• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Dynamic method of force microscopy and microscope to simultaneously acquire topography images and force maps. Dynamic method of force microscopy to acquire surface images, directly determine the force exerted on a material that also allows quantifying non-topographic properties, based on exciting the microscope of a force microscope at a frequency less than the frequency resonance and keep constant the amplitude of oscillation of the same and the force exerted on the surface while acquiring an image. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2732721A1
    申请号:ES201830497
    申请日:2018-05-23
    公开日:2019-11-25
    发明作者:García Ricardo García；Amo Carlos Alvarez
    申请人:Consejo Superior de Investigaciones Cientificas CSIC；
    IPC主号:
    专利说明:

    [0001]
    [0002]
    [0003] OBJECT OF THE INVENTION AND SECTOR OF THE TECHNIQUE
    [0004]
    [0005] The present invention relates to a method of using an atomic force microscope, exciting the micro lever at a lower frequency than the resonant frequency, the amplitude of the oscillation and the force exerted being the parameters that remain constant during the process of Acquisition of a topography image. The microlever deflection and the excitation force are used to directly determine the instantaneous force and, from it, quantify the nanomechanical properties of a sample to be measured.
    [0006]
    [0007] This method allows to obtain an image of the topography of the surface and, at the same time, to obtain the dependence of the force with respect to the distance of the tip of the microscope and the surface of the sample. Various physical properties of the material can be determined from the dependence of force on distance.
    [0008]
    [0009] The present dynamic force microscopy method finds application in the field of scientific research and technological sectors that require topographic characterization and determination with high spatial resolution of the interactions between the microscope probe and the sample. These sectors include pharmacy, food, micro and nanotechnology, polymers, etc. The method is applicable to all types of samples, whether they are formed by organic, polymeric, biological, semiconductor, metallic or inorganic materials and the sample being immersed in a liquid, gaseous or vacuum medium.
    [0010]
    [0011] BACKGROUND OF THE INVENTION
    [0012]
    [0013] The force microscope also called atomic force microscope in this invention or AFM, (for the acronym in English atomic twist microscopy) allows the acquisition of high resolution images of a wide range of materials. Therefore, it has become one of the most relevant techniques for characterizing properties to nanometric scale As a result of their large spatial resolution (lateral and vertical), atomic force microscopes (AFM) have been introduced both in research laboratories and in innovation and quality control departments in various industrial sectors (microelectronics, polymers, food).
    [0014]
    [0015] One of the singularities of force microscopy is its ability to obtain information on various physical properties of a material such as Young's modulus, Hamaker's constant, adhesion force or viscoelasticity coefficient. This capability is known generically as force spectroscopy (HJ Butt, B. Capella and M. Kappl, "Force Measurements with the Atomic Force Microscope: Technique, Interpretation and Applications" Suri. Sci. Rep. 591-152 (2005)).
    [0016]
    [0017] Force spectroscopy requires the determination of the dependence of force interaction with distance at each point on the surface. The acquisition of force curves simultaneously with the acquisition of the topographic image has given rise to a powerful microscopy method that is generically known as force volume. These methods operate at low frequencies (1-100 Hz) typically far from the resonance frequency of the tips that can be found in the range between 20-200 kHz, which implies that the acquisition of a force map requires times of several tens of minutes The pulsed force method ( A. Rosa-Zeiser, E. Weilandt, S. Hild and O. Marti. "The simultaneous measurement of elastic, electrostatic and adhesive properties by scanning force microscopy: pulsed-force mode operation." Measurement Science and Technology 8 ( 11), 1333 ( 1997)) oscillates the piezo that moves the sample vertically at frequencies between 100 Hz and 2 kHz, which allows the determination of mechanical properties more quickly, although the maximum force applied is relatively high (of tens of nN) .A variation of the previous method is the method of jumping mode ' that allows to reduce the lateral force exerted on the sample during the acquisition of the image (F. Moreno-Herrero, PJ de Pablo, J. Colchero, J. Gómez-Herrero, AMBaró, "The role of shear forces in scanning force microscopy: a comparison between the jumping mode and tapping mode", Surface Science 453, 152-158 (2000). More recently, it has made an update Ion of the methods based on the acquisition of force curves as described in the invention of the patent document US 20120131702 A1 'peak force tapping', where certain improvements are introduced such as the use of sinusoidal displacements and the use of force maximum as feedback parameter. This method allows to obtain the force curves against distance and from them extract nanomechanical properties such as Young's modulus (Medalsy, DI; Muller, DJ Nanomechanichal Properties of Proteins and Membranes Depend on Loading Rate and Electrostaic Interactions. ACS Nano 7, 2642-2650 (2013)). Although this method has been applied with frequencies of several kHz, it presents stability problems in the determination of the force when the frequency of the movement of the tip is increased due to the contributions of the hydrodynamic and inertial forces that are not considered in said method. The algorithm used in peal forced tapping is not valid when the frequency approaches the resonance frequency of the tip. The characteristics of this method prevent it from determining dissipative properties such as viscosity. The values of these forces depend on the frequency relationship between the frequency of the movement and the resonance frequency of the micro lever (CA Amo and R. Garcia, “Fundamental High-Speed Limits in Single Molecule, Single-Cell, and Nanoscale Force Spectroscopies ", ACS Nano 10, 7117-7124 (2016). These factors prevent surface characterization from being carried out at high frequencies with the micro-levers currently available.
    [0018]
    [0019] On the other hand, dynamic AFM methods such as bimodal, described in US 7958563 B2 and US 7921466 B2 and in several scientific publications (ET Herruzo, AP Perrino, R. Garcia, "Fast nanomechanical spectroscopy of soft matter", Nat. Commun. 5, 3126 ( 2014); Labuda, A .; Kocun, M .; Meinhold, W .; Walters, D .; Proksch, R. Generalized Hertz Model for Bimodal Nanomechanical Mapping. Beilstein J. Nanotechnol. 7, 970-982 ( 2014)) allow obtaining simultaneously the topography and certain properties of the material such as Young's modulus or viscosity coefficient. The bimodal method is a parametric method and does not allow to obtain directly the dependence of force against distance or time.
    [0020]
    [0021] In summary, none of the methods described above solve the problems that would be faced when acquiring high resolution images in topography, at high speed and simultaneously with the acquisition at each point of the surface of the force curve versus distance with a high degree of numerical precision and control of the force exerted on the sample. From the force versus distance curves it is possible to obtain various mechanical properties such as Young's modulus. The method proposed by the present invention provides a solution to the above problems.
    [0022]
    [0023] DESCRIPTION OF THE INVENTION
    [0024] The present invention relates to a dynamic force microscopy method that combines the acquisition of surface images (typically topography) with the determination of the force curve as a function of time or distance at each point on the surface, and from it quantify the non-topographic properties of the material. The method is based on exciting the microscope's micro lever at a lower frequency than the resonance frequency, obtaining a surface image with a feedback that maintains a constant value of the force and other feedback that maintains the amplitude of oscillation of the micro lever at a constant value using two feedback loops; a first feedback loop exerted on the force that is applied on the sample and a second feedback loop exerted on the amplitude of the oscillation (Figure 1).
    [0025]
    [0026] In this way a feedback loop controls the maximum force that is exerted in each cycle on the Fpeak sample (9) by the tip, responsible for regulating the average distance between the tip of the micro lever and the sample (10) until it is reached a fixed value, which remains constant, of the total force, thus controlling topographic feedback (11).
    [0027]
    [0028] And the feedback loop of the amplitude A (8), varies the excitation amplitude of the micro lever by an excitation force (5), keeping said amplitude constant, Asp.
    [0029]
    [0030] At each point on the surface, the deflection of the micro lever and the excitation force are measured as a function of time. From them and from the determination of the hydrodynamic and inertial components of the force, the interaction force is obtained as a function of time. Figure 2 shows a schematic of the procedure to obtain the instantaneous force from the microscope feedback parameters and loops. In one embodiment of the method of the present invention, optimal conditions have been obtained that allow for speed and resolution on the contributions of the force exerted on the sample to be improved. To find the required estimate that allows a better performance, the instantaneous deflection of the micro lever, the excitation force as a function of the time produced by its oscillation and the sinusoidal behavior of the deflection of the micro lever are used to determine the force in function of the time exerted on the sample. The selection of the above parameters comes from the description of the equation of the movement of the system, which according to the dynamic method of force microscopy, object of the present invention, we define as:
    [0031] m ^ ¿= ~ kz ( t) - ^ ^ Fts + Fd (í) cos ^ í (E.1) where k, z, Asp, w0, Fd ( t) are, respectively, the force constant, the deflection instantaneous, the reference amplitude of the oscillation, the angular frequency of excitation and the amplitude of the excitation force of the micro lever; ro represents the relationship between the angular frequency of excitation of the micro lever and the angular frequency of resonance, always fulfilling the condition w <w0.
    [0032]
    [0033] According to the dynamic force microscopy method, object of this invention, the deflection of the micro lever can be approximated as
    [0034] z (t) = z0 Cospid Asp (E.2) According to the dynamic method of force microscopy, object of this invention, the force exerted on the sample can then be expressed as
    [0035] Fts = kz ( t) - ^ - cos <¿> t - wQ - sinotí - Fd ( t) eos Mt (E.3a) Fts = kz ( t) End Fhd - Fd ( t ) eos a t (E3.b) where ro = w / w0.
    [0036]
    [0037] Thus, assuming E.1, the present dynamic method of force microscopy is used, which allows the dependence of force on time and / or distance to be determined by the following procedure:
    [0038]
    [0039] a) place on the head of a force microscope (1) a micro lever (2) with a tip at its end (3), which interacts with the sample (4), with the tip presenting at least one vibration mode
    [0040] b) have two elements, an excitation unit) (5) to vibrate the micro lever (2) and a displacement unit (6) to move the micro lever (2) on the sample (4) or part of it ;
    [0041] c) send to the excitation unit (5), associated with the micro lever of the microscope head of forces (1) the excitation signal generated by (5) and which make the micro lever vibrate)
    [0042] d) calibrate the following parameters associated with the operation of the micro lever as described in the specialized literature (A. Labuda, M. Kocun, M. Lysy, T. Walsh, J. Meinhold, T. Proksch, W. Meinhold, C Anderson, R. Proksch, "Calibration of higher eigenmodes of cantilevers" Review of Scientific Instruments 87. 073705 (20016)):
    [0043]
    [0044] - force constant, k;
    [0045] - quality factor, Q ;
    [0046] - resonance frequency of the micro lever, f0, w0 = 2-n-f0;
    [0047] - optical sensitivity of the photodiode or detection system of the system
    [0048] - radius, R, of the tip of the micro lever;
    [0049] d) detect, by means of a system adapted for this purpose, the deflection signal of the micro lever (7);
    [0050] e) detect, by means of a system adapted to this effect, the deflection of the micro lever;
    [0051] f) estimate the inertial contribution to the force through the hypothesis of a sinusoidal deflection from:
    [0052] kasp
    [0053] Fj ' = - m A 2 cos ^ t
    [0054] g) estimate the contribution to force due to the hydrodynamic term from:
    [0055]
    [0056]
    [0057]
    [0058] h) check that the following conditions are met according to the following stages:
    [0059] h.1) the excitation frequency of the micro lever is much lower than the resonance frequency of the micro lever, preferably at least 10 times lower.
    [0060] h.2) verify that the inertial force F¡ is much less than at least one of the components of equation E.3b that contribute to calculate the total force exerted on the sample.
    [0061] i) set the feedback loops that comprise
    [0062] - a feedback loop that controls the maximum force that is exerted on each cycle on the Fpeak sample (9) by the tip, responsible for regulating the average distance between the tip of the micro lever and the sample (10) until a fixed value, which remains constant, of the total force, thus controlling topographic feedback (11).
    [0063] - a feedback loop of the amplitude A (8), where the amplitude of excitation of the micro lever is varied by an excitation force (5), keeping said amplitude constant, Asp.
    [0064]
    [0065] j) detect, by means of a system, (7) adapted to the effect, typically a photodiode, the signal of deflection of the lever and from it obtain the curve of forces as a function of time or distance,
    [0066] k) acquire a topography image by and associate a force curve with each pixel of it
    [0067] It can be transformed through the use of analytical formulas, the force depending on the tip-sample separation in parametric maps of the properties of the sample and thus obtain all kinds of mechanical, electrical, etc. properties of the sample qualitatively and even quantitatively .
    [0068]
    [0069] According to the present dynamic force microsocopy method, in step (b) of the method in which the excitation signal is generated, the micro lever is excited according to a sinusoidal signal of a lower frequency (but which can be of the same order of magnitude unlike the prior art methods that work at much lower frequencies), than the resonance frequency of the micro lever, expressed according to the following mathematical relationship:
    [0070] F d (0 = F0 ( t) co s (2 n ft) (E.4) where F0 is the excitation amplitude of the excitation force and f is the excitation frequency. The amplitude of the excitation force is calculated at each instant from the feedback loop of the amplitude of the micro lever as:
    [0071]
    [0072] where A, Asp, P, I are, respectively, the amplitude of the oscillation, the value of the reference amplitude, the proportional gain and the integral gain.
    [0073] According to a possible embodiment, in step (i) of the dynamic force microscopy method, the deflection of the micro lever, z, and the excitation force is used to find the instantaneous force between the tip and the sample according to the following mathematical relationship:
    [0074]
    [0075]
    [0076]
    [0077] This formula is valid as long as condition h.2 is met, otherwise the force is calculated by the expression E.3a.
    [0078]
    [0079] According to the present dynamic force microscopy method, in step (j) the instantaneous distance between the tip and the sample is determined from the equation,
    [0080] d = a0 z ( t) zc - Asp eos 2 n ft (E.7) where a0 is a molecular parameter, as reference is worth 0.165 nm, zc is the average height of the micro lever on the sample and z ( t) the deflection . The average distance between the tip of the micro lever and the sample is optionally controlled, keeping constant the maximum value of the force between the tip and the sample, Fts (t) in another feedback loop, while the micro lever moves along and sample width.
    [0081] According to a possible embodiment, in step (k) of the method the data shown in the force curves are converted into parametric maps of sample properties, by adjusting the force curve to different interaction models.
    [0082]
    [0083] In a particular case the interaction force can be modeled according to Sneddon's theory (Sneddon, IN "The Relation Between Load and Penetration in the Axisymmetric Boussinesq Problem for a Punch of Arbitrary Profile." 1965, Intemational Journal of Engineering Science, 347-57.), And Young's effective module, Eeff, is determined from the following equation
    [0084]
    [0085] F = aEeffSP (E.8)
    [0086]
    [0087] where 5 is the indentation; a is a coefficient that depends on the geometry and the Poisson coefficient and is a geometric factor that depends on the shape of the tip. For example for a semi-spherical tip a = 4/3 R1 / 2 and p = 3/2. Indentation is determined from
    [0088] S = —d ( when d < 0) (E.9) where d is the distance between the tip and the sample.
    [0089]
    [0090] According to an embodiment of the present dynamic method for quantifying non-topographic properties in force microscopy, the microscope's micro lever operates in an attractive or non-contact regime, and the interaction force between the tip and the sample is modeled according to the following model Mathematician, known as Van der Waals model:
    [0091] HR F VdW (d) ~ 6ddi (E.10) where H is Hamaker's constant.
    [0092] According to an embodiment of the present dynamic method for quantifying non-topographic properties in force microscopy, the force of viscoelastic interaction between the tip and the sample is modeled according to the following mathematical model:
    [0093] Fvis {t) = aSit) P ~ 1 [3r] Sit) (E.11) where r¡ is the viscosity coefficient of the sample; a is a coefficient that depends on the geometry and the Poisson coefficient and is a geometric factor that depends on the shape of the tip. For example for a semi-spherical tip a = 4/3 R1 / 2 and p = 3/2
    [0094] According to the dynamic method to quantify non-topographic properties object of the present invention, the tip-micro lever system can be placed on a sample heterogeneous to measure various mechanical properties such as the effective Young's modulus, Eeff of the sample, the viscosity coefficient and / or Hamaker's constant, H, of the interface.
    [0095]
    [0096] According to a form of the present dynamic method for quantifying non-topographic properties in force microscopy, object of the present invention, the measurement can be carried out by having the sample immersed in liquid.
    [0097]
    [0098] According to an embodiment of the present dynamic method for quantifying non-topographic properties in force microscopy, object of the present invention, the measurement can be performed by having the sample immersed in a gaseous medium.
    [0099]
    [0100] According to a form of the present dynamic method for quantifying non-topographic properties in force microscopy, object of the present invention, the measurement can be carried out by having the sample empty.
    [0101]
    [0102] The invention comprises a system that implements the dynamic force microscopy method of the present invention, in particular the system may comprise an atomic force microscope.
    [0103]
    [0104] BRIEF DESCRIPTION OF THE FIGURES
    [0105]
    [0106] The following figures show various embodiments of the present dynamic force microscopy method to simultaneously measure topography and force maps.
    [0107]
    [0108] Figure 1: Shows a diagram of the operation of dynamic force microscopy method of the invention under the existence of two feedback loops, one acting on the maximum force exerted on the sample and another acting on the amplitude of oscillation.
    [0109]
    [0110] Figure 2: Shows a scheme of the method object of the present invention with the observables and values necessary to determine the interaction force between the tip and the sample.
    [0111] Figure 3. Shows a scheme of the method object of the present invention that includes the most relevant steps of the method.
    [0112]
    [0113] Figure 4: Shows the results of a simulation of the method object of the present invention with the different signals as a function of time that allow determining the interaction force as a function of time for an elastic sample of 1 GPa of Young's modulus. The strength of the model is described by E.8 for a tip of radius R = 5 nm.
    [0114]
    [0115] Figure 5: Shows a comparative graph between the simulated force curve and that obtained by applying the method described in the present invention reconstruction performed by the method. The graph has been generated from the data in Figure 4.
    [0116]
    [0117] Figure 6: Shows the results of a simulation of the method object of the present invention with the different signals as a function of time that allow determining the interaction force as a function of time for an elastic sample of 1 kPa of Young's modulus. The strength of the model is described by E.8 for a tip of radius R = 500 nm.
    [0118]
    [0119] Figure 7: Shows a comparative graph of a numerical simulation where the force is compared as a function of the distance of the model and that obtained by applying the method described in the present invention reconstruction carried out by the method. The graph has been generated from the data in Figure 6.
    [0120]
    [0121] Figure 8: Shows the results of a simulation of the method object of the present invention with the different signals as a function of time that allow determining the interaction force as a function of time. The strength of the model is described by E.10 for a sample with H = 10-18 J. Radius R = 50 nm.
    [0122]
    [0123] Figure 9: Shows a comparative graph between where the force is compared according to the distance of the model and that obtained by applying the method described in the present invention (numerical simulation). The graph has been generated from the data in Figure 8.
    [0124]
    [0125] Figure 10: Shows the results of a simulation of the method object of the present invention with the different signals as a function of time that allow to determine the attractive interaction force as a function of time. The strength of the model is described by E.11 for a sample with Eef = 10 kPa, q = 100 Pa s. Radius R = 300 nm.
    [0126] Figure 11: Shows a comparative graph between where the force is compared as a function of the distance of the model and that obtained by applying the method described in this invention (numerical simulation). The graph has been generated from the data in Figure 10.
    权利要求:
    Claims (7)
    [1]
    1. Material characterization method based on force microscopy for image acquisition of the surface of a sample (4) together with the determination of the force curve at each point on the surface of the sample (4), where it is performed a displacement of a tip (3) of a micro lever (2) with respect to the sample (4) or vice versa while excitation of a micro lever is applied at a frequency lower than the resonant frequency,
    the method being characterized by comprising:
    - obtain an image of the surface of the sample (4) by applying a first feedback loop where a constant value of the maximum force exerted on the sample (4) is maintained, and
    - obtain an image of the surface of the sample (4) by applying a second feedback loop where a constant value of the oscillation amplitude of the micro lever (2) is maintained.
    [2]
    2. Method according to claim 1 characterized in that it comprises:
    a) place the micro lever (2) with the tip (3) at its free end on the head of a force microscope (1) so that it interacts with the sample (4), where the tip (3) has at least a vibration mode,
    b) arrange an excitation unit) (5) to vibrate the micro lever (2) and a displacement unit (6) to move the micro lever (2) over at least part of the sample (4);
    c) excite the micro lever (2) by the excitation unit (5) associated with the micro lever (2), making it vibrate;
    d) indicate: - the force constant, k;
    - the quality factor, Q;
    - the resonance frequency of the micro lever, f0, w0 = 2-n / 0;
    - the inverse of the optical sensitivity of the photodiode; Y
    - the radius, R, of the tip of the micro lever;
    e) detect the deflection signal of the micro lever (7);
    f) estimate the inertial contribution to the force by:

    [3]
    3. Method according to any one of claims 1 or 2, characterized in that it comprises transforming force curve data into parametric maps of sample properties (4) by adjusting the force curve to different interaction models.
    [4]
    Method according to any one of the preceding claims, characterized in that the micro lever (2) is excited by at least one of. mechanical excitation, electrical, magnetic excitation, thermal excitation and photothermal excitation.
    [5]
    Method according to any one of the preceding claims, characterized in that the characterization comprises measuring mechanical properties of the sample (4) selected from the group consisting of: Effective Young's modulus, Eeff, the viscosity q, and Hamaker's constant .
    [6]
    Method according to any of the preceding claims, characterized in that the sample (4) is: immersed in liquid or in vacuum.
    [7]
    7. Force microscope (1) characterized in that it is adapted to carry out the method described in any one of claims 1 to 6.
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    同族专利:
    公开号 | 公开日
    WO2019224414A1|2019-11-28|
    ES2732721B2|2021-08-05|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    EP2045818A1|2006-07-04|2009-04-08|Consejo Superior de Investigaciones Cientificas |Method for using an atomic force microscope|
    US20090139315A1|2007-11-30|2009-06-04|Chikuang Charles Wang|Non-destructive ambient dynamic mode afm amplitude versus distance curve acquisition|
    US20120131702A1|2008-11-13|2012-05-24|Bruker Nano, Inc.|Method and Apparatus of Using Peak Force Tapping Mode to Measure Physical Properties of a Sample|
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    PCT/ES2019/070342| WO2019224414A1|2018-05-23|2019-05-23|Dynamic force microscopy method and microscope for simultaneously obtaining topographical images and force maps|
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