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为探究所设计的微结构图案的共振机制,图2(a)展示了器件在不覆盖石墨烯时(命名为Dev.2,也即金属结构阵列)THz透射谱的实验和仿真结果。实验结果(图2(a)红线)表明器件在研究的频段内存在两个共振谷,分别在f=0.32 THz处(记为DA)和f=0.82 THz处(记为DB)。两个谷中间形成一个透射峰(记为P),其频率为f=0.56 THz。器件在该频段的仿真谱线特征(见图2(a)黑线)与实验谱线的共振频率点吻合较好(仿真谱线中DA频率f=0.35 THz,DB频率f=0.82 THz,峰P频率f=0.57 THz),但幅值和线型上仍存在差异,这可能是制备过程中不可避免的误差以及仿真条件和真实情况间的差异导致。在仿真中共振谷的电场分布如图2(b)~(c)所示。图2(b)显示,在水平相对的金属框两边存在明显的电场分布,表明共振谷DA主要源于SPP在边框处产生的偶极子共振。图2(c)显示,DB处的电场主要分布在水平“干”字形金属顶端,说明该共振谷同样由偶极子共振诱导,只是与DA处的电场分布不同。而透射峰P正是源于DA和DB对应的两种偶极子共振模式的耦合。
图 2 (a)器件Dev.2的THz透射谱,红线为实验结果,黑线为仿真结果;(b) f=0.35 THz (共振谷DA)处的仿真电场分布;(c) f=0.82 THz (共振谷DB)处的仿真电场分布,红色代表电场强度最大值,蓝色代表电场强度最小值
Figure 2. (a) THz transmission spectra for the Dev.2, where the red line indicates the experimental result and the black one indicates the simulated result; the simulated electric field distribution for (b) f=0.35 THz (the resonant dip DA) and (c) f=0.82 THz (the resonant dip DB), where the red color represents the maximum electric field intensity, and the blue one represents the minimum electric field intensity
上述结果表明微结构表面存在强局域电场。强局域电场易于受到周围环境细微变化的影响,使器件电磁特性发生改变,最终反映到THz透射谱中,这为物质的高灵敏传感提供了良好平台。因此,接下来将探究器件对样品的传感特性。图1(c)和图1(d)分别展示了传感器的工作示意图和滴加有谷氨酸样品的传感器光学显微镜图像。图3(a)展示了实验中不同谷氨酸浓度下器件Dev.1的THz透射谱。可以看到,覆盖有石墨烯的器件Dev.1和未覆盖石墨烯的器件Dev.2具有非常相似的透射谱,仍存在两个透射谷(仍被分别记为DA和DB)和一个透射峰(仍被记为P)。随着谷氨酸浓度的增加,DA的变化没有规律性,DB虽然在透射幅值上展现了先增加后减小的变化,但并不明显。然而对于透射峰P,随着谷氨酸浓度从C0增加到C3,峰P幅值明显上升;当浓度进一步增加时,峰P幅值转而下降,且变化明显。这表明可以利用峰P的幅值作为传感指标来检测谷氨酸溶液浓度。为了定量表征器件的透射幅值对谷氨酸溶液浓度的传感性能,定义参量${\Delta }{T}{=}{{T}}_{{{C}}_{{i}}}{-}{{T}}_{{{C}}_{\text{0}}} $ 。其中,$ {{T}}_{{{C}}_{{i}}} $($ {{T}}_{{{C}}_{\text{0}}} $)为滴加有Ci (C0)浓度溶液的传感器对某一频率THz波的透射率。图3(d)为器件Dev.1峰P处的$ {\Delta }{T} $随溶液浓度的变化曲线。可以看到,${\Delta }{T} $随着浓度的变化先增加后减小:当浓度为C1时,$ {\Delta }{T} $相较于C0轻微增加;当浓度从C1增至C2时,${\Delta }{T} $变化最为明显,从1.85迅速增长到17.28;在C3浓度下$ {\Delta }{T} $达到最高值,随后单调递减。这一结果表明透射波对不同浓度谷氨酸溶液产生了响应,Dev.1在仅基于$ {\Delta }{T} $单一检测指标时能够对C0~C3浓度的谷氨酸溶液实现检测,并且对C2浓度的检测最为灵敏,检测浓度极限已低至 10−1 fg/mL 量级。据笔者所知,该结果要优于目前其他太赫兹超材料氨基酸传感器(见表1)。
图 3 (a)器件Dev.1、(b)器件Dev.2、(c)器件Dev.3在不同谷氨酸浓度下的THz透射谱;(d)器件Dev.1在共振峰P处、(e)器件Dev.2在共振峰P处、(f)器件Dev.3 在f=0.58 THz处的$ {\Delta }{T} $随浓度的变化
Figure 3. Transmission spectra for (a) Dev.1, (b) Dev.2, and (c) Dev.3 covered by glutamaic acid solution with the concentration of C0-C6; $ \Delta T $ as a function of the solution concentration for (d) Dev.1, (e) Dev.2 at the resonant peak P, and (f) Dev.3 at f=0.58 THz
表 1 与已报道的太赫兹超材料氨基酸传感器的比较
Table 1. Comparison with reported THz amino acid sensors
为证明传感器的高灵敏度检测源于石墨烯与超结构的共同作用,还开展了两组对照实验,探究了仅有超结构、未覆盖石墨烯的器件Dev.2和仅覆盖石墨烯、没有超结构的器件(记为Dev.3)在不同谷氨酸浓度下的THz透射特性。从图3(b)可以看到,Dev.2的共振谷DA、DB及峰P的透射幅值随浓度变化微弱。图3 (e)表明,虽然Dev.2的$ {\Delta }{T} $在C1浓度也具有数值,实现了10−1 fg/mL量级谷氨酸溶液的检测,但远逊于Dev.1在C2浓度附近的检测灵敏性;$ {\Delta }{T} $在C3浓度发生转折,意味着在该指标下器件仅能对C0~C3浓度的样品进行检测。对于纯石墨烯构成的器件Dev.3,不同浓度下的透射谱(已做归一化处理)在图3(c)中给出。可以看到,器件在0.2~0.3 THz范围内具有较为明显的透射峰,但由于实验所用时域光谱仪在该频段内探测结果不准确,故不予考虑。而在0.3 THz以上的频段,不同浓度下透射谱幅值变化没有规律,并且图3(f)显示器件在0.58 THz处的$ {\Delta }{T} $随谷氨酸浓度变化均在9以下。因此,Dev.3也不具备较好的传感能力。
可以看到,借助透射峰幅值随样品浓度的变化,Dev.1相比于Dev.2或Dev.3对谷氨酸溶液确实具有更为灵敏的传感能力,其内在机理可以利用石墨烯能带结构(见图4)结合超结构内电偶极子共振诱导的强局域电场来解释。石墨烯的费米能级EF与载流子浓度之间满足关系:$\left|\text{Δ}{{E}}_{\text{F}}\right|{=}\hbar v_{\mathrm{F}} {\text{(π}{n}\text{)}}^{\text{1/2}}$,其中$\text{Δ}{{E}}_{\text{F}}$是EF与Dirac点的能量差,$\hbar$是约化普朗克常量,${{v}}_{{F}}$是费米速度,n是载流子浓度[20]。实验采用p掺杂石墨烯,EF通常偏离Dirac点,处在价带中(见图4状态①)[15]。根据上述公式,此时石墨烯载流子浓度较高,导电性较好。较高的载流子浓度增强了THz波的损耗,因此器件在C0浓度下的透射幅值较低;随着谷氨酸溶液浓度的增加,掺杂作用使EF上移靠近Dirac点,特别地,当到达C2浓度时,EF非常靠近Dirac点(见图4状态②),此时载流子浓度变化明显,电导率迅速下降,极大减弱了入射THz波的损耗,因此透射幅值大幅增加。不仅如此,载流子浓度的显著变化所导致的器件表面电磁环境的变化可以通过耦合作用被超结构中的强局域电场捕捉,并被反映到太赫兹透射谱线中。正是石墨烯与人工微结构的共同作用才使Dev.1在C2浓度附近具有极高的检测灵敏度。而当溶液浓度继续增加,EF会经过(见图4状态③)并远离(见图4状态④)Dirac点,向导带移动,石墨烯电导率缓慢回增,使器件透射幅值再次降低。
图 4 石墨烯能带中费米能级EF随溶液浓度的演化
Figure 4. The evolution of EF in graphene energy band with the increasing solution concentration
虽然Dev.1能以透射峰幅值作为传感指标实现对10−1 fg/mL量级浓度谷氨酸溶液的检测,但是EF跨越Dirac点导致的透射幅值先递增后递减会使$ {\Delta } T$出现交叠区域,这无疑将影响溶液浓度的判断。因此,需要探寻其他传感指标,与透射峰幅值互为补充,更好地对溶液浓度进行检测。除了透射谱的幅值,相位作为THz波的另一个重要特征参数,也可以作为谷氨酸浓度的检测指标。不同浓度下三种器件的相位差$ \text{Δ}{P}\text{(}{f}\text{)} $($ \text{Δ}{P}\text{(}{f}\text{)=}{{P}}_{{{C}}_{{i}}}\text{(}{f}{)-}{{P}}_{{{C}}_{\text{0}}}\text{(}{f}\text{)} $),其中,$ {{P}}_{{{C}}_{{i}}}\text{(}{f}\text{)} $为Ci浓度下传感器的透射波相位谱,$ {{P}}_{{{C}}_{\text{0}}}\text{(}{f}\text{)} $为C0浓度下传感器的透过波相位谱)在图5(a)~(c)中被给出。图5(a)显示在研究的频段内,器件Dev.1在所有浓度下的$ \text{Δ}{P}\text{(}{f}\text{)} $与频率都呈准线性关系。因此,通过线性拟合提取函数$ \text{Δ}{P}\text{(}{f}\text{)} $的斜率,建立斜率与溶液浓度的关系,也是检测谷氨酸浓度的一种方法。图5(d)就展示了从器件Dev.1的$ \text{Δ}{P}\text{(}{f}\text{)} $中提取出来的斜率与浓度的关系。可以看到,在C5浓度之前,斜率与浓度具有类线性关联,并且从C2增加到C3时,斜率变化最为明显,而当浓度增至C6时,斜率有所下降。这表明器件Dev.1的相位差也能灵敏检测出谷氨酸溶液在低浓度下的变化,因此可以作为传感指标。结合透射峰幅值和相位差两维信息的交叉印证,Dev.1能够实现对C0~C5浓度谷氨酸溶液的准确检测。对于Dev.2,虽然$ \text{Δ}{P}\text{(}{f}\text{)} $与频率呈准线性变化(见图5(b)),但获取的斜率随浓度先减小后增大,最后几乎不变(见图5(e)),相较于Dev.1缺少线性特征,这意味着Dev.2无法通过相位差和透射幅值的相互支撑实现C0~C5浓度的检测。图5(c)和图5(f)显示Dev.3在各浓度下的$ \text{Δ}{P}\text{(}{f}\text{)} $与频率也呈准线性相关,并在C5浓度以前展现了良好的单调递减趋势,表明若仅依靠相位差斜率这一指标,Dev.3可展现良好的传感性,但是振荡的$ {\Delta }T $ (参见图3(f))无法协同器件实现多维传感,降低了检测的稳定性。
图 5 (a)器件Dev.1、(b)器件Dev.2、(c)器件Dev.3在不同谷氨酸浓度下的${ \Delta }{P} $ 谱:(d)器件Dev.1、(e)器件Dev.2、(f)器件Dev.3从$ { \Delta P}{} $ 谱中提取出的斜率和浓度的关系
Figure 5. $ \Delta P $ spectra for (a) Dev.1, (b) Dev.2, and (c) Dev.3 covered by the glutamic acid solution with the concentration of C0-C6; the slope extracted from $ \Delta P $ spectra as a function of the solution concentration for (d) Dev.1, (e) Dev.2, and (f) Dev.3
Graphene-composite metamaterials-based multi-dimensional ultra-sensitive glutamic acid sensor
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摘要: 提出一种石墨烯-金属超材料复合太赫兹传感器,充分利用石墨烯能带Dirac点附近费米能级对样品的灵敏响应结合超材料表面强局域电场实现了对谷氨酸溶液浓度的多维超灵敏传感。实验结果表明,传感器在频率f =0.58 THz处存在一个明显的透射峰,且该透射峰幅值随谷氨酸溶液浓度的增加先升高后降低。若以透射峰幅值作为传感指标,器件能够探测到的最低浓度在10−1 fg/mL量级。另外,从传感器的透射波相位差-频率关系曲线中提取的斜率与浓度具有类线性关联,这意味着相位差信息也可以作为有效的传感指标。结合透射幅值和相位差两个传感指标,器件可以实现对谷氨酸溶液浓度的超灵敏精确检测。文中提出的器件为发展基于太赫兹超材料的超灵敏氨基酸传感器提供了帮助。Abstract:
Objective The pursuit of ultra-sensitive amino acid sensors is of great significance for biomedicine and chemical industry. Due to their low energy, high permeability, and fingerprint, terahertz (THz, 1 THz = 1012 Hz) waves are excellent candidates for the nondestructive detection of biochemical substances or molecules. For metamaterials, the strong local electric field generated by surface plasmon polariton is conducive to reflect the subtle changes of the surrounding environment into the THz signal spectrum, which provides an excellent platform for the development of ultra-sensitive, nondestructive, and unlabeled amino acid sensors. Up to now, however, few researches have been reported on amino acid sensors based on THz metamaterial. Therefore, the development of ultra-sensitive sensors that can detect amino acid solutions with low concentrations is an important subject in the realm of THz functional devices. Methods Taking full advantage of the sensitive response of the Fermi level (EF) around the Dirac point in the graphene energy band to the sample in conjugation with the electric field strongly confined on the surface of the metamaterial, a terahertz sensor composed of graphene and metal metamaterial is proposed to realize the multi-dimensional ultra-sensitive sensing for glutamic acid. The designed sensor (denoted Dev.1) consists of a SiO2 substrate, polyimide (PI), metal arrays, and single-layer graphene. The detailed structure parameters of each metal pattern are as follows: L1=180 μm, L2=150 μm, a=20 μm, b=5 μm, c=14 μm, d=5 μm, e=18.5 μm, f=30 μm (Fig.1). The thickness of the unit cell, PI, and the substrate are 0.2 μm, 8 μm, and 300 μm, respectively. THz transmission spectra of the sensors are measured by THz-time domain spectrometer, and glutamic acid solutions with seven different concentrations are prepared: C0=0 fg/mL, C1=1.25$ \times $10−1 fg/mL, C2=2.50$ \times $10−1 fg/mL, C3=1.08$ \times $101 fg/mL, C4=4.32$ \times $102 fg/mL, C5=3.63$ \times $105 fg/mL, C6=1.03$ \times $1012 fg/mL. The simulation part is implemented by the time domain solver. Results and Discussions For Dev.1, there is a significant resonant peak at f = 0.58 THz in the transmission spectra, which is attributed to the coupling between two groups of electrical dipole resonance modes (Fig.2(b)-(c), Fig.3). More importantly, the peak amplitude first increases and then decreases with the rising solution concentration. It means that taking $ {\Delta }{T} $ ($ {\Delta }{T}{=}{{T}}_{{{C}}_{{i}}}{-}{{T}}_{{{C}}_{{0}}} $, where $ {{T}}_{{{C}}_{{i}}} $($ {{T}}_{{{C}}_{{0}}} $) is transmittance for the sensor covered by Ci (C0) glutamic acid solution) as the sensing indicator, the proposed sensor can detect the minimum value in the order of 10−1 fg/mL. Such ultrasensitivity can be rationalized by the ultra-sensitive response of EF around Dirac point to the surrounding environment (Fig.4) in conjugation with the confined field induced by electrical dipole induced. In addition, one can find that the slope extracted from ΔP(f) ($ {Δ}{P}{(}{f}{)=}{{P}}_{{{C}}_{{i}}}{(}{f}{)-}{{P}}_{{{C}}_{{0}}}{(}{f}{)} $, where $ {{P}}_{{{C}}_{{i}}}{(}{f}{)} $ ($ {{P}}_{{{C}}_{{0}}}{(}{f}{)} $) is the phase of transmitted THz for the sensor covered by Ci (C0) glutamic acid solution vs frequency also exhibits quasi-linear dependence on Ci, and holds monotonically increasing within the range C0-C5 (Fig.5). It demonstrates that the slope related to phase difference can be cross-verified with ∆T to realize multi-dimensional and ultra-sensitive detection of glutamic acid solution with the concentration of C0-C5. Conclusions A multi-dimensional ultra-sensitive THz sensor composed of graphene and metal metamaterials is proposed for the detection of glutamic acid concentration. The experimental results show that there is a transmission peak at 0.58 THz in the THz transmission spectra, which originates from the coupling between two modes of electrical dipoles. With the increase of glutamic acid concentration, the transmission peak amplitude increases first and then decreases. Taking the peak amplitude as the sensing indicator, the limit of detection for the sensor can be as low as the order of 10−1 fg/mL. The strong confined electric field on the surface of the metamaterial together with the sensitive response of the EF in the graphene energy band to different solution concentrations causes significant changes in the electromagnetic properties of the device and the corresponding transmitted THz wave, which is the main reason for the ultra-sensitive sensing characteristics for the composite device. In addition, the effect of glutamic acid solution concentration on the phase of transmitted THz wave was also studied. The results show that the slope extracted from phase difference-frequency curves has a quasi-linear relationship with the concentration from C0 to C5. Therefore, it can also be utilized as an indicator to detect the concentration of the glutamic acid solution with 10−1 fg/mL. This work has contributed to the development of THz metamaterials in amino acid sensors. -
Key words:
- terahertz metamaterials /
- sensors /
- graphene /
- multi-dimension and ultra-sensitivity
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图 1 (a)光学显微镜下制备的金属结构阵列(未铺石墨烯);(b)金属阵列结构单元示意图;(c)传感器工作示意图;(d)光学显微镜下滴加谷氨酸的传感器
Figure 1. (a) Microscopic image of the fabricated metal array (without graphene); (b) Schematic of the unit cell of the metal array; (c) Schematic of the working sensor; (d) Microscopic image of the fabricated sensor covered by glutamic acid
图 2 (a)器件Dev.2的THz透射谱,红线为实验结果,黑线为仿真结果;(b) f=0.35 THz (共振谷DA)处的仿真电场分布;(c) f=0.82 THz (共振谷DB)处的仿真电场分布,红色代表电场强度最大值,蓝色代表电场强度最小值
Figure 2. (a) THz transmission spectra for the Dev.2, where the red line indicates the experimental result and the black one indicates the simulated result; the simulated electric field distribution for (b) f=0.35 THz (the resonant dip DA) and (c) f=0.82 THz (the resonant dip DB), where the red color represents the maximum electric field intensity, and the blue one represents the minimum electric field intensity
图 3 (a)器件Dev.1、(b)器件Dev.2、(c)器件Dev.3在不同谷氨酸浓度下的THz透射谱;(d)器件Dev.1在共振峰P处、(e)器件Dev.2在共振峰P处、(f)器件Dev.3 在f=0.58 THz处的$ {\Delta }{T} $随浓度的变化
Figure 3. Transmission spectra for (a) Dev.1, (b) Dev.2, and (c) Dev.3 covered by glutamaic acid solution with the concentration of C0-C6; $ \Delta T $ as a function of the solution concentration for (d) Dev.1, (e) Dev.2 at the resonant peak P, and (f) Dev.3 at f=0.58 THz
图 5 (a)器件Dev.1、(b)器件Dev.2、(c)器件Dev.3在不同谷氨酸浓度下的${ \Delta }{P} $ 谱:(d)器件Dev.1、(e)器件Dev.2、(f)器件Dev.3从$ { \Delta P}{} $ 谱中提取出的斜率和浓度的关系
Figure 5. $ \Delta P $ spectra for (a) Dev.1, (b) Dev.2, and (c) Dev.3 covered by the glutamic acid solution with the concentration of C0-C6; the slope extracted from $ \Delta P $ spectra as a function of the solution concentration for (d) Dev.1, (e) Dev.2, and (f) Dev.3
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