摘要
采用水浴加热法合成CuO微米颗粒,并用Au、Ag和Cr元素进行掺杂。通过扫描电镜和X射线衍射仪对产物的形貌及组成进行表征,并将合成的粉体制成敏感膜,采用静态配气法对产物气敏性能进行研究。实验结果表明:制备合成的CuO颗粒呈微米片聚合成的橄榄或捧花状,尺寸范围在2μm~3μm;所有样品的XRD图谱与标准卡片一致;微米CuO的气敏性能随着测试温度的降低而提高。气敏测试表明:掺杂1.25 wt%Au的CuO对10×10~(-6)的H_2S气敏性能最好,最佳工作温度降低至40℃,响应值达到128,具有良好的选择性;此外,该传感器的最低检测下限达到100×10~(-9),具有较好的重复性和长期稳定性,有望制备出低功耗H_2S气体传感器。
CuO microparticles were synthesized by water-bath heating and doped with elements of Au,Ag and Cr.The morphology and composition of the product were characterized by scanning electron microscopy and X-ray diffractometry. The synthesized powder was made into a sensitive film. The gas-sensitivity of the product was investigated by static gas distribution method. The experimental results show that the prepared CuO particles are in the form of olives or bouquets of micro-sheets,ranging in size from 2 to 3 μm. The XRD patterns of all samples are the same as those of the standard cards. The gas sensitivity of micro CuO increases as the test temperature decreases. Gas sensitivity tests show that CuO doped with 1.25 wt% Au has the best gas sensitivity and good selectivity to 10×10-6 H2 S. The best operating temperature is reduced to 40 ℃,at the same time the sensitivity reaches 103. In addition,the detected limition of the sensor is 100×10-9,and it has good repeatability and long-term stability. It is expected to produce a low-power H2 S gas sensor.
引文
[1] 胡校兵,谢祯芳,谢骥,等.水热法合成微纳米CuO及在气体传感器中的应用[J].郑州大学学报,2016,37(6):10-14.
[2] 陈诚,姚晓婷,朱永恒,等.亚微米级花状氧化铜粉体的制备及其气敏性能[J].中国粉体技术,2014,20(4):17-27.
[3] 李元,李庆,吴会杰,等.化学水浴法制备CuS纳米花状球及其光学性能研究[J].功能材料,2013,3(44):317-321.
[4] Wei D D,Jiang W H,Gao H G,et al.Facile Synthesis of La-Doped In2O3 Hollow Microspheres and Enhanced Hydrogen Sulfide Sensing Characteristics[J].Sens Actuators B,2018,276:413-420.
[5] Bai S L,Zhang K W,Sun J H,et al.Polythiophene-WO3 Hybrid Architectures for Low-Temperature H2S Detection[J].Sens Actuators B,2014,197:142-148.
[6] Nagarajan V,Chandiramouli R,DFT Studies on Interaction of H2S Gas with α-Fe2O3 Nanostructures[J].Inorg Organomet Polymer,2016,26:394-404.
[7] Kim H,Jin C,Park S,et al.H2S Gas Sensing Properties of Bare and Pd-Functionalized CuO Nanorods[J].Sens Actuators B,2012,161:594-599.
[8] Ramgir N S,Kailasa Ganapathi S,Kaur M,et al.Sub-ppm H2S Sensing at Room Temperature Using CuO Thin Films[J].Sens Actuators B,2010,151:90-96.
[9] Niu X S,Cui T L,Lu X,et al.Synthesis of WO3 Materials with Interwoven Network Structures for High-Performance Sensors[J].Micro Nano Lett,2012,7:41-44.
[10] Guo L L,Xie N,Wang C,et al.Enhanced Hydrogen Sulfide Sensing Properties of Pt-Functionalized α-Fe2O3 Nanowires Prepared by One-Step Electrospinning[J].Sens Actuators B,2018,255:1015-1023.
[11] Hu X B,Zhu Z G,Chen C,et al.Highly Sensitive H2S Gas Sensors Based on Pd-Doped CuO Nanoflowers with Low Operating Temperature[J].Sens Actuators B,2017,253:809-817.
[12] Hu X B,Zhu Z G,Li Z H,et al.Heterostructure of CuO Microspheres Modified with CuFe2O4 Nanoparticles for Highly Sensitive H2S Gas Sensor[J].Sens Actuators B,2018,264:139-149.
[13] Petr Vomka,Václav ?tengl,Ji Henych,et al.Shape-Controlled Synthesis of Sn-Doped CuO Nanoparticles for Catalytic Degradation of Rhodamine B[J].Colloid Interface Sci,2016,481:28-38.
[14] Dhakshinamoorthy J,Pullithadathil B.New Insights Towards Electron Transport Mechanism of Highly Efficient p-Type CuO(111)Nanocuboids-Based H2S Gas Sensor[J].Phys,Chem C,2016,120:4087-4096.
[15] Liu X H,Zhang J,Kang Y F,et al.Brochantite Tabular Microspindles and Their Conversion to Wormlike CuO Structures for Gas Sensing[J].Cryst EngComm,2012,14:620-625.
[16] Wang Y F,Qu F D,Liu J,et al.Enhanced H2S Sensing Characteristics of CuO-NiO Core-Shellmicrospheres Sensors[J].Sens Actuators B,2015,209:515-523.