公开(公告)号：US08719961B2

公开(公告)日：2014-05-06

申请号：US13291480

申请日：2011-11-08

申请人： Sergei V. Kalinin ,  Nina Balke ,  Amit Kumar ,  Nancy J. Dudney ,  Stephen Jesse

发明人： Sergei V. Kalinin ,  Nina Balke ,  Amit Kumar ,  Nancy J. Dudney ,  Stephen Jesse

IPC分类号： G01Q60/60

CPC分类号： G01Q60/60 ,  G01Q60/02 ,  G01Q60/30

摘要： A method and system for probing mobile ion diffusivity and electrochemical reactivity on a nanometer length scale of a free electrochemically active surface includes a control module that biases the surface of the material. An electrical excitation signal is applied to the material and induces the movement of mobile ions. An SPM probe in contact with the surface of the material detects the displacement of mobile ions at the surface of the material. A detector measures an electromechanical strain response at the surface of the material based on the movement and reactions of the mobile ions. The use of an SPM tip to detect local deformations allows highly reproducible measurements in an ambient environment without visible changes in surface structure. The measurements illustrate effective spatial resolution comparable with defect spacing and well below characteristic grain sizes of the material.

摘要翻译： 用于探测自由电化学活性表面的纳米尺度上的移动离子扩散率和电化学反应性的方法和系统包括偏压材料表面的控制模块。 电激励信号被施加到材料并引起移动离子的移动。 与材料表面接触的SPM探针检测到材料表面上的移动离子的位移。 检测器基于移动离子的运动和反应来测量材料表面处的机电应变响应。 使用SPM尖端来检测局部变形允许在周围环境中进行高度可重复的测量，而没有表面结构的可见变化。 测量结果说明了有效的空间分辨率与缺陷间距相当，远远低于材料的特征晶粒尺寸。

公开(公告)号：US20120125783A1

公开(公告)日：2012-05-24

申请号：US13291480

申请日：2011-11-08

申请人： Sergei V. Kalinin ,  Nina Balke ,  Amit Kumar ,  Nancy J. Dudney ,  Stephen Jesse

发明人： Sergei V. Kalinin ,  Nina Balke ,  Amit Kumar ,  Nancy J. Dudney ,  Stephen Jesse

IPC分类号： G01N27/26 ,  G01N27/417 ,  G01N27/403

CPC分类号： G01Q60/60 ,  G01Q60/02 ,  G01Q60/30

摘要： A method and system for probing mobile ion diffusivity and electrochemical reactivity on a nanometer length scale of a free electrochemically active surface includes a control module that biases the surface of the material. An electrical excitation signal is applied to the material and induces the movement of mobile ions. An SPM probe in contact with the surface of the material detects the displacement of mobile ions at the surface of the material. A detector measures an electromechanical strain response at the surface of the material based on the movement and reactions of the mobile ions. The use of an SPM tip to detect local deformations allows highly reproducible measurements in an ambient environment without visible changes in surface structure. The measurements illustrate effective spatial resolution comparable with defect spacing and well below characteristic grain sizes of the material.

摘要翻译： 用于探测自由电化学活性表面的纳米尺度上的移动离子扩散率和电化学反应性的方法和系统包括偏压材料表面的控制模块。 电激励信号被施加到材料并引起移动离子的移动。 与材料表面接触的SPM探针检测到材料表面上的移动离子的位移。 检测器基于移动离子的运动和反应来测量材料表面处的机电应变响应。 使用SPM尖端来检测局部变形允许在周围环境中进行高度可重复的测量，而没有表面结构的可见变化。 测量结果说明了有效的空间分辨率与缺陷间距相当，远远低于材料的特征晶粒尺寸。

公开(公告)号：US08752211B2

公开(公告)日：2014-06-10

申请号：US13566327

申请日：2012-08-03

申请人： Sergei V. Kalinin ,  Nina Balke ,  Albina Y. Borisevich ,  Stephen Jesse ,  Petro Maksymovych ,  Yunseok Kim ,  Evgheni Strelcov

发明人： Sergei V. Kalinin ,  Nina Balke ,  Albina Y. Borisevich ,  Stephen Jesse ,  Petro Maksymovych ,  Yunseok Kim ,  Evgheni Strelcov

IPC分类号： G01Q60/44

CPC分类号： G01Q60/30

摘要： An excitation voltage biases an ionic conducting material sample over a nanoscale grid. The bias sweeps a modulated voltage with increasing maximal amplitudes. A current response is measured at grid locations. Current response reversal curves are mapped over maximal amplitudes of the bias cycles. Reversal curves are averaged over the grid for each bias cycle and mapped over maximal bias amplitudes for each bias cycle. Average reversal curve areas are mapped over maximal amplitudes of the bias cycles. Thresholds are determined for onset and ending of electrochemical activity. A predetermined number of bias sweeps may vary in frequency where each sweep has a constant number of cycles and reversal response curves may indicate ionic diffusion kinetics.

摘要翻译： 激发电压在纳米尺度网格上偏置离子导电材料样品。 偏置以最大幅度增加扫描调制电压。 当前的响应是在网格位置测量的。 电流响应反转曲线映射到偏置周期的最大幅度。 对于每个偏置周期，反转曲线在电网上进行平均，并映射到每个偏置周期的最大偏移幅度。 平均反转曲线区域映射到偏置周期的最大幅度。 确定电化学活性的起始和结束的阈值。 预定数量的偏置扫描可以在频率上变化，其中每个扫描具有恒定的循环次数，反转响应曲线可以指示离子扩散动力学。

公开(公告)号：US20140041085A1

公开(公告)日：2014-02-06

申请号：US13566327

申请日：2012-08-03

申请人： Sergei V. Kalinin ,  Nina Balke ,  Albina Y. Borisevich ,  Stephen Jesse ,  Petro Maksymovych ,  Yunseok Kim ,  Evgheni Strelcov

发明人： Sergei V. Kalinin ,  Nina Balke ,  Albina Y. Borisevich ,  Stephen Jesse ,  Petro Maksymovych ,  Yunseok Kim ,  Evgheni Strelcov

IPC分类号： G01Q60/44

CPC分类号： G01Q60/30

摘要： An excitation voltage biases an ionic conducting material sample over a nanoscale grid. The bias sweeps a modulated voltage with increasing maximal amplitudes. A current response is measured at grid locations. Current response reversal curves are mapped over maximal amplitudes of the bias cycles. Reversal curves are averaged over the grid for each bias cycle and mapped over maximal bias amplitudes for each bias cycle. Average reversal curve areas are mapped over maximal amplitudes of the bias cycles. Thresholds are determined for onset and ending of electrochemical activity. A predetermined number of bias sweeps may vary in frequency where each sweep has a constant number of cycles and reversal response curves may indicate ionic diffusion kinetics.

摘要翻译： 激发电压在纳米尺度网格上偏置离子导电材料样品。 偏置以最大幅度增加扫描调制电压。 当前的响应是在网格位置测量的。 电流响应反转曲线映射到偏置周期的最大幅度。 对于每个偏置周期，反转曲线在电网上进行平均，并映射到每个偏置周期的最大偏置幅度。 平均反转曲线区域映射到偏置周期的最大幅度。 确定电化学活性的起始和结束的阈值。 预定数量的偏置扫描可以在频率上变化，其中每个扫描具有恒定的循环次数，反转响应曲线可以指示离子扩散动力学。

公开(公告)号：US20110004967A1

公开(公告)日：2011-01-06

申请号：US12792477

申请日：2010-06-02

申请人： Stephen Jesse ,  Sergei V. Kalinin

发明人： Stephen Jesse ,  Sergei V. Kalinin

IPC分类号： G01Q60/00

CPC分类号： G01Q20/00 ,  B82Y35/00 ,  G01Q10/06 ,  G01Q30/04 ,  G01Q60/32

摘要： Methods and apparatus are described for scanning probe microscopy. A method includes generating a band excitation (BE) signal having finite and predefined amplitude and phase spectrum in at least a first predefined frequency band; exciting a probe using the band excitation signal; obtaining data by measuring a response of the probe in at least a second predefined frequency band; and extracting at least one relevant dynamic parameter of the response of the probe in a predefined range including analyzing the obtained data. The BE signal can be synthesized prior to imaging (static band excitation), or adjusted at each pixel or spectroscopy step to accommodate changes in sample properties (adaptive band excitation). An apparatus includes a band excitation signal generator; a probe coupled to the band excitation signal generator; a detector coupled to the probe; and a relevant dynamic parameter extractor component coupled to the detector, the relevant dynamic parameter extractor including a processor that performs a mathematical transform selected from the group consisting of an integral transform and a discrete transform.

摘要翻译： 描述扫描探针显微镜的方法和装置。 一种方法包括在至少第一预定频带中产生具有有限和预定义的幅度和相位频谱的频带激励（BE）信号; 使用频带激发信号激发探头; 通过在至少第二预定频带中测量所述探测器的响应来获得数据; 以及在包括分析所获得的数据的预定范围内提取所述探测器的响应的至少一个相关动态参数。 可以在成像（静态带激发）之前合成BE信号，或者在每个像素或光谱步骤调整以适应样品性质（自适应带激发）的变化。 一种装置包括：带激发信号发生器; 耦合到频带激励信号发生器的探头; 耦合到所述探针的检测器; 以及耦合到所述检测器的相关动态参数提取器组件，所述相关动态参数提取器包括执行从由积分变换和离散变换组成的组中选择的数学变换的处理器。

公开(公告)号：US08484759B2

公开(公告)日：2013-07-09

申请号：US12857894

申请日：2010-08-17

申请人： Stephen Jesse ,  Sergei V. Kalinin ,  Maxim P. Nikiforov

发明人： Stephen Jesse ,  Sergei V. Kalinin ,  Maxim P. Nikiforov

IPC分类号： G01Q60/58

CPC分类号： G01Q60/58

摘要： An approach for the thermomechanical characterization of phase transitions in polymeric materials (polyethyleneterephthalate) by band excitation acoustic force microscopy is developed. This methodology allows the independent measurement of resonance frequency, Q factor, and oscillation amplitude of a tip-surface contact area as a function of tip temperature, from which the thermal evolution of tip-surface spring constant and mechanical dissipation can be extracted. A heating protocol maintained a constant tip-surface contact area and constant contact force, thereby allowing for reproducible measurements and quantitative extraction of material properties including temperature dependence of indentation-based elastic and loss moduli.

摘要翻译： 开发了通过频带激发声力显微镜对聚合物材料（聚对苯二甲酸乙二醇酯）中的相变的热机械表征的方法。 该方法允许独立测量作为尖端温度的函数的尖端表面接触面积的谐振频率，Q因子和振荡振幅，从而可以提取尖端表面弹簧常数和机械耗散的热演变。 加热方案保持了不变的顶表面接触面积和恒定的接触力，从而允许重复测量和定量提取材料性能，包括基于压痕的弹性和损耗模量的温度依赖性。

公开(公告)号：US20110041223A1

公开(公告)日：2011-02-17

申请号：US12857894

申请日：2010-08-17

申请人： Stephen Jesse ,  Sergei V. Kalinin ,  Maxim P. Nikiforov

发明人： Stephen Jesse ,  Sergei V. Kalinin ,  Maxim P. Nikiforov

IPC分类号： G01Q20/00

CPC分类号： G01Q60/58

摘要： An approach for the thermomechanical characterization of phase transitions in polymeric materials (polyethyleneterephthalate) by band excitation acoustic force microscopy is developed. This methodology allows the independent measurement of resonance frequency, Q factor, and oscillation amplitude of a tip-surface contact area as a function of tip temperature, from which the thermal evolution of tip-surface spring constant and mechanical dissipation can be extracted. A heating protocol maintained a constant tip-surface contact area and constant contact force, thereby allowing for reproducible measurements and quantitative extraction of material properties including temperature dependence of indentation-based elastic and loss moduli.

摘要翻译： 开发了通过频带激发声力显微镜对聚合物材料（聚对苯二甲酸乙二醇酯）中的相变的热机械表征的方法。 该方法允许独立测量作为尖端温度的函数的尖端表面接触面积的谐振频率，Q因子和振荡振幅，从而可以提取尖端表面弹簧常数和机械耗散的热演变。 加热方案保持了不变的顶表面接触面积和恒定的接触力，从而允许重复测量和定量提取材料性能，包括基于压痕的弹性和损耗模量的温度依赖性。

公开(公告)号：US08448502B2

公开(公告)日：2013-05-28

申请号：US12792477

申请日：2010-06-02

申请人： Stephen Jesse ,  Sergei V. Kalinin

发明人： Stephen Jesse ,  Sergei V. Kalinin

IPC分类号： G01B5/28 ,  G01Q30/00 ,  G01Q60/00

CPC分类号： G01Q20/00 ,  B82Y35/00 ,  G01Q10/06 ,  G01Q30/04 ,  G01Q60/32

摘要： Methods and apparatus are described for scanning probe microscopy. A method includes generating a band excitation (BE) signal having finite and predefined amplitude and phase spectrum in at least a first predefined frequency band; exciting a probe using the band excitation signal; obtaining data by measuring a response of the probe in at least a second predefined frequency band; and extracting at least one relevant dynamic parameter of the response of the probe in a predefined range including analyzing the obtained data. The BE signal can be synthesized prior to imaging (static band excitation), or adjusted at each pixel or spectroscopy step to accommodate changes in sample properties (adaptive band excitation). An apparatus includes a band excitation signal generator; a probe coupled to the band excitation signal generator; a detector coupled to the probe; and a relevant dynamic parameter extractor component coupled to the detector, the relevant dynamic parameter extractor including a processor that performs a mathematical transform selected from the group consisting of an integral transform and a discrete transform.

摘要翻译： 描述扫描探针显微镜的方法和装置。 一种方法包括在至少第一预定频带中产生具有有限和预定义的幅度和相位频谱的频带激励（BE）信号; 使用频带激发信号激发探头; 通过在至少第二预定频带中测量所述探测器的响应来获得数据; 以及在包括分析所获得的数据的预定范围内提取所述探测器的响应的至少一个相关动态参数。 可以在成像（静态带激发）之前合成BE信号，或者在每个像素或光谱步骤调整以适应样品性质（自适应带激发）的变化。 一种装置包括：带激发信号发生器; 耦合到频带激励信号发生器的探头; 耦合到所述探针的检测器; 以及耦合到所述检测器的相关动态参数提取器组件，所述相关动态参数提取器包括执行从由积分变换和离散变换组成的组中选择的数学变换的处理器。

公开(公告)号：US07775086B2

公开(公告)日：2010-08-17

申请号：US11515348

申请日：2006-09-01

申请人： Stephen Jesse ,  Sergei V. Kalinin

发明人： Stephen Jesse ,  Sergei V. Kalinin

IPC分类号： G01B5/28

CPC分类号： G01Q20/00 ,  B82Y35/00 ,  G01Q10/06 ,  G01Q30/04 ,  G01Q60/32

摘要： Methods and apparatus are described for scanning probe microscopy. A method includes generating a band excitation (BE) signal having finite and predefined amplitude and phase spectrum in at least a first predefined frequency band; exciting a probe using the band excitation signal; obtaining data by measuring a response of the probe in at least a second predefined frequency band; and extracting at least one relevant dynamic parameter of the response of the probe in a predefined range including analyzing the obtained data. The BE signal can be synthesized prior to imaging (static band excitation), or adjusted at each pixel or spectroscopy step to accommodate changes in sample properties (adaptive band excitation). An apparatus includes a band excitation signal generator; a probe coupled to the band excitation signal generator; a detector coupled to the probe; and a relevant dynamic parameter extractor component coupled to the detector, the relevant dynamic parameter extractor including a processor that performs a mathematical transform selected from the group consisting of an integral transform and a discrete transform.

摘要翻译： 描述扫描探针显微镜的方法和装置。 一种方法包括在至少第一预定频带中产生具有有限和预定义的幅度和相位频谱的频带激励（BE）信号; 使用频带激发信号激发探头; 通过在至少第二预定频带中测量所述探测器的响应来获得数据; 以及在包括分析所获得的数据的预定范围内提取所述探测器的响应的至少一个相关动态参数。 可以在成像（静态带激发）之前合成BE信号，或者在每个像素或光谱步骤调整以适应样品性质（自适应带激发）的变化。 一种装置包括：带激发信号发生器; 耦合到频带激励信号发生器的探头; 耦合到所述探针的检测器; 以及耦合到所述检测器的相关动态参数提取器组件，所述相关动态参数提取器包括执行从由积分变换和离散变换组成的组中选择的数学变换的处理器。

公开(公告)号：US20100011471A1

公开(公告)日：2010-01-14

申请号：US11515348

申请日：2006-09-01

申请人： Stephen Jesse ,  Sergei V. Kalinin

发明人： Stephen Jesse ,  Sergei V. Kalinin

IPC分类号： G01N13/10

CPC分类号： G01Q20/00 ,  B82Y35/00 ,  G01Q10/06 ,  G01Q30/04 ,  G01Q60/32

摘要： Methods and apparatus are described for scanning probe microscopy. A method includes generating a band excitation (BE) signal having finite and predefined amplitude and phase spectrum in at least a first predefined frequency band; exciting a probe using the band excitation signal; obtaining data by measuring a response of the probe in at least a second predefined frequency band; and extracting at least one relevant dynamic parameter of the response of the probe in a predefined range including analyzing the obtained data. The BE signal can be synthesized prior to imaging (static band excitation), or adjusted at each pixel or spectroscopy step to accommodate changes in sample properties (adaptive band excitation). An apparatus includes a band excitation signal generator; a probe coupled to the band excitation signal generator; a detector coupled to the probe; and a relevant dynamic parameter extractor component coupled to the detector, the relevant dynamic parameter extractor including a processor that performs a mathematical transform selected from the group consisting of an integral transform and a discrete transform.

摘要翻译： 描述扫描探针显微镜的方法和装置。 一种方法包括在至少第一预定频带中产生具有有限和预定义的幅度和相位频谱的频带激励（BE）信号; 使用频带激发信号激发探头; 通过在至少第二预定频带中测量所述探测器的响应来获得数据; 以及在包括分析所获得的数据的预定范围内提取所述探测器的响应的至少一个相关动态参数。 可以在成像（静态带激发）之前合成BE信号，或者在每个像素或光谱步骤调整以适应样品性质（自适应带激发）的变化。 一种装置包括：带激发信号发生器; 耦合到频带激励信号发生器的探头; 耦合到所述探针的检测器; 以及耦合到所述检测器的相关动态参数提取器组件，所述相关动态参数提取器包括执行从由积分变换和离散变换组成的组中选择的数学变换的处理器。