石墨烯量子點基復(fù)合濕敏膜的制備與特性研究
發(fā)布時間：2018-11-02 09:11
【摘要】：濕度作為環(huán)境監(jiān)測中的重要物理參數(shù),其實時監(jiān)測在氣象勘探、工業(yè)制造、農(nóng)業(yè)種植、智能家居等方面都有著重要的意義。開發(fā)并制備高性能濕敏薄膜與濕度傳感器是實現(xiàn)高精度、實時濕度監(jiān)測重要前提。隨著材料科學(xué)的發(fā)展,許多新型材料受到了科研人員的廣泛關(guān)注。其中,石墨烯量子點作為新型零維材料,在保持了石墨烯眾多優(yōu)良特性的同時,具有量子限域效應(yīng)和邊界效應(yīng),其重要衍生物氧化石墨烯量子點通過在表面修飾大量的親水含氧官能團使其成為一種高性能的濕敏材料。本文以石英晶體微天平(QCM)為傳感器件,制備了聚合物/氧化石墨烯量子點和金屬氧化物/氧化石墨烯量子點復(fù)合膜QCM濕度傳感器,并對復(fù)合敏感薄膜進行了分析表征及濕敏性能測試,對并對其濕敏機理進行分析與模型建立。論文主要內(nèi)容如下:1、采用氣噴工藝QCM器件電極表面制備了聚乙烯亞胺/氧化石墨烯量子點(PEI/GOQDs)和聚乙烯醇/氧化石墨烯量子點(PVA/GOQDs)復(fù)合濕敏薄膜。測試表征并對比分析了PEI與GOQD混合復(fù)合、分層復(fù)合膜相較單一材料薄膜相比的濕敏特性。測試結(jié)果表明,PEI/GOQDs分層濕敏膜的靈敏度為16.59Hz/%RH,濕滯為2.88%RH,最小響應(yīng)時間2s,最小恢復(fù)時間2s,具有良好的濕敏特性。通過透射電鏡、傅立葉變換紅外光譜等表征方法對復(fù)合薄膜進行表征,結(jié)果表明PEI與GOQDs間存在酰胺反應(yīng)鍵合作用。結(jié)合濕敏測試與表征結(jié)果。提出了在低濕、中濕、高濕環(huán)境下的PEI/GOQDs分層薄膜QCM濕度傳感器的濕敏機理,分析了濕滯產(chǎn)生原因。此外,本論文初步探討了不同體積配比PVA/GOQDs復(fù)合薄膜QCM濕度傳感器的濕敏特性,結(jié)果表明當PVA與GOQDs體積比為1:1時在97.3%相對濕度下具有最優(yōu)響應(yīng)1683Hz,其靈敏度為17.92 Hz/%RH,濕滯為2.416667%RH。由紅外光譜證明了PVA與GOQDs存在酯化反應(yīng),并提出濕敏機理、分析濕滯產(chǎn)生原因。2、采用氣噴工藝在QCM器件電極表面沉積氧化鋅(ZnO)種子層,采用水熱法制備ZnO納米棒陣列、ZnO/PEI納米棒陣列、ZnO/PEI/GOQDs納米棒陣列QCM濕度傳感器,對不同結(jié)構(gòu)濕敏薄膜進行表征及濕敏測試,以研究比較其特性。濕敏測試表明,ZnO/PEI/GOQDs納米棒QCM傳感器在97.3%相對濕度下具有最優(yōu)的響應(yīng)值1354Hz,靈敏度為14.89 Hz/%RH。薄膜形貌表征表明,ZnO/PEI/GOQDs三元復(fù)合的納米棒結(jié)構(gòu)更致密,直徑分布均勻,且納米棒上覆蓋有PEI薄膜。通過紅外光譜可以推測PEI與GOQDs附生長在ZnO納米棒上。通過分析濕敏表征與測試結(jié)果,復(fù)合薄膜的濕敏性能增益可歸因于附生長在ZnO納米棒上的PEI與GOQDs提供了更多的水分子吸附點位,同時提出了低濕、中濕、高濕環(huán)境下的ZnO/PEI/GOQDs納米棒陣列薄膜QCM濕度傳感器的濕敏機理,分析了濕滯產(chǎn)生的原因。
[Abstract]:Humidity as an important physical parameter in environmental monitoring, its real-time monitoring is of great significance in meteorological exploration, industrial manufacturing, agricultural planting, intelligent home and so on. Developing and fabricating high performance humidity sensitive film and humidity sensor is an important prerequisite to realize high precision and real time humidity monitoring. With the development of material science, many new materials are paid more and more attention by researchers. As a new zero-dimensional material, graphene quantum dots (QDs) have quantum limiting and boundary effects while maintaining many excellent properties of graphene. Its important derivative graphene oxide quantum dots (QDs) become a high performance humidity sensitive material by modifying a large number of hydrophilic oxygen-containing functional groups on the surface. In this paper, QCM humidity sensors with polymer / graphene oxide quantum dots and metal oxide / graphene oxide quantum dots composite films were fabricated using quartz crystal microbalance (QCM) as sensing device. The composite sensitive film was characterized and its humidity sensitivity was tested. The mechanism of humidity sensitivity was analyzed and the model was established. The main contents of this thesis are as follows: 1. Poly (ethylene imide / graphene oxide) quantum dots (PEI/GOQDs) and polyvinyl alcohol / graphene oxide (PVA/GOQDs) composite humidity sensitive films were prepared on the electrode surface of QCM devices by gas jet technology. The humidity sensitivity of PEI / GOQD composite film was compared with that of single material film. The results show that the sensitivity of the PEI/GOQDs layered humidity sensitive film is 16.59 Hz / r, the humidity lag is 2.88 RH, the minimum response time is 2 s and the minimum recovery time is 2 s. The composite films were characterized by transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR). The results showed that there was amide-bond cooperation between PEI and GOQDs. Combined with the results of humidity sensitivity test and characterization. The humidity sensing mechanism of PEI/GOQDs layered film QCM humidity sensor under low, medium and high humidity conditions is proposed, and the causes of moisture lag are analyzed. In addition, the humidity sensitivity of PVA/GOQDs composite film QCM humidity sensor with different volume ratio is discussed. The results show that when the volume ratio of PVA to GOQDs is 1:1, the optimal response is 1683 Hz at 97.3% relative humidity. The sensitivity is 17.92 Hz/%RH, and the humidity lag is 2.416667RH. The esterification reaction between PVA and GOQDs was proved by infrared spectroscopy, and the mechanism of humidity sensitivity was put forward, and the reason of wet hysteresis was analyzed. 2. QCM nanorods array was prepared by hydrothermal method by gas jet deposition of ZnO (ZnO) seed layer on the surface of QCM device electrode. ZnO/PEI nanorod array and ZnO/PEI/GOQDs nanorod array QCM humidity sensor were used to characterize the humidity sensitive films with different structures and to study and compare their characteristics. The humidity sensitivity test shows that the ZnO/PEI/GOQDs nanorod QCM sensor has the best response value of 1354 Hz at 97.3% relative humidity, and the sensitivity is 14.89 Hz/%RH.. The morphology of the films shows that the nanorods with ZnO/PEI/GOQDs ternary composites have more compact structure and uniform diameter distribution, and the nanorods are covered with PEI thin films. It is inferred by IR spectra that PEI and GOQDs are attached to ZnO nanorods. Through the analysis of the results of hygroscopic characterization and measurement, the gain of the humidity sensitivity of the composite film can be attributed to the fact that the PEI and GOQDs attached to the ZnO nanorods provide more adsorption sites for water molecules. At the same time, the low humidity and moderate humidity are proposed. The humidity sensing mechanism of ZnO/PEI/GOQDs nanorod array thin film QCM humidity sensor in high humidity environment was analyzed.
【學(xué)位授予單位】：電子科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TB383.2;TH765.51
本文編號：2305591
[Abstract]:Humidity as an important physical parameter in environmental monitoring, its real-time monitoring is of great significance in meteorological exploration, industrial manufacturing, agricultural planting, intelligent home and so on. Developing and fabricating high performance humidity sensitive film and humidity sensor is an important prerequisite to realize high precision and real time humidity monitoring. With the development of material science, many new materials are paid more and more attention by researchers. As a new zero-dimensional material, graphene quantum dots (QDs) have quantum limiting and boundary effects while maintaining many excellent properties of graphene. Its important derivative graphene oxide quantum dots (QDs) become a high performance humidity sensitive material by modifying a large number of hydrophilic oxygen-containing functional groups on the surface. In this paper, QCM humidity sensors with polymer / graphene oxide quantum dots and metal oxide / graphene oxide quantum dots composite films were fabricated using quartz crystal microbalance (QCM) as sensing device. The composite sensitive film was characterized and its humidity sensitivity was tested. The mechanism of humidity sensitivity was analyzed and the model was established. The main contents of this thesis are as follows: 1. Poly (ethylene imide / graphene oxide) quantum dots (PEI/GOQDs) and polyvinyl alcohol / graphene oxide (PVA/GOQDs) composite humidity sensitive films were prepared on the electrode surface of QCM devices by gas jet technology. The humidity sensitivity of PEI / GOQD composite film was compared with that of single material film. The results show that the sensitivity of the PEI/GOQDs layered humidity sensitive film is 16.59 Hz / r, the humidity lag is 2.88 RH, the minimum response time is 2 s and the minimum recovery time is 2 s. The composite films were characterized by transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR). The results showed that there was amide-bond cooperation between PEI and GOQDs. Combined with the results of humidity sensitivity test and characterization. The humidity sensing mechanism of PEI/GOQDs layered film QCM humidity sensor under low, medium and high humidity conditions is proposed, and the causes of moisture lag are analyzed. In addition, the humidity sensitivity of PVA/GOQDs composite film QCM humidity sensor with different volume ratio is discussed. The results show that when the volume ratio of PVA to GOQDs is 1:1, the optimal response is 1683 Hz at 97.3% relative humidity. The sensitivity is 17.92 Hz/%RH, and the humidity lag is 2.416667RH. The esterification reaction between PVA and GOQDs was proved by infrared spectroscopy, and the mechanism of humidity sensitivity was put forward, and the reason of wet hysteresis was analyzed. 2. QCM nanorods array was prepared by hydrothermal method by gas jet deposition of ZnO (ZnO) seed layer on the surface of QCM device electrode. ZnO/PEI nanorod array and ZnO/PEI/GOQDs nanorod array QCM humidity sensor were used to characterize the humidity sensitive films with different structures and to study and compare their characteristics. The humidity sensitivity test shows that the ZnO/PEI/GOQDs nanorod QCM sensor has the best response value of 1354 Hz at 97.3% relative humidity, and the sensitivity is 14.89 Hz/%RH.. The morphology of the films shows that the nanorods with ZnO/PEI/GOQDs ternary composites have more compact structure and uniform diameter distribution, and the nanorods are covered with PEI thin films. It is inferred by IR spectra that PEI and GOQDs are attached to ZnO nanorods. Through the analysis of the results of hygroscopic characterization and measurement, the gain of the humidity sensitivity of the composite film can be attributed to the fact that the PEI and GOQDs attached to the ZnO nanorods provide more adsorption sites for water molecules. At the same time, the low humidity and moderate humidity are proposed. The humidity sensing mechanism of ZnO/PEI/GOQDs nanorod array thin film QCM humidity sensor in high humidity environment was analyzed.
【學(xué)位授予單位】：電子科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TB383.2;TH765.51
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