CN108956710B - A kind of preparation method of grid-like ZnO spiral porous hollow nanowire sensor - Google Patents
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Abstract
Description
技术领域technical field
本发明属于传感器制备技术领域，主要涉及一种网格状ZnO螺旋式多孔空心纳米线传感器的制备方法。The invention belongs to the technical field of sensor preparation, and mainly relates to a preparation method of a grid-shaped ZnO spiral porous hollow nanowire sensor.
背景技术Background technique
传感器是当今科学发展中非常重要的一个领域，它可以在智能家居、安全生产、环境保护、国防等领域发挥积极的作用。因此，高性能传感器一直是科研人员努力的目标。Si具有制备工艺成熟、成本低廉、尺寸大等优点，因而Si基传感器受到人们的广泛关注。为了实现Si基传感器，人们一般是通过对高质量Si衬底进行刻蚀，在Si衬底上获得Si纳米阵列，接着增加Au电极和引出Au线，从而构成完整的传感器结构。Sensor is a very important field in today's scientific development, it can play an active role in smart home, safety production, environmental protection, national defense and other fields. Therefore, high-performance sensors have always been the goal of researchers' efforts. Si has the advantages of mature preparation technology, low cost, and large size, so Si-based sensors have received extensive attention. In order to realize the Si-based sensor, people generally etch a high-quality Si substrate to obtain a Si nanoarray on the Si substrate, and then add Au electrodes and lead out Au wires to form a complete sensor structure.
然而，Si纳米阵列传感器的最小探测极限一般为100ppm，远亚于其它半导体传感器(5-10ppm)。此外，它的相应时间一般为30-50s，即它的灵敏度也需要进一步提高。除了Si基传感器，ZnO基传感器也受到了人们的重视。ZnO具有电学和光学性能优异、无毒、原材料丰富、制备工艺相对简单等优点，因而，在半导体器件领域中得到了广泛的应用。However, the minimum detection limit of Si nanoarray sensors is generally 100 ppm, which is much lower than that of other semiconductor sensors (5-10 ppm). In addition, its corresponding time is generally 30-50s, that is, its sensitivity needs to be further improved. In addition to Si-based sensors, ZnO-based sensors have also received much attention. ZnO has the advantages of excellent electrical and optical properties, non-toxicity, abundant raw materials, and relatively simple preparation process. Therefore, ZnO has been widely used in the field of semiconductor devices.
目前，Au/ZnO纳米柱阵列传感器最小探测极限一般为10ppm，要优于Si纳米阵列传感器。然而，现有技术的缺点有：At present, the minimum detection limit of Au/ZnO nano-pillar array sensors is generally 10 ppm, which is better than that of Si nano-array sensors. However, the disadvantages of the prior art are:
1.ZnO纳米柱/纳米线的制备工艺较复杂，成本较高；1. The preparation process of ZnO nanopillars/nanowires is complicated and the cost is high;
2.垂直分布ZnO纳米柱/纳米线电信号的传播路径较长，传感器响应时间较长。2. The propagation path of the electrical signal of the vertically distributed ZnO nanopillars/nanowires is longer, and the response time of the sensor is longer.
发明内容SUMMARY OF THE INVENTION
本发明的目的是在于为克服现有技术的不足，提供一种网格状ZnO螺旋式多孔空心纳米线传感器的制备方法，采用本发明的方法可以改善ZnO纳米线的生产工艺，降低工艺的复杂性和生产成本以及提高传感器响应的灵敏度。The object of the present invention is to provide a method for preparing a grid-like ZnO spiral porous hollow nanowire sensor in order to overcome the deficiencies of the prior art, and the method of the present invention can improve the production process of ZnO nanowires and reduce the complexity of the process. performance and production costs as well as improving the sensitivity of the sensor response.
本发明采用的技术方案是：一种网格状ZnO螺旋式多孔空心纳米线传感器的制备方法，包括以下步骤：The technical scheme adopted in the present invention is: a preparation method of a grid-like ZnO spiral porous hollow nanowire sensor, comprising the following steps:
A.前驱体纤维的制备：A. Preparation of Precursor Fibers:
配制无机物/PVP纺丝液，进行静电纺丝，制得网格状螺旋式无机物/PVP前驱体纤维；所述无机物/PVP纺丝液是Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O、Al(NO3)3·6H2O和PVP的混合溶液；The inorganic/PVP spinning solution is prepared, and electrospinning is performed to obtain a grid-like spiral inorganic/PVP precursor fiber; the inorganic/PVP spinning solution is Zn(NO 3 ) 2 ·4H 2 O, Mixed solution of Zn(CH 2 COO) 2 ·4H 2 O, Al(NO 3 ) 3 ·6H 2 O and PVP;
B.纳米线的制备：B. Preparation of Nanowires:
将网格状螺旋式无机物/PVP前驱体纤维煅烧，获得网格状Al掺杂ZnO螺旋式多孔空心纳米线；calcining grid-like spiral inorganic/PVP precursor fibers to obtain grid-like Al-doped ZnO spiral porous hollow nanowires;
C.传感器的制备：C. Preparation of the sensor:
在网格状Al掺杂ZnO螺旋式多孔空心纳米线四周涂覆导电极，并引出导线，即可获得网格状ZnO螺旋式多孔空心纳米线传感器。A grid-shaped ZnO spiral porous hollow nanowire sensor can be obtained by coating a conductive electrode around the grid-shaped Al-doped ZnO spiral porous hollow nanowire, and drawing out the wires.
优选的，所述无机物/PVP纺丝液的制备方法是：将Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O和Al(NO3)3·6H2O混合，得到无机物；将无机物溶于去离子水，加入聚乙PVP，搅拌30-90min，静置，得到无机物/PVP纺丝液。Preferably, the preparation method of the inorganic matter/PVP spinning solution is as follows: Zn(NO 3 ) 2 ·4H 2 O, Zn(CH 2 COO ) 2 ·4H 2 O and Al(NO 3 ) 3 ·6H 2 Mix with O to obtain inorganic matter; dissolve the inorganic matter in deionized water, add polyethylene PVP, stir for 30-90 min, and let stand to obtain inorganic matter/PVP spinning solution.
优选的，Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O和Al(NO3)3·6H2O的质量比为1:0.5-3:0.01-0.05。Preferably, the mass ratio of Zn(NO 3 ) 2 ·4H 2 O, Zn(CH 2 COO) 2 ·4H 2 O and Al(NO 3 ) 3 ·6H 2 O is 1:0.5-3:0.01-0.05.
优选的，所述无机物/PVP纺丝液中，PVP的浓度为40-50wt％，无机物浓度为8-15wt％。更优选的，PVP的浓度为46wt％，无机物浓度为10wt％。Preferably, in the inorganic/PVP spinning solution, the concentration of PVP is 40-50 wt%, and the concentration of inorganic matter is 8-15 wt%. More preferably, the concentration of PVP is 46 wt %, and the concentration of inorganic substances is 10 wt %.
优选的，PVP的分子量是2000-50000。Preferably, the molecular weight of PVP is 2000-50000.
优选的，所述网格状螺旋式无机物/PVP前驱体纤维的网格为正方形，其边长为400-2500nm。Preferably, the grid of the grid-shaped helical inorganic/PVP precursor fiber is square, and the side length is 400-2500 nm.
优选的，步骤B中，煅烧过程控制的条件为：升温速率1-5℃/min，升温至600-900℃，煅烧8-16小时。Preferably, in step B, the conditions for controlling the calcination process are: a heating rate of 1-5°C/min, heating to 600-900°C, and calcination for 8-16 hours.
优选的，所述电极是Ag电极、Au电极或者导电胶。Preferably, the electrodes are Ag electrodes, Au electrodes or conductive glue.
优选的，所述的传感器是气敏传感器。Preferably, the sensor is a gas sensor.
更具体的，网格状ZnO螺旋式多孔空心纳米线传感器的制备方法的具体步骤如下：More specifically, the specific steps of the preparation method of the grid-like ZnO helical porous hollow nanowire sensor are as follows:
(1)将质量比为1:0.5-3:0.015的Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O和Al(NO3)3·6H2O、均匀混合，溶于去离子水，称取一定量的分子量聚乙烯吡咯烷酮(PVP(K40))，室温下搅拌30-120min，静置即可获得纺丝液，纺丝液中的PVP的含量为46wt％，无机盐含量为10wt％；(1) Zn(NO 3 ) 2 .4H 2 O, Zn(CH 2 COO) 2 .4H 2 O, and Al(NO 3 ) 3 .6H 2 O in a mass ratio of 1:0.5 to 3:0.015, uniformly Mixed, dissolved in deionized water, weighed a certain amount of molecular weight polyvinylpyrrolidone (PVP(K40)), stirred at room temperature for 30-120min, stood still to obtain spinning solution, the content of PVP in the spinning solution was 46wt %, the inorganic salt content is 10wt%;
(2)在ITO导电玻璃上，采用静电纺丝，制备网格状螺旋式无机物/PVP前驱体纤维，网格为正方形，边长为400-2500nm；(2) On ITO conductive glass, electrospinning is used to prepare grid-like spiral inorganic/PVP precursor fibers, the grid is square, and the side length is 400-2500nm;
(3)将前驱体纤维转移至箱式电阻炉中，然后1-5℃/min的升温速率，升温至600-900℃，煅烧8-16小时，即可获得网格状ZnO螺旋式多孔空心纳米线；(3) Transfer the precursor fiber to the box-type resistance furnace, then at a heating rate of 1-5 °C/min, heat up to 600-900 °C, and calcinate for 8-16 hours to obtain a grid-like ZnO spiral porous hollow Nanowires;
(4)在网格状ZnO螺旋式多孔空心纳米线四周涂覆Ag或者Au电极或者导电胶，并引出导线，即可获得结构完成的气敏传感器。(4) Coating Ag or Au electrodes or conductive glue around the grid-shaped ZnO spiral porous hollow nanowires, and drawing out the wires, the gas sensor with completed structure can be obtained.
本发明的有益效果如下：(1)使用静电纺丝制备ZnO纳米线，可控性好，且有利于降低工艺复杂程度和生产成本；(2)ZnO纳米线改为平面式分布，缩短了信号的传播路程，有利于提高器件响应的灵敏度。The beneficial effects of the present invention are as follows: (1) Electrospinning is used to prepare ZnO nanowires, which has good controllability and is conducive to reducing process complexity and production cost; (2) ZnO nanowires are changed to planar distribution, which shortens the signal The propagation distance is beneficial to improve the sensitivity of the device response.
附图说明Description of drawings
图1是网格状Al掺杂ZnO多孔螺旋式纳米线气敏传感器的示意图，其中，11是ITO衬底，12是网格状Al掺杂ZnO多孔螺旋式纳米线，13是电极。1 is a schematic diagram of a grid-shaped Al-doped ZnO porous helical nanowire gas sensor, wherein 11 is an ITO substrate, 12 is a grid-shaped Al-doped ZnO porous helical nanowire, and 13 is an electrode.
具体实施方式Detailed ways
为了更好的解释本发明，现结合以下具体实施例做进一步说明，但是本发明不限于具体实施例。In order to better explain the present invention, further description will now be made in conjunction with the following specific embodiments, but the present invention is not limited to the specific embodiments.
实施例1Example 1
将质量比为1:0.5:0.01的Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O和Al(NO3)3·6H2O、均匀混合，溶于去离子水，称取一定量的分子量为2000的聚乙烯吡咯烷酮(PVP(K40))，室温下搅拌30min，静置即可获得纺丝液，其中纺丝液中的PVP的浓度为40wt％，无机盐浓度为10wt％；Zn(NO 3 ) 2 ·4H 2 O, Zn(CH 2 COO) 2 ·4H 2 O and Al(NO 3 ) 3 ·6H 2 O with a mass ratio of 1:0.5:0.01 were uniformly mixed and dissolved in Ionized water, weigh a certain amount of polyvinylpyrrolidone (PVP(K40)) with a molecular weight of 2000, stir at room temperature for 30min, and stand to obtain a spinning solution, wherein the concentration of PVP in the spinning solution is 40wt%, inorganic The salt concentration is 10wt%;
在ITO导电玻璃上使用静电纺丝制备网格状螺旋式无机物/PVP前驱体纤维，网格为正方形，边长为1000nm；Grid-like helical inorganic/PVP precursor fibers were prepared by electrospinning on ITO conductive glass. The grid was square and the side length was 1000 nm;
将前驱体纤维转移至箱式电阻炉中，然后1℃/min的升温速率，升温至600℃，煅烧8小时，即可获得网格状ZnO螺旋式多孔空心纳米线；The precursor fibers were transferred to a box-type resistance furnace, then heated to 600°C at a heating rate of 1°C/min, and calcined for 8 hours to obtain grid-like ZnO spiral porous hollow nanowires;
在网格状ZnO螺旋式多孔空心纳米线四周涂覆导Au电极，并引出导线，即可获得气敏传感器。A gas sensor can be obtained by coating conductive Au electrodes around the grid-like ZnO helical porous hollow nanowires and drawing out the wires.
所得的气敏传感器的结构如图1所示。The structure of the obtained gas sensor is shown in Figure 1.
实施例2Example 2
将质量比为1:1:0.015的Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O和Al(NO3)3·6H2O、均匀混合，溶于去离子水，称取一定量的分子量为30000的聚乙烯吡咯烷酮(PVP(K40))，室温下搅拌60min，静置即可获得纺丝液，其中纺丝液中的PVP的浓度为45wt％，无机盐浓度为10wt％；Zn(NO 3 ) 2 ·4H 2 O, Zn(CH 2 COO) 2 ·4H 2 O and Al(NO 3 ) 3 ·6H 2 O with a mass ratio of 1:1:0.015 were uniformly mixed and dissolved in Ionized water, weigh a certain amount of polyvinylpyrrolidone (PVP(K40)) with a molecular weight of 30000, stir at room temperature for 60min, and stand to obtain a spinning solution, wherein the concentration of PVP in the spinning solution is 45wt%, inorganic The salt concentration is 10wt%;
在ITO导电玻璃上使用静电纺丝制备网格状螺旋式无机物/PVP前驱体纤维，网格为正方形，边长为1000nm；Grid-like helical inorganic/PVP precursor fibers were prepared by electrospinning on ITO conductive glass. The grid was square and the side length was 1000 nm;
将前驱体纤维转移至箱式电阻炉中，然后1℃/min的升温速率，升温至600℃，煅烧8小时，即可获得网格状ZnO螺旋式多孔空心纳米线；The precursor fibers were transferred to a box-type resistance furnace, then heated to 600°C at a heating rate of 1°C/min, and calcined for 8 hours to obtain grid-like ZnO spiral porous hollow nanowires;
在网格状ZnO螺旋式多孔空心纳米线四周涂覆导Au电极，并引出导线，即可获得气敏传感器。A gas sensor can be obtained by coating conductive Au electrodes around the grid-like ZnO helical porous hollow nanowires and drawing out the wires.
实施例3Example 3
将质量比为1:2:0.02的Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O和Al(NO3)3·6H2O、均匀混合，溶于去离子水，称取一定量的分子量为50000的聚乙烯吡咯烷酮(PVP(K40))，室温下搅拌90min，静置即可获得纺丝液，其中纺丝液中的PVP的浓度为50wt％，无机盐浓度为10wt％；Zn(NO 3 ) 2 ·4H 2 O, Zn(CH 2 COO) 2 ·4H 2 O and Al(NO 3 ) 3 ·6H 2 O with a mass ratio of 1:2:0.02 were uniformly mixed and dissolved in Ionized water, weigh a certain amount of polyvinylpyrrolidone (PVP(K40)) with a molecular weight of 50000, stir at room temperature for 90min, and stand to obtain a spinning solution, wherein the concentration of PVP in the spinning solution is 50wt%, inorganic The salt concentration is 10wt%;
在ITO导电玻璃上使用静电纺丝制备网格状螺旋式无机物/PVP前驱体纤维，网格为正方形，边长为1000nm；Grid-like helical inorganic/PVP precursor fibers were prepared by electrospinning on ITO conductive glass. The grid was square and the side length was 1000 nm;
将前驱体纤维转移至箱式电阻炉中，然后1℃/min的升温速率，升温至600℃，煅烧8小时，即可获得网格状ZnO螺旋式多孔空心纳米线；The precursor fibers were transferred to a box-type resistance furnace, then heated to 600°C at a heating rate of 1°C/min, and calcined for 8 hours to obtain grid-like ZnO spiral porous hollow nanowires;
在网格状ZnO螺旋式多孔空心纳米线四周涂覆导Au电极，并引出导线，即可获得气敏传感器。A gas sensor can be obtained by coating conductive Au electrodes around the grid-like ZnO helical porous hollow nanowires and drawing out the wires.
实施例4Example 4
将质量比为1:2.5:0.03的Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O和Al(NO3)3·6H2O、均匀混合，溶于去离子水，称取一定量的分子量为30000的聚乙烯吡咯烷酮(PVP(K40))，室温下搅拌60min，静置即可获得纺丝液，其中纺丝液中的PVP的浓度为45wt％，无机盐浓度为10wt％；Zn(NO 3 ) 2 ·4H 2 O, Zn(CH 2 COO) 2 ·4H 2 O and Al(NO 3 ) 3 ·6H 2 O with a mass ratio of 1:2.5:0.03 were uniformly mixed and dissolved in Ionized water, weigh a certain amount of polyvinylpyrrolidone (PVP(K40)) with a molecular weight of 30000, stir at room temperature for 60min, and stand to obtain a spinning solution, wherein the concentration of PVP in the spinning solution is 45wt%, inorganic The salt concentration is 10wt%;
在ITO导电玻璃上使用静电纺丝制备网格状螺旋式无机物/PVP前驱体纤维，网格为正方形，边长为1000nm；Grid-like helical inorganic/PVP precursor fibers were prepared by electrospinning on ITO conductive glass. The grid was square and the side length was 1000 nm;
将前驱体纤维转移至箱式电阻炉中，然后3℃/min的升温速率，升温至750℃，煅烧12小时，即可获得网格状ZnO螺旋式多孔空心纳米线；The precursor fibers were transferred to a box-type resistance furnace, and then heated to 750 °C at a heating rate of 3 °C/min, and calcined for 12 hours to obtain a grid-like ZnO spiral porous hollow nanowire;
在网格状ZnO螺旋式多孔空心纳米线四周涂覆导Au电极，并引出导线，即可获得气敏传感器。A gas sensor can be obtained by coating conductive Au electrodes around the grid-like ZnO helical porous hollow nanowires and drawing out the wires.
实施例5Example 5
将质量比为1:3:0.05的Zn(NO3)2·4H2O、Zn(CH2COO)2·4H2O和Al(NO3)3·6H2O、均匀混合，溶于去离子水，称取一定量的分子量为3的聚乙烯吡咯烷酮(PVP(K40))，室温下搅拌60min，静置即可获得纺丝液，其中纺丝液中的PVP的浓度为45wt％，无机盐浓度为10wt％；Zn(NO 3 ) 2 ·4H 2 O, Zn(CH 2 COO) 2 ·4H 2 O and Al(NO 3 ) 3 ·6H 2 O in a mass ratio of 1:3:0.05 were uniformly mixed and dissolved in Ionized water, weigh a certain amount of polyvinylpyrrolidone (PVP(K40)) with a molecular weight of 3, stir at room temperature for 60min, and stand to obtain a spinning solution, wherein the concentration of PVP in the spinning solution is 45wt%, inorganic The salt concentration is 10wt%;
在ITO导电玻璃上使用静电纺丝制备网格状螺旋式无机物/PVP前驱体纤维，网格为正方形，边长为1000nm；Grid-like helical inorganic/PVP precursor fibers were prepared by electrospinning on ITO conductive glass. The grid was square and the side length was 1000 nm;
将前驱体纤维转移至箱式电阻炉中，然后5℃/min的升温速率，升温至900℃，煅烧16小时，即可获得网格状ZnO螺旋式多孔空心纳米线；The precursor fibers were transferred to a box-type resistance furnace, and then heated to 900 °C at a heating rate of 5 °C/min, and calcined for 16 hours to obtain grid-like ZnO spiral porous hollow nanowires;
在网格状ZnO螺旋式多孔空心纳米线四周涂覆导Au电极，引出导线，即可气敏传感器。A conductive Au electrode is coated around the grid-shaped ZnO spiral porous hollow nanowire, and the lead wire is drawn out to form a gas sensor.
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