WO2013189111A1 - 一种基于原子力显微镜的纳米热电塞贝克系数原位定量表征装置 - Google Patents
一种基于原子力显微镜的纳米热电塞贝克系数原位定量表征装置 Download PDFInfo
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- WO2013189111A1 WO2013189111A1 PCT/CN2012/079076 CN2012079076W WO2013189111A1 WO 2013189111 A1 WO2013189111 A1 WO 2013189111A1 CN 2012079076 W CN2012079076 W CN 2012079076W WO 2013189111 A1 WO2013189111 A1 WO 2013189111A1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/58—SThM [Scanning Thermal Microscopy] or apparatus therefor, e.g. SThM probes
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- the present application relates to an in-situ quantitative characterization device for a nano-thermoelectric plug-in coefficient based on atomic force microscopy (AFM), which belongs to the field of signal detecting instruments.
- AFM atomic force microscopy
- Nano-thermoelectric energy materials have become an important strategic energy material and have broad application prospects in many important fields such as microelectronics, optoelectronics, deep space exploration, national defense, and energy conservation and environmental protection. At present, nano-thermoelectric performance testing is increasingly becoming a challenging issue in this field.
- the Seebeck coefficient is an important physical parameter of thermoelectric materials. At present, its characterization still follows the traditional method, that is, not only the temperature sensor is used to directly measure the temperature difference between the two ends of the material, but also the potential difference caused by the temperature difference needs to be measured at the same time.
- this method has the following insurmountable limitations for nano-thermoelectric materials: (1) It is difficult to directly introduce and directly measure the temperature difference of low-dimensional nano-thermoelectric materials, and it is difficult to realize the potential difference caused by the temperature difference. (2) The traditional method cannot reflect the dynamic performance of the thermoelectric material and continuously reflect the change state of the detected parameter with the spatial position.
- the present application hopes to establish an in-situ, non-destructive, real-time, dynamic characterization technique for realizing the Seebeck coefficient of nano-thermoelectric materials without directly measuring temperature changes, in order to meet the urgent needs of the current rapid development of nano-thermoelectric material performance characterization.
- the present application discloses an atomic force microscope-based nano thermoelectric plug-in coefficient in-situ quantitative characterization device for detecting a micro-area Seebeck coefficient of a sample of a nano-thermoelectric material to be tested, wherein the device further comprises: a harmonic An atomic force microscope in-situ excitation platform for wave signals, which is used to provide an atomic force microscope platform for developing a nano-thermoelectric plug-in coefficient in-situ characterization device, and simultaneously excites the nano-thermoelectric material micro-domain double-frequency and triple-frequency harmonic signals in situ;
- the nano-thermoelectric plug-in coefficient in-situ detection platform is used for real-time detection and processing of the double-frequency and triple-frequency of the nano-thermoelectric material micro-region, and shows the in-situ characterization result of the micro-area Seebeck coefficient thermoelectric parameter.
- the atomic force microscope in-situ excitation platform of the harmonic signal further comprises: an atomic force microscope platform, a thermoelectric detection probe, a thermoelectric reference probe, two adjustable resistance networks, a signal generator, and a signal generator a thermoelectric material, a ceramic insulating layer, a magnetic base, a signal transmission end, a micro-region double-frequency harmonic voltage signal output port, a micro-region triple-frequency harmonic voltage signal output port, wherein the measured thermoelectricity A sample of the material is placed on the magnetic base by underlying the ceramic insulating layer, and the thermoelectric detection probe, the thermoelectric reference probe, the two adjustable resistor networks, and the signal generator form a Wheatstone bridge, the thermoelectric Detecting a probe placed on the sample of the thermoelectric material to be tested and contacting to detect a voltage of the excitation point of the sample of the thermoelectric material to be tested; and transmitting, by the signal, the first end of the micro-frequency double-frequency voltage signal output port Receiving a voltage signal of another region of the sample of the
- the mode of operation of the atomic force microscope platform is a contact mode.
- the thermoelectric detection probe is a probe having thermistor characteristics, and has the functions of a micro-region excitation source, a signal sensor and a detection source; the thermoelectric detection probe is an atomic force display.
- the micro-mirror contact mode, the micro-cantilever shape variable as a feedback parameter is 0. l-5 nm, and the diameter of the interaction contact area with the sample of the thermoelectric material to be tested is 30-100 nm.
- thermoelectric probe has an operating frequency range of 100 Hz to 10 kHz and an operating current range of 1 mA to 100 mA.
- the nano-thermoelectric plug-in coefficient in-situ detection platform further comprises: a high-sensitivity lock-in amplifier, a front-end loop processing module, a high-sensitivity lock-in amplifier, a data processing and display system, etc., for implementing In-situ real-time detection, processing and display of in-situ characterization results of micro-area Seebeck coefficient thermoelectric parameters for weak double-frequency and triple-frequency harmonic voltage signals
- the purpose of the present application is to provide an in situ quantitative nanocharacterization device that can be used for the thermoelectric parameter characterization of nano-Sebeck coefficient of nano-thermoelectric energy materials without directly measuring temperature changes.
- the method combines the atomic force microscope nano-detection function, the three-frequency detection principle of macroscopic thermal conductivity, the Joule heating effect principle and the macro Seebeck coefficient test principle. Based on the commercial AFM nano-detection platform, a method is not needed to directly measure temperature changes.
- the harmonic detection technology that realizes the in-situ direct characterization of the nano-Sebeck coefficient thermoelectric parameters, the new method not only completely avoids the requirement of direct measurement of the temperature change necessary for the macro thermoelectric plug-in coefficient testing technology, but also has a nano temperature difference, nano-Sebeck Harmonic signals have the unique functions of simultaneous in-situ excitation and in-situ synchronous characterization, and have the advantages of high resolution, high sensitivity, high signal-to-noise ratio, direct test, etc.
- the key technical devices described in the present application are simple in structure and strong in compatibility. Suitable for combination with different commercial AFM systems, it is a new technology that is easy to promote and apply.
- the nanometer characterization device of the present application has the unique advantage of obtaining a nano-thermoelectric plug-in coefficient by directly detecting the double-frequency and triple-harmonic signals without directly measuring the temperature.
- the method expands the nano-thermoelectric property evaluation function not available in the existing commercial atomic force microscope, and provides important in-situ, quantitative, and nano-in-depth research on the thermoelectric transport theory of nano-thermoelectric materials and the in-depth development of nano-thermoelectric materials and their devices. Characterize new methods. DRAWINGS
- FIG. 1 is a schematic diagram showing the in-situ characterization of the nano-thermoelectric plug-in coefficient of the present application
- FIG. 2 is a block diagram showing the structure of the nano-thermoelectric plug-in coefficient in-situ characterization device of the present application
- FIG. 3 is a block diagram showing the structure of the AFM in-situ excitation platform of the harmonic signal shown in FIG. 1
- FIG. 4 is a diagram showing the atomic force of FIG. A block diagram of the microscope platform (AFM);
- Figure 5 is a block diagram showing the structure of the nano-thermoelectric plug-in coefficient in-situ detection platform of Figure 2;
- Figure 6 is a block diagram showing the structure of the front-end loop processing in Figure 5;
- Figure 7 (a) shows the test results of the double-frequency signal ( ⁇ 2 ⁇ ) at different excitation voltages of Bi-Sb-Te nano-thermoelectric thin films.
- Figure 7 (b) shows the micro-domain triple-frequency signals at different excitation voltages (v 3 [omega]) test results;
- Figure 8 shows the test results of the double-frequency signal ( ⁇ 2 ⁇ ) and the triple-frequency signal ( ⁇ 3 ⁇ ) at different excitation voltages of another Bi-Sb-Te nano-thermoelectric film, from which the slope of the linear part can be calculated.
- thermoelectric multi-parameters of the nano-thermoelectric thin film material micro-area Seebeck coefficient by using the nano-thermoelectric plug-in coefficient in-situ quantitative characterization device of the present application, to further illustrate the effect of the present application, but not limited to the following Example.
- thermoelectric probe When an alternating voltage V of frequency ⁇ . When cos ⁇ t acts on a thermoelectric probe, the thermoelectric probe will generate a temperature wave ( ⁇ 2 ⁇ ) having a frequency of 2 ⁇ due to the Joule heating effect and diffuse into the thermoelectric material. For a thermoelectric material, the temperature ⁇ 2 ⁇ will generate a Seebeck voltage resonance signal of the same frequency based on the Seebeck effect unique to the thermoelectric material, that is, the Seebeck voltage double frequency signal ( ⁇ 2 ⁇ ).
- this application establishes an in-situ quantitative characterization device for thermoelectric parameters of nano-Sebeck coefficient based on atomic force microscopy.
- the working principle structure is shown in Figure 2.
- the characterization device consists of two parts: harmonic signal AFM in-situ excitation platform 1, nano-thermoelectric plug-in coefficient in-situ detection platform 2.
- the AFM in-situ excitation platform 1 of the harmonic signal is used to provide an AFM platform foundation for developing a nano-thermoelectric plug-in coefficient in-situ characterization device, and thereby realizes the micro-harmonic double-frequency and triple-frequency harmonic signals of the nano-thermoelectric material.
- the working structure of the AFM in-situ excitation platform 1 of harmonic signals is shown in Figure 3. It mainly includes the atomic force microscope platform 11, the thermoelectric detection probe 12, the thermoelectric reference probe 13, and two adjustable resistor networks 14, 15, which generate signals.
- the device 16 the thermoelectric material 17, the ceramic insulating layer 18, the magnetic base 19, the signal transmitting end 1 10, the micro-region double-frequency harmonic signal output port 111, the micro-region triple-frequency harmonic signal output port 112, and the like.
- thermoelectric detection probe 12 is placed on the sample 17 of the thermoelectric material to be tested and contacted to detect the voltage at the excitation point of the sample.
- the first end of the micro-region double-frequency harmonic signal output port 11 1 receives the voltage signal of another region of the sample of the thermoelectric material 17 to be tested through the signal transmitting end 110, The second end of the micro-region double-frequency harmonic signal output port 1 1 1 is connected to the bridge ground.
- the first end of the micro-region triple-frequency harmonic signal output port 12 is connected to the connection end of the thermoelectric detection probe 12 and the bridge, and the second end is connected to the connection end of the thermoelectric reference probe 13 and the bridge.
- the AFM in-situ excitation platform 1 of the harmonic signal of the above structure is used to provide the basic hardware platform required for in-situ characterization of the nano-thermoelectric plug-in coefficient, and simultaneously realizes the in-situ simultaneous excitation of the nano-thermoelectric material micro-domain double frequency and triple harmonic Wave signal.
- FIG 4 shows a further block diagram of the AFM platform 1 1 in Figure 3.
- the microscope platform 1 1 is a commercial atomic force microscope (AFM) with high-precision control and nano-scale high-resolution imaging characteristics. It mainly includes a scanning component l l a, a force detecting component l ib , a position detecting component l i e , a feedback control component l i d , etc., to provide a basic hardware platform required for nano thermoelectric detection.
- the AFM mode of operation is contact mode, and its feedback parameter (microcantilever variable) is 0. 1-5 awake to achieve good nanoscale contact between the thermoelectric probe and the sample and effective signal excitation and transmission.
- thermoelectric detection probe 12, the thermoelectric reference probe 13, and the two adjustable resistor networks 14, 15, constitute a thermoelectric circuit, and realize triple-frequency signal excitation directly related to the temperature change of the micro-thermoelectric material micro-region.
- the thermoelectric circuit employs a bridge structure with high detection sensitivity characteristics, which is significantly different from a general bridge structure capable of detecting only a single physical quantity.
- the bridge of the thermoelectric circuit is completely enclosed in the metal box to shield the interference signal; and the two adjustable resistor networks 14 and 15 use precision non-inductive resistors to avoid the influence of the distribution parameters of the electronic components on the detection accuracy.
- the thermoelectric detection probe 12 is the core component of the system in the thermoelectric circuit.
- the thermoelectric detection probe 12 is significantly different from the commercial AFM probe. Its structure is a V-shaped structure, made of Pt/Rh material, and has a thermistor characteristic, that is, its resistance value will change with the temperature of the probe.
- the probe has three functions of micro-region heat source, micro-zone temperature sensor and micro-region harmonic signal lead-out line, and has a single structure and convenient use.
- the working mode is AFM contact mode, and the diameter of the interaction area with the sample of the thermoelectric material sample 17 is 30-100 nm, which realizes the effective excitation and output of the nano-scale micro-area signal.
- thermoelectric detection probe 12 generates a harmonic effect under the excitation of the periodic signal, and detects the double-frequency and triple-frequency higher harmonic signals associated with the sample of the thermoelectric material to be tested, which can be used to reflect the sample 17 of the thermoelectric material to be tested. Micro-area Seebeck coefficient.
- the working frequency of the thermoelectric detection probe 12 must be the same It also takes into account the optimal working state of the thermoelectric probe and the effective output of the harmonic signal. Its operating frequency range is 100 Hz-10 kHz, and its operating current range is lmA-100 mA.
- thermoelectric detection probe 12 and the thermoelectric reference probe 13 form a double probe structure and are connected to the system by a differential input method, thereby effectively overcoming the influence of ambient temperature interference, improving the detection sensitivity of the harmonic signal, and ensuring the test data.
- the accuracy of the test reduces the working conditions of the test.
- the signal generator 16 provides a working power supply for the thermoelectric circuit formed by the thermoelectric detection probe 12, the thermoelectric reference probe 13, and the two adjustable resistor networks 14, 15 with adjustable signal amplitude and frequency.
- the signal amplitude takes into account the operating current of the thermal probe operation 12, and the signal frequency simultaneously takes into account the excitation signal of the required steady-state thermal power of the micro-domain double-frequency harmonic signal and the triple-frequency harmonic signal.
- thermoelectric sample 17, ceramic insulating layer 18, magnetic base 19, constitutes a thermoelectric sample stage, which is bonded with each other by conductive adhesive, which effectively ensures the mechanical stability of the sample and the effective transmission of signals.
- the signal transmitting end 110 is a surface copper piece adhered to the surface of the sample of the thermoelectric material to be tested 17 and its lead-out conductive line, and constitutes a transmission end of the micro-zone Seebeck voltage double-frequency harmonic signal.
- the copper piece is bonded by soldering, which not only ensures the micro-ohmic contact of the Seebeck voltage harmonic signal lead; at the same time, the lead wire is robust to ensure the stability of the test conditions and the reliability of the data.
- the micro-zone Seebeck voltage double-frequency harmonic signal output port 1 11 realizes the detection of the nano-thermoelectric material micro-zone Seebeck voltage double-frequency harmonic signal output.
- One end of the signal lead originates from the thermoelectric detection probe
- the other end is derived from a copper sheet 110 adhered to the upper surface of the pyroelectric sample 17 to be tested and soldered with a conductive wire.
- the micro-area triple-frequency harmonic signal output port 112 realizes the micro-area triple-frequency harmonic signal output directly related to the temperature change of the detected micro-thermoelectric material micro-region.
- the ends of the signal are derived from the 12-terminal lead of the thermoelectric detection probe and the 13-terminal lead of the thermoelectric reference probe.
- the working structure of the nano-thermoelectric plug-in coefficient in-situ detection platform 2 is shown in Fig. 5, including a high-sensitivity lock-in amplifier 21, a front-end loop processing module 22, a high-sensitivity lock-in amplifier 23, a data processing and display module 24, etc.
- In-situ characterization results of in-situ real-time detection, processing and display of micro-Sebeck coefficient thermoelectric parameters of weak double-frequency and triple-frequency harmonic signals are realized.
- the working structure principle of the front-end loop processor 22 is as shown in FIG. 6, and includes a pre-circuit 221, an amplifying circuit 222, a protection circuit 223, and a power source 224 to implement resistance to the output signal of the thermoelectric circuit. Anti-transformation, at the same time, it has improved signal amplitude and protection function to prevent overload and damage to the next-level circuit and instrument when the bridge is out of balance or the signal is distorted.
- the high-sensitivity phase-locked signal amplifiers 21 and 23 have the advantages of high measurement sensitivity, strong anti-interference, linear and non-linear detection functions, and system operation requirements, enabling high-sensitivity detection of weak harmonic signals.
- the data processing and display module 24 includes a signal processing module and a result display module based on a computer platform. Based on the ratio of the micro-region double-frequency harmonic signal to the triple-frequency harmonic signal, that is, 8 2 ⁇ 3 £0 , the micro-region thermoelectric plug-in coefficient can be calculated.
- Example 1 Based on the ratio of the micro-region double-frequency harmonic signal to the triple-frequency harmonic signal, that is, 8 2 ⁇ 3 £0 , the micro-region thermoelectric plug-in coefficient can be calculated.
- FIG. 7 shows the test results.
- Figure 7 (a) shows the test results of the double-frequency signal ( ⁇ 2 ⁇ ) of the Bi-Sb-Te nano-thermoelectric film at different excitation voltages with an AC conversion rate of 200 Hz;
- Figure 7 (b) shows the difference obtained simultaneously in situ.
- Figure 7 (c) is the curve of the double-frequency signal according to the graph (a) and the triple-frequency signal of the graph (b), according to the slope of the linear portion thereof.
- Example 2 shows the test results of the double-frequency signal ( ⁇ 2 ⁇ ) of the Bi-Sb-
- the above example shows the in situ of the nano-thermoelectric plug-in coefficient based on atomic force microscopy.
- the new method of quantitative characterization solves the key technical problem that nano-thermoelectric materials can directly and quantitatively characterize the nano-thermoelectric plug-in coefficient without directly measuring the temperature change.
- the novel nano-characterization device realizes in-situ simultaneous excitation and in-situ simultaneous characterization of the double-frequency and triple-frequency harmonic signals required by the nano-thermoelectric plug-in coefficient, and expands the evaluation of nano-thermoelectric properties not available in existing commercial atomic force microscopes.
- the function provides an important new method for in situ, quantitative and nano-characterization for the in-depth study of thermoelectric transport theory and devices of nano-thermoelectric materials, especially nano-thermal wires.
- the outstanding advantages of the present application are that the atomic force microscope nano-detection function, the macroscopic thermal conductivity triple frequency test principle, the Joule heating effect principle and the macro Seebeck coefficient test principle are combined to propose a method based on AFM thermal probe.
- the harmonic effect is used to characterize the new principle of the nano-Sebeck coefficient, and thereby establish an in-situ harmonic excitation and detection technique for characterizing the nano-Sebeck coefficient on the AFM platform without directly measuring the temperature change.
- the new method not only does not require direct measurement of the temperature variation necessary for macroscopic Seebeck coefficient testing, but also has the unique function of nano temperature difference, in situ simultaneous excitation of nano-Sebeck harmonic signals, in-situ synchronous characterization, and high resolution.
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Abstract
一种基于原子力显微镜的纳米热电材料微区塞贝克系数原位定量表征装置，包括：一谐波信号的原子力显微镜原位激励平台（11），用于原位同时激发纳米热电材料微区二倍频、三倍频谐波信号，具体包括由热电检测探针（12）、热电参考探针（13）、两个可调电阻网络（14，15）和信号发生器（16）组成的惠斯通电桥；一纳米热电塞贝克系数原位检测平台（2），用于实现所述纳米热电材料微区二倍频、三倍频的原位实时检测和处理，利用所述二倍频、三倍频信号来计算所述微区塞贝克系数，并显示结果。通过将原子力显微镜纳米检测功能、宏观热导三倍频测试原理、焦耳热效应原理及宏观塞贝克系数测试原理相结合，建立起基于商用原子力显微镜热探针所诱导的谐波效应来表征纳米塞贝克系数的新方法。
Description
一种基于原子力显微镜的纳米热电塞贝克系数原位定量表征装置 技术领域
本申请涉及一种基于原子力显微镜 （简称 AFM) 的纳米热电塞贝克系数 的原位定量表征装置， 属于信号检测仪器领域。
冃 不
纳米热电能源材料巳成为作为一种重要的战略性能源材料， 在微电子、 光电子、 深空探测、 国防军工、 以及节能环保等众多重要领域具有十分广阔 的应用前景。 当前， 纳米热电性能检测亦日益成为该领域急需解决的挑战性 课题。 塞贝克系数是热电材料一个重要的物理参量， 目前其表征仍然沿用传 统方法， 即不仅要采用温度传感器直接测量材料两端的温度差， 而且也需要 同时测量由温差所引起的电位差。 显然， 该方法对纳米热电材料而言具有以 下几点难以克服的局限性： （1 ) 难以实现低维纳米热电材料温度差的直接 引入及直接测量， 进而难以实现该温差所引起的电位差的测定； （2 ) 传统 方法无法反映热电材料动态性能及连续反映被检测参量随空间位置的变化 状态。 针对上述局限性， 本申请希望建立无需直接测量温度变化而实现纳米 热电材料塞贝克系数的原位、 无损、 实时、 动态表征技术， 以满足当前迅猛 发展的纳米热电材料性能表征之急需。
发明内容
基于目前纳米热电物理性能表征之迫切需求，本申请是在同日递交的发 明专利申请 "一种基于原子力显微镜的纳米热电多参量原位定量表征装置" 的基础上， 进一步提出了一种基于原子力显微镜纳米平台表征热电材料纳米 塞贝克系数的新技术原理， 并藉此建立了无需直接测量温度变化即可直接原 位定量表征纳米热电塞贝克系数参量的关键技术装置和相关的测试方法， 实
现了纳米热电材料塞贝克系数的原位、 实时、 动态、 定量测试， 为有关热电 材料纳米尺度热电输运行为物理本质的深入研究及有关纳米热电器件的物 性评价提供了一种原理简单、 测试直接的原位定量纳米表征技术。
本申请公开了一种基于原子力显微镜的纳米热电塞贝克系数原位定量表 征装置， 用于检测一被测纳米热电材料样品的微区塞贝克系数， 其特征在于， 所述装置进一步包括： 一谐波信号的原子力显微镜原位激励平台， 用于提供发 展纳米热电塞贝克系数原位表征装置的原子力显微镜平台， 并原位同时激发纳 米热电材料微区二倍频、 三倍频谐波信号； 一纳米热电塞贝克系数原位检测 平台， 用于实现所述纳米热电材料微区二倍频、 三倍频的原位实时检测和处 理， 并显示微区塞贝克系数热电参量的原位表征结果。
比较好的是， 所述谐波信号的原子力显微镜原位激励平台进一步包 括： 一原子力显微镜平台， 一热电检测探针， 一热电参考探针， 两个可调 电阻网络， 一信号发生器， 一热电材料， 一陶瓷绝缘层， 一磁性底座， 一 信号传输端， 一微区二倍频谐波电压信号输出端口， 一微区三倍频谐波电 压信号输出端口， 其中， 所述被测热电材料样品通过下垫所述陶瓷绝缘层置 于所述磁性底座上， 所述热电检测探针、 热电参考探针、 两个可调电阻网 络和信号发生器组成一惠斯通电桥， 所述热电检测探针置于所述被测热电 材料样品上并接触， 以检测所述被测热电材料样品激励点的电压； 所述微 区二倍频电压信号输出端口的第一端通过所述信号传输端接收所述被测热 电材料样品另一区域的电压信号，所述微区二倍频电压信号输出端口的第二 端与所述惠斯通电桥接地端相连； 所述微区三倍频电压信号输出端口的第 一端连接所述热电检测探针与所述惠斯通电桥相连端， 其第二端连接所述 热电参考探针与所述惠斯通电桥相连端。
比较好的是， 所述原子力显微镜平台的工作模式为接触模式。 比较好的是， 所述热电检测探针为一具热敏电阻特性的探针， 同时具 有微区激励源、 信号传感器及检测源的功能； 所述热电检测探针为原子力显
微镜接触模式， 其作为反馈参量的微悬臂形变量为 0. l-5 nm， 与所述被测热 电材料样品互作用接触面积的直径为 30-100 nm。
比较好的是， 所述热电探针的工作频率范围为 100 Hz-10 kHz , 工作电 流范围为 lmA-100 mA。
比较好的是， 所述纳米热电塞贝克系数原位检测平台进一步包括： 一 高灵敏度锁相放大器， 一前端回路处理模块， 一高灵敏度锁相放大器， 一数 据处理和显示系统等，用于实现微弱二倍频和三倍频谐波电压信号的原位实 时检测、 处理和显示微区塞贝克系数热电参量的原位表征结果
本申请目的在于提供一种无需直接测量温度变化而能够用于纳米热 电能源材料纳米塞贝克系数热电参量表征用的原位定量纳米表征装置。 该 方法将原子力显微镜纳米检测功能、 宏观热导率的三倍频检测原理、 焦耳 热效应原理以及宏观塞贝克系数测试原理相结合起来， 基于商用 AFM纳米 检测平台， 建立起一种无需直接测量温度变化而实现纳米塞贝克系数热电 参量原位直接表征的谐波检测技术， 该新型方法不仅完全避免了宏观热电 塞贝克系数测试技术所必需的温度变化直接测量的要求， 而且具有纳米温 差、 纳米塞贝克谐波信号原位同时激发、 原位同步表征的独特功能， 且具 有高分辨率、 高灵敏度、 高信噪比、 测试直接等优点， 本申请所述的关键 技术装置结构简单、 兼容性强， 适与不同商用 AFM系统相结合， 是一项易 于推广和应用的新技术。
本申请的纳米表征装置具有无需直接测量温度， 只需直接检测二倍 频、 三倍谐波信号即可获得纳米热电塞贝克系数的独特优点。 该方法拓展 了现有商用原子力显微镜所不具有的纳米热电物性评价功能， 为深入研究 纳米热电材料的热电输运理论及纳米热电材料及其器件的深入发展提供 了重要的原位、 定量、 纳米表征新方法。 附图说明
下面， 参照附图， 对于熟悉本技术领域的人员而言， 从对本申请的详细
描述中， 本申请的上述和其他目的、 特征和优点将显而易见。
图 1示意出本申请的纳米热电塞贝克系数原位表征原理图；
图 2示意出本申请的纳米热电塞贝克系数原位表征装置的结构框图； 图 3示意出图 1中所述谐波信号的 AFM原位激励平台的结构框图； 图 4示意出图 3中原子力显微镜平台 （AFM) 的结构框图；
图 5示意出图 2中纳米热电塞贝克系数原位检测平台的结构框图； 图 6示意出图 5中前端回路处理的结构框图；
图 7 (a) 给出了 Bi-Sb-Te 纳米热电薄膜不同激发电压下二倍频信号 ( ν2ω) 的测试结果； 图 7 (b)为不同激发电压下微区三倍频信号 （ν3ω) 的 测试结果； 图 7 (c)为根据图（a)二倍频信号与图 （b )三倍频信号所作的曲 线， 据此可计算出其线性部分斜率即为微区塞贝克系数 s=v2G)/v3co=i4o. oi μν/Κ ο
图 8给出了另一 Bi-Sb-Te纳米热电薄膜不同激发电压下二倍频信号 ( ν2ω) 与三倍频信号 （ν3ω) 的测试结果， 据此可计算出其线性部分斜率 即为微区塞贝克系数 S=V2 CO/V3CO=50. 49 μν/Κ ο 具体实施方式
以下实例均是应用本申请的纳米热电塞贝克系数原位定量表征装置对 纳米热电薄膜材料微区赛贝克系数热电多参量的定量表征结果， 以进一步说 明本申请的效果， 但并非仅限于下述实施例。
本申请建立了一种基于原子力显微镜的原位表征纳米热电塞贝克系数 的新方法。 该新方法工作原理如图 1所示， 具体可表述如下： 当一频率为 ω 的交变电压 V。cos ω t作用于一热电探针时，该热电探针将由于焦耳热效应产 生一频率为 2ω的温度波（Τ2ω)并向热电材料内扩散。 对于一热电材料而言， 该温度波 Τ2ω将基于该热电材料所特有的塞贝克效应产生同频率的塞贝克电 压谐振信号，即塞贝克电压二倍频信号（ν2ω)。根据热电材料塞贝克系数定义， 塞贝克系数 （S ) 可表示为塞贝克电压 （V ) 与温度差（ΔΤ)之比，即 S=V/AT。
因此， 材料微区塞贝克系数可表达为 S=V/AT=V2C0/T2C0。
而另一方面， 根据宏观热导率三倍频（3ω)测试方法原理可知， 当频率 为 ω的交变电流作用于该热电探针时， 将产生频率为 3ω的交流电压成分， 即三倍频信号（ν3 ω )；该三倍频信号的振幅直接与温度波谐振信号的振幅成 正比， 即温度谐振信号 Τ2 ω可由三倍频电压信号 ν3 ω给出。
因此， 热电材料微区塞贝克系数可表达为 S=V/AT=V2 CO/T2 (0=V2 CO/V3CO, 即 微区塞贝克系数可表示为二倍频电压谐振信号与三倍频电压信号之比， 其 中二倍频信号与微区塞贝克电压信号有关， 而三倍频电压信号与微区温度 变化有关。
基于该工作原理， 本申请建立了一种基于原子力显微镜的纳米塞贝克 系数热电参量的原位定量表征装置， 其工作原理结构如图 2所示， 该表征 装置由二部分组成： 谐波信号的 AFM原位激励平台 1， 纳米热电塞贝克系 数原位检测平台 2。 其中的谐波信号的 AFM原位激励平台 1， 用于提供发展 纳米热电塞贝克系数原位表征装置的 AFM平台基础， 并基此实现纳米热电 材料微区二倍频、 三倍频谐波信号的原位同时激发； 其纳米热电塞贝克系数 原位检测平台 2， 用于实现纳米热电材料微区二倍频、 三倍频的原位实时检 测和处理， 显示微区塞贝克系数热电参量的原位表征结果。
谐波信号的 AFM原位激励平台 1的工作结构如图 3所示， 主要包括原 子力显微镜平台 11 , 热电检测探针 12， 热电参考探针 13， 两个可调电阻 网络 14、 15， 信号发生器 16， 热电材料 17， 陶瓷绝缘层 18， 磁性底座 19， 信号传输端 1 10， 微区二倍频谐波信号输出端口 111， 微区三倍频谐波信号 输出端口 112等。 其中， 一被测热电材料样品 17通过下垫陶瓷绝缘层 18置 于原子力显微镜平台 11的磁性底座 19上， 热电检测探针 12， 热电参考探 针 13 , 两个可调电阻网络 14、 15， 信号发生器 16 组成惠斯通电桥 ( Wheatstone bridge ) ， 热电检测探针 12置于被测热电材料样品 17上 并接触， 以检测样品激励点的电压。 微区二倍频谐波信号输出端口 11 1的 第一端通过信号传输端 110接收被测热电材料样品 17另一区域的电压信号，
微区二倍频谐波信号输出端口 1 1 1的第二端与电桥接地端相连。 此外， 微 区三倍频谐波信号输出端口 1 12 的第一端连接热电检测探针 12与电桥相 连端， 其第二端连接热电参考探针 13与电桥相连端。
上述结构的谐波信号的 AFM原位激励平台 1用以提供纳米热电塞贝克 系数原位表征所需的基本硬件平台， 并实现原位同时激发纳米热电材料微 区二倍频、 三倍频谐波信号。
图 4给出了图 3 中原子力显微镜平台 1 1 的进一步结构框图， 该显微 镜平台 1 1为商用原子力显微镜 （AFM ) ， 具有高精度控制、 纳米级高分辨 率成像特性。主要包括扫描部件 l l a，力检测部件 l ib ,位置检测部件 l i e , 反馈控制部件 l i d 等， 用以提供纳米热电检测所需的基本硬件平台。 AFM 工作模式为接触模式， 其反馈参量 （微悬臂形变量） 为 0. 1-5醒， 用以实 现热电探针与样品之间良好的纳米尺度接触及有效的信号激发和传输。
再回到图 3 中， 热电检测探针 12 , 热电参考探针 13， 两个可调电阻 网络 14、 15， 构成热电回路， 实现与纳米热电材料微区温度变化直接相关 的三倍频信号激发。 该热电回路采用具有高检测灵敏度特点的电桥结构， 该电桥结构与仅能检测单一物理量的一般电桥结构显著不同。 其中热电回 路的桥路整体封闭于金属盒内，以屏蔽干扰信号；而两个可调电阻网络 14、 15选用精密无感电阻， 以避免电子元件的分布参数影响检测精度。
热电检测探针 12 在该热电回路中是系统的核心部件。 热电检测探针 12与商用 AFM探针有显著的不同，其结构为 V型结构、由 Pt/Rh材料制成， 具热敏电阻特性， 即其电阻阻值将随探针温度变化而改变。 该探针同时具 有微区热源、 微区温度传感器及微区谐波信号引出线等三种功能， 结构单 一、 使用方便。 其工作模式为 AFM接触模式， 与被测热电材料样品 17互 作用接触面积的直径为 30- 100 nm，实现了纳米尺度微区信号的有效激励 及输出。 热电检测探针 12 在周期性信号激励下产生谐波效应， 检测与被 测热电材料样品 1 7 相关的二倍频和三倍频高次谐波信号， 可用以反映被 测热电材料样品 17的微区塞贝克系数。 热电检测探针 12的工作频率须同
时兼顾热电探针的最佳工作状态及谐波信号的有效输出， 其工作频率范围 为 100 Hz-10 kHz , 其工作电流范围为 lmA-100 mA。
热电检测探针 12与热电参考探针 13构成双探针结构，采用差动输入方 式与系统相连，如此有效地克服了环境温度干扰的影响，提高了谐波信号的 检测灵敏度， 确保了测试数据的准确性， 降低了测试工作条件。
信号发生器 16提供热电检测探针 12、 热电参考探针 13、 两个可调电 阻网络 14、 15所构成的热电回路的工作电源， 其信号幅度和频率均可调。 信号幅度兼顾热探针工作 12 的工作电流， 而信号频率同时兼顾微区二倍 频谐波信号及三倍频谐波信号激发所需稳态热功率的激励信号。
热电样品 17， 陶瓷绝缘层 18， 磁性底座 19 , 构成热电样品台， 彼此之 间采用导电胶粘结， 有效地保证了样品的机械稳定性和信号的有效传输。
信号传输端 110，为粘在被测热电材料样品 17上表面铜片及其引出导电 线， 构成微区塞贝克电压二倍频谐波信号传输一端。 其中铜片以焊接方式粘 结， 不仅保证了塞贝克电压谐波信号引线的微欧姆接触； 同时引线坚固保证 了测试条件的稳定性和数据的可靠性。
微区塞贝克电压二倍频谐波信号输出端口 1 11 , 实现所检测纳米热电材 料微区塞贝克电压二倍频谐波信号输出。其信号引线一端源于热电检测探针
12， 另一端源于粘在被测热电样品 17上表面并焊有导电线的铜片 110。
微区三倍频谐波信号输出端口 112， 实现与所检测纳米热电材料微区温 度变化直接相关的微区三倍频谐波信号输出。其信号两端引线源于热电检测 探针 12—端引线以及热电参考探针 13—端引线。
纳米热电塞贝克系数原位检测平台 2 的工作结构图如图 5所示， 包括 高灵敏度锁相放大器 21 , 前端回路处理模块 22， 高灵敏度锁相放大器 23， 数据处理和显示模块 24 等， 用以实现微弱二倍频、 三倍频谐波信号的原 位实时检测、 处理和显示微区塞贝克系数热电参量的原位表征结果。
前端回路处理器 22的工作结构原理如图 6所示， 包括前置电路 221， 放大电路 222， 保护电路 223， 电源 224， 以对热电回路的输出信号实现阻
抗变换， 同时具有提高信号幅度与保护功能， 防止电桥失衡或信号畸变时 产生过载而损坏下一级电路和仪器。
高灵敏度锁相信号放大器 21和 23具有测量灵敏度高、 抗干扰性强、 且具线性和非线性检测功能、 满足系统工作要求等优点， 可实现微弱谐波 信号的高灵敏度检测。
数据处理及显示模块 24包括基于计算机平台的信号处理模块和结果显 示模块。 基于微区二倍频谐波信号与三倍频谐波信号的比值， 即 8 2^3£0， 可计算获得微区热电塞贝克系数。 实施例 1
应用本申请建立的纳米热电塞贝克系数原位定量表征装置对
Bi-Sb-Te热电薄膜的微区塞贝克系数进行了测试， 图 7显示了测试结果。 其中图 7 (a)为 Bi-Sb-Te纳米热电薄膜在交变频率为 200Hz的不同激发电 压下二倍频信号 （ν2ω) 的测试结果； 图 7 (b)为原位同时获得的不同激发 电压下微区三倍频信号 （ν3ω) 的测试结果； 图 7 (c)为根据图（a)二倍频信 号与图 （b ) 三倍频信号所作的曲线， 根据其线性部分斜率即可计算出微 区塞贝克系数， 即 S=V2CO/V3CD=140. 01 μν/Κ, 该值非常接近于该薄膜的宏观 测试结果 S=138 μν/Κ, 表明微区塞贝克定量表征装置的可行性及结果的准 确性。 实施例 2
应用本申请建立的纳米热电塞贝克系数原位定量表征装置对一热电 体材料微区塞贝克系数进行了测试， 图 8显示了交变频率为 200Hz下的测 试结果。 根据其线性部分斜率即可计算出微区塞贝克系数为 S=50. 49 μν/Κ ο 该值非常接近于该薄膜的宏观测试结果 S=50 μν/Κ， 进一步表明微 区塞贝克定量表征技术的可行性及结果的准确性。 上述实例表明了基于原子力显微镜所建立的纳米热电塞贝克系数原位
定量表征新方法解决了纳米热电材料无需直接测量温度变化即可直接原位 定量表征纳米热电塞贝克系数参量这一关键技术难题。 该新型纳米表征装 置实现了纳米热电塞贝克系数所需的二倍频及三倍频谐波信号原位同时 激发、 原位同步表征， 拓展了现有商用原子力显微镜所不具有的纳米热电 物性评价功能， 为深入研究纳米热电材料， 特别是纳米热电线等低维热电 材料的热电输运理论及器件的深入发展提供了重要的原位、 定量、 纳米表 征新方法。
综上所述， 本申请突出优点在于将原子力显微镜纳米检测功能、 宏观热 导三倍频测试原理、 焦耳热效应原理及宏观塞贝克系数测试原理相结合， 提 出了一种基于 AFM 热探针所诱导的谐波效应来表征纳米塞贝克系数的新原 理， 并藉此建立起一种无需直接测量温度变化而在 AFM平台上实现表征纳米 塞贝克系数的原位谐波激发及检测技术。该新型方法不仅完全不需宏观塞贝 克系数测试所必需的温度变化的直接测量， 而且具有纳米温差、 纳米塞贝克 谐波信号原位同时激发、 原位同步表征的独特功能， 且具有高分辨率、 高灵 敏度、 高信噪比、 测试直接等优点； 同时其关键技术装置结构简单、 兼容性 强， 适宜广泛推广和应用。 由此， 提供了一种基于新表征原理的纳米热电塞 贝克系数表征新方法， 可望在纳米材料、 能源材料等战略性新兴材料及其产 业中获得重要应用。
前面提供了对较佳实施例的描述， 以使本领域内的任何技术人员可使用 或利用本申请。对这些实施例的各种修改对本领域内的技术人员是显而易见 的， 可把这里所述的总的原理应用到其他实施例而不使用创造性。 因而， 本 申请将不限于这里所示的实施例， 而应依据符合这里所揭示的原理和新特征 的最宽范围。
Claims
权利要求书
L一种基于原子力显微镜的纳米热电塞贝克系数原位定量表征装置，用 于检测一被测纳米热电材料样品的微区塞贝克系数， 其特征在于， 所述装置 进一步包括：
一谐波信号的原子力显微镜原位激励平台， 用于提供发展纳米热电塞 贝克系数原位表征装置的原子力显微镜平台， 并原位同时激发纳米热电材 料微区二倍频、 三倍频谐波信号；
一纳米热电塞贝克系数原位检测平台， 用于实现所述纳米热电材料微区 二倍频、 三倍频的原位实时检测和处理， 并显示微区塞贝克系数热电参量的 原位表征结果。
2. 根据权利要求 1 所述的基于原子力显微镜的纳米热电塞贝克系 数原位定量表征装置， 其特征在于， 所述谐波信号的原子力显微镜原位激 励平台进一歩包括：
一原子力显微镜平台， 一热电检测探针， 一热电参考探针， 两个可调 电阻网络， 一信号发生器， 一热电材料， 一陶瓷绝缘层， 一磁性底座， 一 信号传输端， 一微区二倍频谐波电压信号输出端口， 一微区三倍频谐波电 压信号输出端口， 其中， 所述被测热电材料样品通过下垫所述陶瓷绝缘层置 于所述磁性底座上， 所述热电检测探针、 热电参考探针、 两个可调电阻网 络和信号发生器组成一惠斯通电桥， 所述热电检测探针置于所述被测热电 材料样品上并接触， 以检测所述被测热电材料样品激励点的电压； 所述微 区二倍频电压信号输出端口的第一端通过所述信号传输端接收所述被测热 电材料样品另一区域的电压信号，所述微区二倍频电压信号输出端口的第二 端与所述惠斯通电桥接地端相连； 所述微区三倍频电压信号输出端口的第 一端连接所述热电检测探针与所述惠斯通电桥相连端， 其第二端连接所述 热电参考探针与所述惠斯通电桥相连端。
3.根据权利要求 2所述的基于原子力显微镜的纳米热电塞贝克系数原位 定量表征装置， 其特征在于，
所述原子力显微镜平台的工作模式为接触模式。
4.根据权利要求 2所述的基于原子力显微镜的纳米热电塞贝克系数原位 定量表征装置， 其特征在于，
所述热电检测探针为一具热敏电阻特性的探针， 同时具有微区激励源、 信号传感器及检测源的功能； 所述热电检测探针为原子力显微镜接触模式， 其作为反馈参量的微悬臂形变量为 0. 1-5 nm, 与所述被测热电材料样品互作 用接触面积的直径为 30-100 nm。
5.根据权利要求 2所述的基于原子力显微镜的纳米热电塞贝克系数原位 定量表征装置， 其特征在于，
所述热电探针的工作频率范围为 100 Hz-10 kHz , 工作电流范围为
1mA - 100 mA。
6.根据权利要求 1所述的基于原子力显微镜的纳米热电塞贝克系数原位 定量表征装置， 其特征在于， 所述纳米热电塞贝克系数原位检测平台进一步 包括：
一高灵敏度锁相放大器， 一前端回路处理模块， 一高灵敏度锁相放大 器， 一数据处理和显示系统等， 用于实现微弱二倍频和三倍频谐波电压信号 的原位实时检测、 处理和显示微区塞贝克系数热电参量的原位表征结果。
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| CN103586590A (zh) * | 2013-11-12 | 2014-02-19 | 温州大学 | 基于焦耳热的纳米焊接方法 |
| CN103901081B (zh) * | 2014-03-19 | 2016-03-30 | 中国矿业大学 | ZnO-In2O3纳米半导体晶体气敏材料制备方法 |
| CN103901234B (zh) * | 2014-04-16 | 2018-01-09 | 中国科学院上海硅酸盐研究所 | 多铁性材料纳米尺度畴结构的原位集成表征装置 |
| CN110579628B (zh) * | 2018-06-11 | 2022-05-13 | 中国科学院上海硅酸盐研究所 | 一种纳米尺度极低热导的原位表征装置 |
| CN112881464B (zh) * | 2021-01-20 | 2022-12-09 | 中国科学院工程热物理研究所 | 一种直接原位综合测量微纳材料热电性能的方法及装置 |
| CN112857456A (zh) * | 2021-02-04 | 2021-05-28 | 上海大学 | 一种针对块体材料的多个参数集成表征装置及方法 |
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