Dataset for Insulator material deposited with Molybdenum disulphide prospective for sensing application
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The primary target of molybdenum disulfide (MoS2) crystal 99.995 % with a size of about 0.5 cm × 1.0 cm × 0.2 mm and a density of 5.06 g/cm3 at 15 °C has been purchased from Sigma Aldrich. The deposition of the adopted insulators occurred in a vacuum of about 7.6·10-3 mbar inside a vacuum chamber. A Q-switching Nd: YAG laser operating at a wavelength of 1064 nm, a pulse duration of 5 ns, was used at a repetition rate of 10 Hz and 30 minutes of irradiation time. The laser beam passed through a 50 cm lens to focus the beam to a diameter of 0.5 mm on a solid target of MoS2 placed in a rotating carrousel to avoid deep ablation which could modify the laser density. A fresh target surface was always exposed to the incident laser light. The distance between the window of incoming laser and the target is of 22 cm. The volume of the vacuum chamber is about 52 liters. The energy of the laser pulse was 600 mJ and the laser incidence angle was 45° on the surface of the target corresponding to a laser fluence of about 76 J/cm2. When the laser fluence overcame the ablation threshold of the MoS2, ions, besides other particles, atoms, and clusters, were ejected. A Tencor P-10 has been employed as a surface profiler to measure the crater size and shape formed on the surface of the MoS2 after one laser shot to evaluate the amount of removed material during the laser irradiation. A mass quadrupole spectrometer QMG F3 220 PrismaPlus (MQS) from Pfeiffer Vacuum was used to detect the emitted atoms and molecules from the laser ablation of a target of MoS2 in vacuum. Typically, the spectrometer detects the emission of the gas produced in the vacuum chamber. This spectrometer detects masses ranging between 1amu and 300 amu, with a sensitivity lower than 1 ppm and a mass resolution better than 1 amu. The MQS is equipped with a SEM detector with a power supply of 1100 V. The masses of interest have been selected as follows: 18 (H2O), 32 (S), 48 (SO), 64 (S2), 96 (Mo), 112 (MoO), 128 (MoS), 160 (MoS2) amu. The MQS detects the emitted atoms and molecules as a function of the time at the laser switching on and 1 Hz laser repetition rate. The Attenuated Total Reflectance – Fourier Transform Infrared (ATR-FTIR) spectroscopy using a Jasco 4700 and UV-VIS spectroscopy by means a Jasco V750 spectrophotometers, have been employed to analyze the alteration of the presence of specific functional groups, the changes of the chemical structure and of the optical transmittance in the polymer after the deposition of MoS2. The control of the quality of the deposited MoS2 has been explored by Atomic Force Microscope (AFM) analysis. The accomplishment of the surface average roughness (Ra) and the mean roughness parameter (RMS) was performed using a Dimension ICON- Bruker Corp. has been used. The 3D images with scan size of 1 mm have been captured using an exposure time of 1s, and processed by NanoScope Analysis software. The monitoring of the electrical capacitance alteration was performed by the I–V characteristic curve through frequency dependence measurements of the output voltage of a high-pass filter at the constant current of 0.5 mA for pristine samples and 0.1 mA . A metallic mask containing two stripes at distance of 1 mm each other and width of 10 mm was used to assist the production of two gold electrodes 50 nm thick sputtered on the composite surface. The resistivity of the used resistor was 1 MW. The voltage response was recorded over frequencies ranging between 20kHz and 100 kHz. The alternating current (AC) with sinusoidal waveform was generated using a Keithley 6221 current source. The AC voltage vs frequency was monitored by a Tektronix TDS5104B. oscilloscope. Commercial ceramic capacitor of 2.6 pF. 6.8 pF and 12 pF have been used to display the corresponding voltage frequency. In the experimental configuration shown in Figure 2 the prepared composite or the used commercial ceramic capacitor are alternatively positioned.
本实验所用的二硫化钼(MoS₂)晶体靶材纯度为99.995%,尺寸约为0.5 cm × 1.0 cm × 0.2 mm,15 ℃下的密度为5.06 g/cm³,购自Sigma Aldrich公司。 本实验的绝缘层沉积过程于真空腔室内完成,腔室真空度约为7.6×10⁻³ mbar。实验采用调Q Nd:YAG激光器,其工作波长为1064 nm,脉冲宽度5 ns,重复频率10 Hz,辐照时长30分钟。激光束经焦距50 cm的透镜聚焦,在置于旋转载物台的MoS₂固体靶材表面形成直径0.5 mm的光斑,此举可避免因过度烧蚀改变激光能量密度。实验中始终保持新鲜的靶材表面正对入射激光。 激光入射窗口与靶材之间的距离为22 cm,真空腔室体积约为52 L。单脉冲激光能量为600 mJ,靶面激光入射角为45°,对应激光通量约为76 J/cm²。当激光通量超过MoS₂的烧蚀阈值时,除其他粒子外,离子、原子与团簇均会被溅射出来。 采用Tencor P-10型表面轮廓仪测量单次激光辐照后MoS₂靶面形成的凹坑尺寸与形貌,以评估激光辐照过程中被移除的材料量。 采用普发真空(Pfeiffer Vacuum)生产的QMG F3 220 PrismaPlus型四极杆质谱仪(MQS),用于检测真空环境下MoS₂靶材激光烧蚀产生的溅射原子与分子。该质谱仪通常用于检测真空腔室内产生的气体组分,其可检测的质量范围为1 amu至300 amu,灵敏度低于1 ppm,质量分辨率优于1 amu。MQS配备工作电压为1100 V的SEM探测器。本实验选定的待检测质量数如下:18(H₂O)、32(S)、48(SO)、64(S₂)、96(Mo)、112(MoO)、128(MoS)、160(MoS₂) amu。实验中以激光触发时刻为时间零点,在1 Hz重复频率下,MQS实时检测溅射原子与分子的信号随时间的变化。 采用Jasco 4700型衰减全反射-傅里叶变换红外(ATR-FTIR)光谱仪与Jasco V750型紫外-可见(UV-VIS)分光光度计,分别分析MoS₂沉积后聚合物基底中特定官能团的存在变化、化学结构演变以及光学透过率的改变。 采用原子力显微镜(AFM)表征沉积得到的MoS₂薄膜质量。实验使用布鲁克(Bruker Corp.)Dimension ICON型原子力显微镜,测量样品的表面平均粗糙度(Ra)与均方根粗糙度(RMS)参数。扫描尺寸为1 mm的三维表面形貌图像以1 s的曝光时间采集,并通过NanoScope Analysis软件进行后期处理。 通过恒流下高通滤波器输出电压的频率依赖性测量结合I-V特性曲线,实现对电容变化的监测:原始样品采用0.5 mA恒流,改性样品采用0.1 mA恒流。实验使用带有两条间距1 mm、宽度10 mm条纹的金属掩模板,辅助在复合薄膜表面溅射制备厚度为50 nm的双金电极。所用电阻的阻值为1 MΩ。电压响应信号的采集频率范围为20 kHz至100 kHz。 采用Keithley 6221型电流源产生正弦波形交流电。使用泰克(Tektronix)TDS5104B型示波器监测交流电压随频率的变化。实验使用标称容量分别为2.6 pF、6.8 pF与12 pF的商用陶瓷电容器,用于展示对应的电压频率特性。在图2所示的实验配置中,待测复合薄膜与商用陶瓷电容器可交替置于测试回路中。



