CN105319245A - Flexible organic film capacitive sensor capable of sensing humidity and gas simultaneously and manufacturing method thereof - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 17
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- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 4
- 229920001721 polyimide Polymers 0.000 claims abstract description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 16
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- 238000002360 preparation method Methods 0.000 claims description 8
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- 238000005566 electron beam evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
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- BYIMSFXYUSZVLI-UHFFFAOYSA-N 3-methoxysilylpropan-1-amine Chemical compound CO[SiH2]CCCN BYIMSFXYUSZVLI-UHFFFAOYSA-N 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 238000004062 sedimentation Methods 0.000 claims 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical group CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 abstract description 4
- ZLDHYRXZZNDOKU-UHFFFAOYSA-N n,n-diethyl-3-trimethoxysilylpropan-1-amine Chemical compound CCN(CC)CCC[Si](OC)(OC)OC ZLDHYRXZZNDOKU-UHFFFAOYSA-N 0.000 abstract description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 2
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- 229910052751 metal Inorganic materials 0.000 abstract description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 10
- 239000010409 thin film Substances 0.000 description 9
- 239000010408 film Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
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- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供的一种可同时感应湿度和气体的柔性有机薄膜电容传感器，其结构如图1所示，包括衬底(1)、下电极(2)、湿度敏感层(3)、气体敏感层(4)、两个介质层(501、502)和两个上电极(601、602)；该传感器中，构成衬底的材料为PET；构成下电极的材料为ITO；构成湿度敏感层的材料为聚酰亚胺或聚甲基丙烯酸甲酯；构成气体敏感层的材料为丙基-三甲氧基硅烷或3-二乙基氨丙基-三甲氧基硅烷；构成介质层的材料为绝缘有机物，分别位于气体敏感层的两侧，中间部分暴露在外部；构成两个上电极的材料为金属金，分别位于两个介质层之上。
The present invention provides a flexible organic film capacitive sensor capable of simultaneously sensing humidity and gas, its structure is shown in Figure 1, including a substrate (1), a lower electrode (2), a humidity sensitive layer (3), a gas sensitive layer (4), two dielectric layers (501, 502) and two upper electrodes (601, 602); in this sensor, the material forming the substrate is PET; the material forming the lower electrode is ITO; the material forming the humidity sensitive layer It is polyimide or polymethyl methacrylate; the material constituting the gas sensitive layer is propyl-trimethoxysilane or 3-diethylaminopropyl-trimethoxysilane; the material constituting the dielectric layer is insulating organic , are respectively located on both sides of the gas sensitive layer, and the middle part is exposed to the outside; the material constituting the two upper electrodes is metal gold, which are respectively located on the two dielectric layers.
Description
【技术领域】【Technical field】
本发明属于有机电子传感器领域，特别涉及一种可同时感应湿度和气体的柔性有机薄膜电容传感器及其制作方法。The invention belongs to the field of organic electronic sensors, in particular to a flexible organic film capacitive sensor capable of simultaneously sensing humidity and gas and a manufacturing method thereof.
【背景技术】【Background technique】
湿度传感器和气体传感器应用范围十分广泛，现在相对成熟的湿度传感器大多采用电阻检测的方法，然而这种传感器的精度不高，且容易受到其它条件的影响。近年来，有很多电容性传感器被提出，但大多采用了刚性材料，当需要测量不平整或是弯曲表面时不能很好的覆盖。而柔性有机薄膜电容传感器作为薄膜形态，其面积可大可小的特点使得其不仅能检测精密位置的湿度或者气体浓度，在做成大面积的情况下，还可以贴附与物体表面进行大范围的检测，且不限于平面。采用有机材料制作的柔性传感器是未来发展的趋势，多功能传感器集成于一个器件更是复杂条件下检测重要的一个方向，本发明对柔性薄膜传感器的发展意义重大。Humidity sensors and gas sensors have a wide range of applications. Most of the relatively mature humidity sensors now use the resistance detection method. However, the accuracy of this sensor is not high, and it is easily affected by other conditions. In recent years, many capacitive sensors have been proposed, but most of them use rigid materials, which cannot cover well when measuring uneven or curved surfaces. As a film form, the flexible organic film capacitive sensor can be large or small, so that it can not only detect the humidity or gas concentration at a precise position, but also can be attached to the surface of an object for large-scale detection when it is made into a large area. detection, and is not limited to planes. Flexible sensors made of organic materials are the future development trend, and the integration of multifunctional sensors into one device is an important direction for detection under complex conditions. The present invention is of great significance to the development of flexible thin film sensors.
【发明内容】【Content of invention】
本发明的目的是提供一种可同时感应湿度和气体的柔性有机薄膜电容传感器及其制作方法。The object of the present invention is to provide a flexible organic film capacitive sensor capable of simultaneously sensing humidity and gas and a manufacturing method thereof.
本发明提供的一种可同时感应湿度和气体的柔性有机薄膜电容传感器，其结构如图1所示，包括衬底(1)、下电极(2)、湿度敏感层(3)、气体敏感层(4)、两个介质层(501、502)和两个上电极(601、602)；该传感器中，构成衬底的材料为PET；构成下电极的材料为ITO；构成湿度敏感层的材料为聚酰亚胺或聚甲基丙烯酸甲酯；构成气体敏感层的材料为丙基-三甲氧基硅烷或3-二乙基氨丙基-三甲氧基硅烷；构成介质层的材料为绝缘有机物，分别位于气体敏感层的两侧，中间部分暴露在外部；构成两个上电极的材料为金属金，分别位于两个介质层之上。The present invention provides a flexible organic film capacitive sensor capable of simultaneously sensing humidity and gas, its structure is shown in Figure 1, including a substrate (1), a lower electrode (2), a humidity sensitive layer (3), a gas sensitive layer (4), two dielectric layers (501, 502) and two upper electrodes (601, 602); in this sensor, the material forming the substrate is PET; the material forming the lower electrode is ITO; the material forming the humidity sensitive layer It is polyimide or polymethyl methacrylate; the material constituting the gas sensitive layer is propyl-trimethoxysilane or 3-diethylaminopropyl-trimethoxysilane; the material constituting the dielectric layer is insulating organic , are respectively located on both sides of the gas sensitive layer, and the middle part is exposed to the outside; the material constituting the two upper electrodes is metal gold, which are respectively located on the two dielectric layers.
本发明提供的制备上述柔性有机薄膜湿度传感器的方法，包括如下步骤：The method for preparing the above-mentioned flexible organic film humidity sensor provided by the present invention comprises the following steps:
1)在衬底上制备下电极；1) preparing the lower electrode on the substrate;
2)在所述步骤1)得到的下电极之上制备湿度敏感层；2) preparing a humidity sensitive layer on the lower electrode obtained in step 1);
3)在所述步骤2)得到的带有湿度敏感层的衬底之上制备气体敏感层；3) preparing a gas-sensitive layer on the substrate with a humidity-sensitive layer obtained in step 2);
4)在所述步骤3)得到的气体敏感层上制备两个介质层；4) preparing two dielectric layers on the gas-sensitive layer obtained in step 3);
5)制备源电极和漏电极，得到所述柔性有机薄膜湿度传感器；5) preparing a source electrode and a drain electrode to obtain the flexible organic thin film humidity sensor;
上述制备方法的步骤1)中，衬底材料可以通过商业途径购买得到，制作下电极之前先将衬底分别用丙酮、乙醇、去离子水各超声清洗15分钟；制备下电极的方法为磁控溅射，磁控溅射的工作气压为2.5帕斯卡，溅射功率为140瓦，沉积时间为20分钟；In step 1) of the above-mentioned preparation method, the substrate material can be purchased through commercial channels. Before making the lower electrode, the substrate is cleaned with acetone, ethanol, and deionized water for 15 minutes respectively; the method for preparing the lower electrode is magnetron Sputtering, the working pressure of magnetron sputtering is 2.5 pascals, the sputtering power is 140 watts, and the deposition time is 20 minutes;
步骤2)中，制备湿度敏感层的方法为旋涂，旋涂速度为6000转/分，旋涂时间为45秒；In step 2), the method for preparing the humidity sensitive layer is spin coating, the spin coating speed is 6000 rpm, and the spin coating time is 45 seconds;
步骤3)中，制备气体敏感层的方法为旋涂，旋涂速度为4500转/分，旋涂时间为30秒；In step 3), the method for preparing the gas-sensitive layer is spin coating, the spin coating speed is 4500 rpm, and the spin coating time is 30 seconds;
步骤4)中，制备两个介质层的方法为真空热蒸镀，真空度为8×10-3帕斯卡以下，蒸镀速率为0.1埃/秒；In step 4), the method for preparing the two dielectric layers is vacuum thermal evaporation, the vacuum degree is below 8×10 -3 Pascal, and the evaporation rate is 0.1 Angstroms/second;
步骤5)中，制备两个上电极的方法为电子束蒸发，电子束蒸发的气压为6×10-3帕斯卡，蒸发速率为0.25埃/秒。In step 5), the method for preparing the two upper electrodes is electron beam evaporation, the pressure of electron beam evaporation is 6×10 −3 Pascal, and the evaporation rate is 0.25 Å/s.
本发明的技术分析：Technical analysis of the present invention:
该可同时感应湿度和气体的柔性有机薄膜电容传感器的湿度敏感层选取的湿敏材料在湿度变化下，导致电容值发生变化；该电容传感器气体敏感层对二氧化硅气体表现出敏感的特性，当气体敏感层吸收二氧化硅后与之相互作用导致电容发生变化；传感器结构采用有机薄膜的形式，由于是薄膜状传感器，其形状可以做成大面积平面状，可以贴附与物体表面，且没有面积限制；该器件灵敏度高，无论是在要求固定点湿度检测还是大面积范围检测都可实现的特点优于现有传感器。The moisture-sensitive material selected for the humidity-sensitive layer of the flexible organic thin-film capacitive sensor that can sense humidity and gas at the same time causes a change in capacitance value under humidity changes; the gas-sensitive layer of the capacitive sensor exhibits sensitivity to silicon dioxide gas, When the gas-sensitive layer absorbs silicon dioxide and interacts with it, the capacitance changes; the sensor structure is in the form of an organic thin film. Because it is a thin-film sensor, its shape can be made into a large-area planar shape, which can be attached to the surface of an object, and There is no area limitation; the device has high sensitivity, and it is better than existing sensors whether it requires fixed-point humidity detection or large-area range detection.
【附图说明】【Description of drawings】
图1为本发明提供的一种可同时感应湿度和气体的柔性有机薄膜电容传感器的结构示意图。Fig. 1 is a structural schematic diagram of a flexible organic thin film capacitive sensor capable of simultaneously sensing humidity and gas provided by the present invention.
图中，(101、102)为两个上电极、(201、202)为两个介质层、3为气体敏感层、4为湿度敏感层、5为下电极、6为衬底。In the figure, (101, 102) are two upper electrodes, (201, 202) are two dielectric layers, 3 is a gas sensitive layer, 4 is a humidity sensitive layer, 5 is a lower electrode, and 6 is a substrate.
【具体实施方式】【detailed description】
下面结合具体实例对本发明作进一步说明。The present invention will be further described below in conjunction with specific examples.
本发明中，电容分别在不同环境条件下测量电容：In the present invention, the capacitance is measured under different environmental conditions respectively:
1)暴露于不含二氧化硫的空气中，相对湿度3％；1) Expose to air without sulfur dioxide, relative humidity 3%;
2)暴露于含二氧化硫的空气中，相对湿度54％2) Expose to air containing sulfur dioxide, relative humidity 54%
3)暴露于不含二氧化硫的空气中，相对湿度3％；3) Expose to air without sulfur dioxide, relative humidity 3%;
4)暴露于不含二氧化硫的空气中，相对湿度54％；4) Expose to air that does not contain sulfur dioxide, with a relative humidity of 54%;
在上述不同环境条件下测量电容变化，测试表面，湿度和二氧化硫都会对传感器的电容造成影响。To measure the capacitance change under the different environmental conditions mentioned above, the test surface, humidity and sulfur dioxide will all affect the capacitance of the sensor.
实施例1Example 1
本实施例按照下述步骤制备柔性有机薄膜电容传感器：In this embodiment, a flexible organic thin film capacitive sensor is prepared according to the following steps:
1)所用衬底层为PET，采用磁控溅射法制作下电极，在PEt衬底上溅射ITO薄膜；所采用的是ITO陶瓷靶材In2O3∶SnO2＝90∶10wt.％，纯度为99％，溅射前先将PET分别用丙酮，乙醇，去离子水，超声清洗15分钟，制备下电极的方法为磁控溅射，磁控溅射的工作气压为2.5帕斯卡，溅射功率为140瓦，沉积时间为20分钟。1) The substrate layer used is PET, the lower electrode is made by magnetron sputtering, and the ITO film is sputtered on the PET substrate; the ITO ceramic target material In 2 O 3 : SnO 2 =90:10wt.% is used, The purity is 99%. Before sputtering, the PET is cleaned with acetone, ethanol, deionized water, and ultrasonic for 15 minutes. The method of preparing the lower electrode is magnetron sputtering. The working pressure of magnetron sputtering is 2.5 Pascals. The power was 140 watts and the deposition time was 20 minutes.
2)采用旋涂的方法在下电极上制备湿度敏感层，将聚甲基丙烯酸甲酯溶于苯甲醚中(溶液浓度为50毫克/毫升)，旋涂速度为6000转/分，旋涂时间为45秒。2) Prepare a humidity sensitive layer on the lower electrode by spin coating, dissolve polymethyl methacrylate in anisole (solution concentration is 50 mg/ml), spin coating speed is 6000 rpm, spin coating time for 45 seconds.
3)在步骤2)得到的绝湿度敏感层上通过旋涂制备气体敏感层，选择材料为丙基-三甲氧基硅烷，旋涂速度为4500转/分，旋涂时间为30秒。3) Prepare a gas-sensitive layer by spin-coating on the humidity-sensitive layer obtained in step 2). The material is propyl-trimethoxysilane, the spin-coating speed is 4500 rpm, and the spin-coating time is 30 seconds.
4)通过真空热蒸镀的方法制备两个介质层，用掩膜版遮挡，真空度为8×10-3帕斯卡以下，蒸镀速率为0.1埃/秒；4) Prepare two dielectric layers by vacuum thermal evaporation, cover with a mask, the degree of vacuum is below 8×10 -3 Pascal, and the evaporation rate is 0.1 Angstroms/second;
5)通过电子束蒸发的方法制备两个电极，用掩膜版遮挡，电子束蒸发的气压为6×10-3帕斯卡，蒸发速率为0.25埃/秒。5) Two electrodes were prepared by electron beam evaporation, covered with a mask, the pressure of electron beam evaporation was 6×10 −3 Pascal, and the evaporation rate was 0.25 Å/s.
实施例2Example 2
按照与实施例1完全相同的制备方法，仅将步骤2)中的甲基丙烯酸甲酯改为聚酰亚胺，在与上述实施例完全相同的制备条件下得到柔性有机薄膜电容传感器，该传感器的形貌以及器件性能与实施例1相同。According to the same preparation method as in Example 1, only the methyl methacrylate in step 2) is changed to polyimide, and a flexible organic thin film capacitive sensor is obtained under the same preparation conditions as in the above-mentioned embodiment. The morphology and device performance are the same as in Example 1.
实施例3Example 3
按照与实施例1完全相同的制备方法，仅将步骤3)中的丙基-三甲氧基硅烷改为3-二乙基氨丙基-三甲氧基硅烷，在与上述实施例完全相同的制备条件下得到柔性有机薄膜电容传感器，该传感器的形貌以及器件性能与实施例1相同。According to the same preparation method as in Example 1, only the propyl-trimethoxysilane in step 3) was changed to 3-diethylaminopropyl-trimethoxysilane, in the same preparation as in the above-mentioned examples The flexible organic thin film capacitive sensor was obtained under the same conditions, and the morphology and device performance of the sensor were the same as those in Example 1.
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| CN106124576A (en) * | 2016-06-28 | 2016-11-16 | 上海申矽凌微电子科技有限公司 | Integrated humidity sensor and multiple-unit gas sensor and manufacture method thereof |
| CN108700540A (en) * | 2016-02-18 | 2018-10-23 | ams有限公司 | Sensor device for generating measuring signal and method |
| CN109959682A (en) * | 2017-12-26 | 2019-07-02 | 意法半导体有限公司 | Adaptive Test Method and Design for Low Power MOX Sensors |
| CN111801572A (en) * | 2018-03-14 | 2020-10-20 | 希奥检测有限公司 | Monolithic sensor device, method for producing and method for measuring |
| CN112229878A (en) * | 2020-01-07 | 2021-01-15 | 南通大学 | Humidity sensor chip with three-electrode structure |
| CN118518603A (en) * | 2024-07-19 | 2024-08-20 | 宁波大学 | Micro-nano sensing structure and application thereof |
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| CN109959682A (en) * | 2017-12-26 | 2019-07-02 | 意法半导体有限公司 | Adaptive Test Method and Design for Low Power MOX Sensors |
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| CN111801572A (en) * | 2018-03-14 | 2020-10-20 | 希奥检测有限公司 | Monolithic sensor device, method for producing and method for measuring |
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| CN113588727A (en) * | 2020-01-07 | 2021-11-02 | 南通大学 | Humidity sensor chip without storage module |
| CN113588727B (en) * | 2020-01-07 | 2022-04-05 | 南通大学 | Humidity sensor chip without storage module |
| CN112229878B (en) * | 2020-01-07 | 2021-08-10 | 南通大学 | Humidity sensor chip with three-electrode structure |
| CN112229878A (en) * | 2020-01-07 | 2021-01-15 | 南通大学 | Humidity sensor chip with three-electrode structure |
| CN118518603A (en) * | 2024-07-19 | 2024-08-20 | 宁波大学 | Micro-nano sensing structure and application thereof |
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