Recent Advances in High-Frequency Electron Spin Resonance Detection Using a Microcantilever

Our recent developments in highly sensitive high-frequency electron spin resonance (ESR) using a microcantilever are reviewed. ESR signals of a Co Tutton salt microcrystal (<1 μg) have been detected at low temperature at frequencies up to 315 GHz under a static magnetic field using a microcantilever and a modulation technique. The achieved sensitivity is about 10⁹ spins/G at 4.5 K. Moreover, we have shown that similar ESR detection using a microcantilever is possible up to 130 GHz under a pulsed magnetic field without using a modulation technique. The achieved sensitivity is about 10¹¹ spins/G at 1.7 K. These results suggest that the ESR detection using a microcantilever is promising for applications to high-resolution and high-sensitivity terahertz ESR.     

Integrated mechano-optical hydrogen gas sensor using cantilever bending readout with a Si3N4 grated waveguide

We demonstrate a proof of concept of a novel and compact integrated mechano-optical sensor for H(2) detection based on a microcantilever suspended above a Si(3)N(4) grated waveguide. The fabricated devices are mechanically and optically modeled and characterized. Sensing operation of the sensor is demonstrated with 1% H(2) in N(2). The error in detection of the cantilever bending induced by absorption of H(2) is estimated to be approximately 10 nm. Significantly improved sensitivity (down to ～33 pm) is expected for reduced initial bending of the microcantilever. The simulation and experimental results are in good agreement and provide a good guideline for further optimization of the sensor.     

New Possibilities of OD ESR: Vacuum Ultraviolet Generation of Radical Ion Pairs

A new version of the optically detected electron spin resonance (OD ESR) technique using vacuum ultraviolet radiation to generate radical ion pairs is discussed. The technique can be used to study the spin-correlated processes of charge recombination in thin films that can be useful in spintronics. Distinctive features of photoionization and high-energy (including X-ray) ionization are discussed. The first results obtained by the technique in the study of charge recombination in polymeric and liquid crystal films are presented. The results of the concurrent observation of the OD ESR and electron cyclotron resonance (ECR) in the low-pressure gas over the sample are outlined. A possible application of ECR in the context of the OD ESR spectroscopy is suggested.     

Stripping voltammetry of Pb and Cu using a microcantilever electrode

Microfabricated silicon microcantilevers coated with gold on one side have been used as working electrode in a three-electrode electrochemical arrangement. In addition to electrochemical current, cantilever bending has been used as a signal for monitoring electrode reactions on the cantilever surface. The microcantilever bending was measured by an optical beam deflection method as the surface potential was scanned and electrochemical reactions occurred on the surface. The microcantilever bending due to differential surface stress was used to sense Pb and Cu using cyclic voltammetry (CV) and linear sweep stripping voltammetry (LSSV).     

High-field ESR on aligned membranes: a simple method to record spectra from different membrane orientations in the magnetic field

A combination of isopotential spin-dry ultracentrifugation (ISDU) and microtome techniques was used to facilitate the collection of high field/high frequency (170 GHz) ESR spectra corresponding to different orientations of the membrane normal relative to the magnetic field. This technique is particularly valuable for aligned biological samples in vitro. At 170 GHz, conventional sample preparation techniques based solely on ISDU constrained the sample to be oriented so that the membrane normal was parallel to the applied magnetic field due to the geometry and the millimeter wave field distribution of the Fabry-Pérot resonator used in these experiments. This orientational constraint limited the information that could be obtained from aligned membranes at high field. The combined ISDU/microtome technique overcame this limitation. Spectra from spin-labeled Gramicidin A and the spin label cholestane in aligned DPPC membranes provide a demonstration of the technique. We also discuss some virtues of high field/high frequency ESR on aligned membranes compared to X-band.     

Pixels array matching for optical readout microcantilever array sensing system

An approach based on pixels array matching is proposed for optical readout bimaterial microcantilever focal plane array (FPA) sensing system, by which the CCD's pixel array can match the low resolution FPA properly. Compared with the old method, it has the following three advantages: (1) reduces the impact on the infrared imaging quality due to the bending deformation of the microcantilever pixels; (2) decreases the background noise and lower the infrared imaging system's noise equivalent temperature difference; (3) increases the imaging system's frame rate. A microcantilever FPA infrared imaging system with a programmable smart camera was developed to demonstrate the effectiveness of the approach. In addition, the approach can be applied to a similar optical readout micro-array sensing system whose resolution is lower than the CCD.     

Parameter optimization of microcantilevers optically excited by a semiconductor laser with optical feedback

A novel approach of optically exciting and detecting the vibration of a microcantilever by a sinusoidally driven semiconductor laser subject to optical feedback is proposed. A theoretical model for the approach is established, and the working parameters are optimized. In our experiments, an Al-coated microcantilever is designed with the optimized working parameters, and the microcantilever is optically excited by a sinusoidally driven semiconductor laser. We have demonstrated that there exist periodic dips of the optical power of the semiconductor laser, which is caused by the resonant vibration of the microcantilever. The optical power of the semiconductor laser is also analyzed theoretically by using the Lang–Kobayashi (L–K) equations. The experimental result is consistent with the result of theoretical analysis.     

Variable Coupling Scheme for High-Frequency Electron Spin Resonance Resonators Using Asymmetric Meshes

The sensitivity of a high-frequency electron spin resonance (ESR) spectrometer depends strongly on the structure used to couple the incident millimeter wave to the sample that generates the ESR signal. Subsequent coupling of the ESR signal to the detection arm of the spectrometer is also a crucial consideration for achieving high spectrometer sensitivity. In previous work, we found that a means for continuously varying the coupling was necessary for attaining high sensitivity reliably and reproducibly. We report here on a novel asymmetric mesh structure that achieves continuously variable coupling by rotating the mesh in its own plane about the millimeter-wave transmission-line optical axis. We quantify the performance of this device with nitroxide spin label spectra in both a lossy aqueous solution and a low-loss solid-state system. These two systems have very different coupling requirements and are representative of the range of coupling achievable with this technique. Lossy systems, in particular, are a demanding test of the achievable sensitivity and allow us to assess the suitability of this approach for applying high-frequency ESR, e.g., to the study of biological systems at physiological conditions. The variable coupling technique reported on here allows us to readily achieve a factor of ca. 7 improvement in the signal-to-noise ratio at 170 GHz and a factor of ca. 5 at 95 GHz over what has previously been reported for lossy samples.     

利用微悬臂梁研究聚N-异丙基丙烯酰胺在金表面的自组装

利用微悬臂梁传感技术研究了巯基化的聚N-异丙基丙烯酰胺（HS-PNIPAM）在微悬臂梁金面上的自组装过程.由于大分子的构象变化改变了分子间的相互作用,导致微悬臂梁的表面应力改变,使微悬臂梁发生弯曲.通过光学方法实时读出微悬臂梁的弯曲信号,得到HS-PNIPAM的自组装动力学曲线.通过对不同分子量HS-PNIPAM的实验结果分析表明：HS-PNIPAM在自组装过程中存在三个阶段,分别对应不同的分子构象.第一阶段为物理吸附阶段,第二、三阶段为伴随着分子构象变化的化学吸附阶段.吸附曲线符合Langmuir等温吸附.分析结果还显示HS-PNIPAM的表面吸附速率κ远小于小分子的吸附速率,并与分子量成负指数关系;HS-PNIPAM的自组装时间远大于小分子的自组装时间,并与分子量成正比;底物表面应力的改变与HS-PNIPAM的分子量成线性关系. 关键词： 微悬臂梁 聚N-异丙基丙烯酰胺 自组装 构象转变     

Thermal transpiration at the microscale: a Crookes cantilever

Local temperature inhomogeneities in systems containing micron and submicron objects can result in unexpected consequences. If the mean free path of the host gas constituents is comparable to a characteristic length of the system, then a net exchange of momentum occurs between the constituents and the involved surfaces. For a given temperature gradient and a given pressure range, this results in the presence of Knudsen and Knudsen-like forces (KF). The pressure dependence of these forces has been studied using a microelectromechanical system composed of a microcantilever near a substrate surface. Nano-Newton scale KF are observed by the bending of the microcantilever as monitored by the charge variation on the microcantilever-substrate assembly in a capacitive mode.     

双材料微梁阵列室温物体红外成像

针对近年出现的新概念光学读出双材料微梁阵列红外成像技术，提出了具有热变形放大效果的无硅基底回折腿间隔镀金的微梁单元结构,并建立了其热机械模型，在模型分析基础上，成功的设计制作了100×100像素的焦平面阵列(focal plane array,FPA).在构建的红外成像系统中，实现了对室温物体——人体的热成像，噪声等效温度差约为200mK.实验结果与热机械模型的分析一致. 关键词： 非制冷红外成像 光学读出 双材料微梁阵列     

The status quo and prospect of ESR imaging applications to study on catalysts

ESR imaging technique supplies us with the possibility of spatial imaging of spin species, and has been widely accepted as a useful tool in many fields. ESR imaging can be applied to observing the spatial distribution of spin species and determining the diffusion processes. These applications will certainly interest chemists in catalyst field. In this paper, the characteristics and limitations of ESR imaging technique, and the status quo and prospect, of ESR imaging applications to catalyst study are discussed. With a current ESR apparatus, the sensitivity and spatial resolution are good enough for the most applications in catalyst studies. Although few works in this field have been reported, its prospect will be interesting. We suggestin situ observation of spatial distribution of paramagnetic species (such as reactants, products and intermediates) in a catalyst system, determination of diffusion in a catalyst pellet and characterization of poisoning in micro fixed-bed reactors with ESR imaging method. Not only paramagnetic species could be studied directly, but also antimagnetic species, which quench spin signals, could be studied indirectly with this method.     

Conformational Transition of Poly （Acrylic Acid） Detected by Microcantilever Sensing

Poly （acrylic acid） （PAA） chains are grafted on one side of a microcantilever by the self-assembled method and the deflections of the microcantilever are detected as a function of medium pH from 3 to 11. It is found that when the pH varies, the microcantilever deflects because of the changing surface stress. By analysing the electrostatic repulsive effect, the surface stress change is related to the conformation transition of PAA from a collapse state to a swelling state. This method offers the interaction information among the polymer chains during the conformational transition and affords an alternative way to study conformational change of polymers.     

The electron spin resonance of polycarbonate track detectors

Polycarbonate films are widely used as solid state track detectors (SSTDs) of radiation, but as yet our knowledge of the microscopic nature of the latent track is limited. The processes of chemical etching and thermal annealing are not fully understood. The lack of stability of track parameters bears on the accuracy of the charge determination of energetic heavy nuclei.

We have applied the technique of electron spin resonance, (ESR) in order to seek a correlation between the density of tracks and the growth and decay of free radicals detected by ESR. Samples of polycarbonate were irradiated with thermal neutrons and then etched progressively with NaOH. The ESR signal increased initially and then became weaker as the bulk of the polycarbonate was removed. Other samples were annealed after partial etching. ESR monitoring of this annealing showed that free radicals were recombining, probably due to diffusion processes.     

Non-destructive observation of electrically detected magnetic resonance in bulk material using AC bias

DC bias is normally found in conventional measurements of electrically detected magnetic resonance (EDMR). Usually, electrodes are formed on the sample surface to make ohmic contacts for detecting changes in the electrical characteristics of the sample material. Thus, destructive procedures are required to detect the EDMR signal of bulk material with such methods. An AC bias detection technique was developed to allow the non-destructive EDMR measurement of bulk materials. An AC bridge circuit was constructed to detect the change in impedance of the sample, which when changed by ESR, an unbalanced AC voltage can be detected. By detecting this AC bias, it is possible to cancel the effects, such as Shottky barriers, that disturb the ohmic contact between the electrodes and a sample material. Further, the AC bias current penetrates the thin surface layer of a sample such as silicon oxide, which normally obstructs a DC current. This method was utilized using conductive rubber contacts for non-destructive EDMR measurements of part of a silicon wafer. EDMR spectra observed were the same as those obtained by the conventional method of using DC bias detection.     

Direct measurement of two-electron contributions to the ground state energy of heliumlike high-Z ions

We report on a novel technique which exploitsradiative recombination transitions for a direct experimental determination of the two-electron contributions to the ground state energy in heliumlike high-Z ions. Results are presented of a first experiment which was conducted at an electron beam ion trap for various elements ranging from Z=32 to 83. The comparison with theoretical predictions demonstrates that the achieved precision already provides a sensitive test of second order many-body contributions and approaches the size of the two-electron (screened) Lamb shift. The potential of the new technique will be outlined and the capability of the ESR storage ring for future investigations will be emphasized.     

Imaging of electrically detected magnetic resonance of a silicon wafer.

An imaging technique of electrically detected magnetic resonance (EDMR) was newly developed. Because the EDMR signal is obtained from paramagnetic recombination centers, one may expect the image to represent the distribution of defect and/or impurity sites in the sample. We successfully obtained EDMR images of a light-illuminated silicon plate 8 mm in width and 15 mm in length, which was cut from a silicon wafer (n-type, 100 Omega cm), under ESR irradiation at a frequency of 890 MHz (wavelength, 340 mm). The reproducibility of the EDMR image obtained from a sample was amply satisfactory. When the oxidized surface of the silicon was removed, the EDMR signal disappeared. Although the EDMR signal reappeared when the surface of the sample became reoxidized, the EDMR image obtained was slightly different from the earlier one. This finding shows that the EDMR image obtained from the sample shows the distribution of defects at the Si/SiO(2) interface.     

1mm压电柱式超声微电机的研制

介绍了一种超声波微电机的设计研制工作。这种基于压电柱弯曲振动模态的超声波微电机,其直径仅有1 mm细,长约5 mm,重量仅有36 mg。它是采用压电柱作为定子,在压电柱的表面均匀分割出四个电极,进行极化和施加驱动电压。详细介绍了极化方式的选择,电极间隔的优化设计以及对原型样机的性能测试。实验表明,该电机能承受350V_pp的驱动电压,获得1800 rpm的转速和4 μNm的堵转力炬。此外,这种电机具有明显的微型化优势,根据现有工艺还可使电机直径减小到0.5 mm左右。     

试样激励下轻敲模式原子力声显微镜的非线性动力学特性

利用Euler-Bernoulli梁理论和DMT针尖-样品作用力模型建立了试样激励下轻敲模式原子力声显微镜(AFAM)系统的动力学方程,并应用非线性动力学分析方法对AFAM微悬臂梁的振动特性进行研究。通过合理改变超声激励幅值、超声激励频率和针尖-样品初始间距等模型参数模拟得到微悬臂梁的超谐波、次谐波、准周期和混沌振动现象,采用时间序列、频谱、相空间、Poincare截面和Lyapunov指数等方法对不同非线性振动特性进行表征。通过分析不同模型参数条件下微悬臂梁针尖-样品作用力特性,探索了微悬臂梁不同非线性振动现象的产生机制。此外,研究了AFAM微悬臂梁运动的分岔特性,发现当超声激励幅值和针尖-样品初始间隙连续变化时,周期、准周期和混沌运动交替出现。研究结果对AFAM系统非线性动力学行为分析和混沌振动控制提供了理论参考。     

碳纳米管微悬臂梁红外探测器的优化设计

对复合层微悬臂梁红外探测器进行了理论分析，并建立了相应的理论模型，实验研究了在硅基底上生长碳纳米管的吸热特性，优化设计了一种生长有碳纳米管的三层硅微悬臂梁谐振式红外探测器。该探测器基于复合层微悬臂梁的谐振频率随着微悬臂梁温度的改变发生漂移的特性，在一定的红外辐射下，微悬臂梁的温度会随着辐射光强的强弱而发生变化，从而根据微悬臂梁谐振频率的漂移而感知温度变化实现对辐射光的探测，利用碳纳米管的红外吸收特性，在二层微悬臂梁上生长碳纳米管薄膜作为吸收层，提高了微悬臂梁探测器的红外吸收性能。研究表明：其功率灵敏度可达fw级，比传统的静态测试方法提高了两个数量级。而且这种基于微机电系统技术的传感器与集成电路工艺是兼容的。