中，源电极、漏电极与电介质 材料形成在MoS2薄膜周围构成封闭的传感器槽。A pH sensor comprising an insulating substrate material, a MoS 2 film deposited on the insulating substrate material, a source electrode, a drain electrode and a dielectric material; wherein the source electrode, the drain electrode and the dielectric material are formed on the MoS 2 film A closed sensor slot is formed around it.
本发明使用MoS2薄膜作为敏感层材料制备pH传感器，该pH传感器是一 种基于类似场效应管结构的传感器。MoS2材料是一种分层结晶。它的每一层平 面都包含一个晶胞，并且通过范德华力将各个平面维持在一起。每个MoS2晶胞 由硫原子和夹在硫原子之间的钼原子组成。当剥离成单层或少层时，二维MoS2材料表现出独特的电学、光学、机械和化学特性。类似于石墨烯和其他二维纳 米材料，MoS2由于其较大表面积以及良好的生物相容性，可以显著提升生物传 感性能。并且，由于直接带隙的存在，基于MoS2的FET生物传感器的整体灵 敏度远大于基于石墨烯和氧化石墨烯这些不具有或具有小的带隙的器件。 The present invention uses the MoS2 thin film as the sensitive layer material to prepare the pH sensor, and the pH sensor is a sensor based on a structure similar to a field effect tube. MoS2 material is a layered crystal. Each of its planes contains a unit cell, and the planes are held together by van der Waals forces. Each MoS2 unit cell consists of sulfur atoms and molybdenum atoms sandwiched between the sulfur atoms. When exfoliated into monolayers or few layers, 2D MoS2 materials exhibit unique electrical, optical, mechanical, and chemical properties. Similar to graphene and other 2D nanomaterials, MoS2 can significantly enhance biosensing performance due to its large surface area and good biocompatibility. And, due to the existence of direct bandgap, the overall sensitivity of MoS2 - based FET biosensors is much greater than that of graphene and graphene oxide-based devices with no or small bandgap.
一种所述pH传感器的制备方法，包括以下步骤：A preparation method of the pH sensor, comprising the following steps:
(1)清洗衬底，在衬底上涂一层光刻胶；(1) cleaning the substrate, and coating a layer of photoresist on the substrate;
(2)在光刻胶上曝光形成MoS2薄膜沉积区域；(2) exposure on the photoresist to form a MoS 2 thin film deposition area;
(3)使用化学气相沉积技术在该区域沉积MoS2，形成MoS2薄膜；(3) using chemical vapor deposition technology to deposit MoS 2 in this area to form a MoS 2 thin film;
(4)去除光刻胶保留MoS2薄膜图形，然后在MoS2薄膜图形的外侧形成源 电极和漏电极；(4) removing the photoresist to retain the MoS 2 thin film pattern, and then forming a source electrode and a drain electrode on the outside of the MoS 2 thin film pattern;
(5)沉积电介质材料形成传感器槽，得到pH传感器的器件单元。(5) depositing a dielectric material to form a sensor groove to obtain a device unit of a pH sensor.
本发明的优点在于：The advantages of the present invention are:
(1)操作简单，节省时间。本发明通过构建高性能的MoS2的pH传感器 能够实现快速监测。(1) Simple operation and time saving. The present invention can realize rapid monitoring by constructing a high-performance MoS 2 pH sensor.
(2)经济。采用本发明构建一个传感器件仅需要极少的成本。(2) Economy. Construction of a sensing device using the present invention requires only minimal costs.
(3)高产，利于集成化。可使用标准的金属氧化物半导体工艺制备芯片型 传感器件，且芯片体积较小有助于未来集成其他模块。(3) High yield, conducive to integration. Chip-type sensing devices can be fabricated using standard metal-oxide-semiconductor processes, and the small size of the chip facilitates future integration of other modules.
(4)性能优越。本发明构建的pH传感器电学信号优越，且具有良好的稳 定性。(4) Superior performance. The pH sensor constructed by the present invention has superior electrical signal and good stability.
附图说明Description of drawings
图1为表示本发明的pH传感器的制备过程的示意图。FIG. 1 is a schematic diagram showing the production process of the pH sensor of the present invention.
图2为本发明的pH传感器的截面结构示意图。FIG. 2 is a schematic cross-sectional structure diagram of the pH sensor of the present invention.
图3为本发明的pH传感器的工作原理图。FIG. 3 is a working principle diagram of the pH sensor of the present invention.
图4((a)-(c))为本发明的pH传感器中单层MoS2薄膜的AFM图像。Figure 4((a)-(c)) are the AFM images of the monolayer MoS 2 film in the pH sensor of the present invention.
图5((a)-(c))为本发明的pH传感器中双层MoS2薄膜的AFM图像。Figure 5((a)-(c)) are AFM images of the bilayer MoS 2 thin film in the pH sensor of the present invention.
图6为采用实施例1的pH传感器测试时不同pH对应的栅压与漏电流曲线。FIG. 6 is the gate voltage and leakage current curves corresponding to different pHs when the pH sensor of Example 1 is used for testing.
图7为采用实施例1的pH传感器测试时pH值与阈值电压及电流之间的关 系曲线。Fig. 7 is the relation curve between pH value and threshold voltage and current when using the pH sensor of Example 1 to test.
具体实施方式Detailed ways
以下结合附图和实施例对本发明进行进一步详细说明，但并不意味着对本 发明保护范围的限制。The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments, but it is not intended to limit the protection scope of the present invention.
如图1所示，本发明的pH传感器是一种基于类似场效应管结构的传感器， 其制备过程如下；首先清洗氧化硅衬底1，在氧化硅衬底1上涂一层光刻胶2， 然后曝光出要沉积MoS2薄膜的图形3，采用CVD方法沉积MoS2薄膜4，去除 光刻胶保留MoS2薄膜图形，然后在MoS2薄膜图形的外侧形成源电极5和漏电 极6，最后沉积电介质材料7形成传感器槽，使整个传感器的器件对于待测电解 液为槽状，与周围隔离。As shown in FIG. 1 , the pH sensor of the present invention is a sensor based on a structure similar to a field effect transistor, and its preparation process is as follows; first, a
实施例1Example 1
如图2所示，为本发明的pH传感器的截面结构示意图。具体地，该pH传 感器的制作方法包括以下工艺：As shown in FIG. 2 , it is a schematic cross-sectional structure diagram of the pH sensor of the present invention. Specifically, the manufacturing method of the pH sensor includes the following processes:
在SiO2(300nm)/Si衬底旋涂一层SU-8 GM10xx系列光刻胶，厚度为3μm， 曝光得到要沉积MoS2薄膜的图形，然后使用CVD方法沉积MoS2薄膜，具体 工艺过程如下：生长区温度为650℃，硫区温度为180℃，硫源、钼源的加载量 分别为1000mg和100mg，生长时间为20min，载气流量为10sccm。然后去 胶得到MoS2薄膜图形。使用光刻以及电子束蒸发的方法制造源电极和漏电极。 单个芯片的尺寸是10μm。源电极与漏电极的厚度均为500nm，两个电极之间 间隔10μm。同时，为了增强Au电极和氧化硅衬底之间的粘合性，另外在两者 之间加入了厚度为20nm的Ti层。然后使用光刻以及磁控溅射方法生长HfO2电介质层，厚度为500nm。A layer of SU-8 GM10xx series photoresist was spin-coated on a SiO 2 (300nm)/Si substrate with a thickness of 3 μm, exposed to obtain the pattern of the MoS 2 film to be deposited, and then the MoS 2 film was deposited by CVD. The specific process is as follows : The temperature of the growth zone is 650 °C, the temperature of the sulfur zone is 180 °C, the loadings of the sulfur source and the molybdenum source are 1000 mg and 100 mg, respectively, the growth time is 20 min, and the carrier gas flow is 10 sccm. Then the glue is removed to obtain the MoS 2 thin film pattern. The source and drain electrodes were fabricated using photolithography and electron beam evaporation. The size of a single chip is 10 μm. The thickness of the source electrode and the drain electrode are both 500 nm, and the distance between the two electrodes is 10 μm. At the same time, in order to enhance the adhesion between the Au electrode and the silicon oxide substrate, a Ti layer with a thickness of 20 nm was added between the two. The HfO2 dielectric layer was then grown to a thickness of 500 nm using photolithography and magnetron sputtering methods.
图3为本发明的传感器工作原理图，在电化学检测之前，首先将待测电解 液9通过微流控制器件滴入所制备的传感器中，将Ag/AgCl参比电极8固定于 传感器的旁边，我们采用的是两电极系统因此将参比电极夹和对电极夹共同连 接在参比电极上，与工作电极构成电流回路，从而评价pH。Fig. 3 is the working principle diagram of the sensor of the present invention. Before the electrochemical detection, the
图4(a)-(e)为本发明的pH传感器中单层MoS2薄膜的AFM图像，所测量的 MoS2厚度为0.8nm左右。图5(d)-(f)为本发明的pH传感器中双层MoS2薄膜的 AFM图像，所测量的MoS2厚度约为1.5nm。4(a)-(e) are the AFM images of the monolayer MoS 2 thin film in the pH sensor of the present invention, and the measured thickness of MoS 2 is about 0.8 nm. Figures 5(d)-(f) are AFM images of the bilayer MoS 2 thin film in the pH sensor of the present invention, and the measured thickness of MoS 2 is about 1.5 nm.
图6为本发明传感器测试中不同pH对应的栅压与漏电流曲线，可以看出对 不同pH值得良好区分。Fig. 6 is the grid voltage and leakage current curves corresponding to different pHs in the sensor test of the present invention, and it can be seen that different pH values are well differentiated.
图7本发明传感器pH值与阈值电压及电流之间的关系曲线。可以看出本发 明传感器对pH具有优异的敏感特性。FIG. 7 is a relationship curve between pH value and threshold voltage and current of the sensor of the present invention. It can be seen that the sensor of the present invention has excellent sensitivity to pH.
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