(19)
(11)EP 2 045 818 B1

(12)EUROPEAN PATENT SPECIFICATION

(45)Mention of the grant of the patent:
08.05.2019 Bulletin 2019/19

(21)Application number: 06764394.0

(22)Date of filing:  04.07.2006
(51)Int. Cl.: 
G01Q 30/04  (2010.01)
G01Q 60/34  (2010.01)
(86)International application number:
PCT/ES2006/070096
(87)International publication number:
WO 2008/003796 (10.01.2008 Gazette  2008/02)

(54)

METHOD FOR USING AN ATOMIC FORCE MICROSCOPE

VERFAHREN ZUR VERWENDUNG EINES RASTERKRAFTMIKROSKOPS

PROCÉDÉ D'UTILISATION D'UN MICROSCOPE À FORCE ATOMIQUE


(84)Designated Contracting States:
AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC NL PL PT RO SE SI SK TR

(43)Date of publication of application:
08.04.2009 Bulletin 2009/15

(73)Proprietor: Consejo Superior de Investigaciones Científicas (CSIC)
28006 Madrid (ES)

(72)Inventors:
  • GARCIA GARCIA, Ricardo
    28760 Tres Cantos (Madrid) (ES)
  • RODRÍGUEZ LOZANO, José Luis
    28760 Tres Cantos (Madrid) (ES)
  • MARTÍNEZ CUADRADO, Nicolás F.
    28760 Tres Cantos (Madrid) (ES)
  • PATIL, Shivaprasad Vitthal
    28760 Tres Cantos (Madrid) (ES)

(74)Representative: Pons 
Glorieta Ruben Dario 4
28010 Madrid
28010 Madrid (ES)


(56)References cited: : 
EP-A1- 1 912 055
US-A1- 2004 134 265
US-A1- 2003 175 945
US-A1- 2005 034 512
  
  • TOMÁS R. RODRIGUEZ ET AL: "Compositional mapping of surfaces in atomic force microscopy by excitation of the second normal mode of the microcantilever", APPLIED PHYSICS LETTERS, vol. 84, no. 3, 1 January 2004 (2004-01-01), pages 449-451, XP55018876, ISSN: 0003-6951, DOI: 10.1063/1.1642273
  • HILLENBRAND R ET AL: "Higher-harmonics generation in tapping-mode atomic-force microscopy: Insights into the tip-sample interaction", APPLIED PHYSICS LETTERS, AIP, AMERICAN INSTITUTE OF PHYSICS, MELVILLE, NY, US, vol. 76, no. 23, 5 June 2000 (2000-06-05), pages 3478-3480, XP012025504, ISSN: 0003-6951, DOI: 10.1063/1.126683
  • MARTINEZ N ET AL: "Enhanced compositional sensitivity in atomic force microscopy by the excitation of the first two flexural modes", APPLIED PHYSICS LETTERS, AIP, AMERICAN INSTITUTE OF PHYSICS, MELVILLE, NY, US, vol. 89, no. 15, 11 October 2006 (2006-10-11), pages 153115-153115, XP012086336, ISSN: 0003-6951, DOI: 10.1063/1.2360894
  • LI ET AL.: 'Analytical solutions of the first three frequency shifts of AFM non-uniform probe subjected to the Lennard-Jones force' ULTRAMICROSCOPY vol. 106, 2006, pages 508 - 515, XP008102229
 
Remarks:
The file contains technical information submitted after the application was filed and not included in this specification
 
Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention).


Description


[0001] In general, this invention relates to a method of using an atomic force microscope (AFM) by means of amplitude modulation in order to analyse a sample at a nanometric scale, and, in particular, to a method of using said AFM by the simultaneous excitation of several normal vibration modes of the microlever thereof.

PRIOR STATE OF THE ART



[0002] In the past few years, atomic force microscopy (AFM), in its dynamic modes, has become one of the most powerful and versatile techniques for the nanometric-scale characterisation of the topography of a large variety of materials, such as biological molecules, polymers, semiconductors, ceramic materials or organic molecules. Due to their very high resolution (lateral and vertical) and robust operation, atomic force microscopes have been incorporated into both research laboratories and innovation and characterisation departments in technological sectors, such as the development of polymers or integrated circuits, to mention two examples. The potential of AFM microscopies in both basic research and technological applications would considerably expand if they could detect very small forces, in the pN range. Thus, the high spatial resolution could be accompanied by a great capacity to measure other surface physical or chemical properties, such as the chemical composition or the mechanical properties.

[0003] On the other hand, atomic force microscopy technology has led to a new type of micro- and nanomechanical sensors based on the changes in the dynamic properties (amplitude, phase or frequency) undergone by a microlever when chemical or biological molecules are adsorbed thereon (J. Fritz et al. Science 288, 316 (2000)).

[0004] The most widely spread AFM mode is known as amplitude modulation mode (AM-AFM; the most widespread commercial name is tapping mode AFM), which consists of the excitation of the microlever at the (fundamental) resonance frequency and the establishment of a feedback system based on the monitoring of the oscillation amplitude.

[0005] Since 1993, various schemes have been proposed to combine topography and compositional contrast using the dynamic modes of AFM. The most noteworthy has consisted of measuring the phase displacement between the oscillation signal and the excitation force. The measurement of the phase displacement is performed jointly and simultaneously with the measurement of the amplitude. In this case, the phase has been proposed in order to obtain information about compositional variations (D. Chernoff, Proc. Microscopy and Microanalysis, New York 1996; J. Tamayo and R. Garcia, Appl. Phys. Lett. 71, 2394 (1997); J.P. Cleveland et al. Appl. Phys. Lett. 72, 2613 (1998); G. Bar et al. Langmuir 14, 7343 (1998)). These measurements have made it possible to obtain images where the various components of polymer materials, semiconductors or organic compounds are visualised. However, various works have shown that the phase signal pertaining to the oscillation is governed by the inelastic energy dissipated between the tip and the sample. This suggests that different combinations of inelastic processes and elastic properties of the material may cause the same phase displacement; consequently, the phase displacement of the first harmonic does not provide quantitative information about the properties of the material (Tamayo, Garcia Applied Phys. Letters 73, 2926 (1998)). On the other hand, it has been shown that the phase signal also includes a topographic component, which makes separation between topographic and compositional information more difficult (M. Stark et al. Biophys. J. 80, 3009 (2001)).

[0006] Recently, other methods have been proposed to combine topographic information and chemical information, such as patent (P. Hinterdorfer, J. Nelson, US2004/0129064 A1); however, this type of schemes are only applicable to measure specific interactions between biological molecules, which considerably restricts the scope of application of the method.

[0007] Several factors may contribute to explain the current limitations of atomic force microscopy to obtain information beyond topography. Amongst them, it is worth mentioning the consideration of the AFM microlever as a single-mode mechanical system, i.e. the microlever is considered to be a mechanical system characterised by a single resonance frequency (the fundamental one). Consequently, the excitation is performed at frequencies close to the resonance frequency. However, a microlever has several vibration modes, all of them at frequencies higher than the fundamental frequency. For example, for a lever in the shape of a rectangular prism, with a uniform density, the ratio between frequencies is v0, 6.39v0, 17.9v0,. In atomic force microscopy, the contributions of the modes higher than the oscillation amplitude are quite small, but they are, however, noticeable under experimental conditions (R. Hillenbrand et al. Appl. Phys. Lett. 76, 3478 (2000); Stark T.R. Rodriguez, R. Garcia, Appl. Phys. Lett. 80, 1646 (2002)).

[0008] In order to increase the higher mode components, the simultaneous excitation of several oscillation modes of the microlever has been proposed (T.R. Rodriguez, R. García, WO2007/036591 A1 and Appl. Phys. Lett. 449, 84 (2004)).

[0009] The final result entails having a microscope that has 2n independent interaction channels with the material (two for each vibration mode), each of which could analyse a different property.

[0010] Document WO2007/036591 A1 proposes a method of using an atomic force microscope by means of amplitude modulation, which comprises exciting two natural vibration modes of the microlever, and analysing the variation of the oscillation amplitude of the microlever's response to the excitation in the lower mode, in order to obtain topographic information about the sample, and analysing the phase variation, or phase displacement, of the microlever's (M) response to the excitation in the higher mode, in order to obtain compositional information about the sample.

[0011] In this application, said variations are analysed with respect to the total oscillation amplitude of the microlever, both that of the amplitude of the lower mode (as was conventionally done) and that of the phase, or phase displacement, of the higher mode, and it is shown that, for changes in the properties of the sample material, the phase variation, or phase displacement, in the higher mode is significant, contrary to what occurs with the lower mode, which justifies said proposal, in the sense of using the variation of amplitude of the lower mode, or first mode, with respect to the variation of said total amplitude to obtain topographic information about the sample and the variation of the phase of the higher mode, with respect to the total amplitude, to obtain information about the compositional contrast of the sample, or of different samples.

[0012] Although said proposal represented a great advance in the field of atomic force microscopy, by assuming the microlever's multi-mode character, and was able to significantly increase the sensitivity of such microscopes to compositional contrast, said proposal still carries one of the limitations of conventional methods; namely, performing the analyses of the variations of the variables with respect to the total oscillation amplitude of the microlever's response, both in regards to the conventional use of the amplitude of the lower mode as the variable to be analysed, and the proposed use, in said document WO2007/036591 A1, of the phase of the higher mode as the variable to be analysed.

EXPLANATION OF THE INVENTION



[0013] These inventors have observed that, starting from the advantages obtained upon assuming the microlever's multi-mode character, as done in document WO2007/036591 A1, but eliminating the limitations described above, it is possible to increase the sensitivity of an atomic force microscope even further, as well as not limit the use of the amplitude of the lower mode to obtain topographic information, nor that of the phase of the higher mode for the compositional information.

[0014] To do so, this invention relates to a method of using an atomic force microscope by means of amplitude modulation, of the type that comprises exciting, normally in a simultaneous manner, at least one natural lower vibration mode and one natural higher vibration mode of a microlever of said microscope, placed on a sample to be examined.

[0015] The proposed method comprises:
  • analysing at least the variation of the resonance frequency of a first output signal that is representative of the response of said microlever to said excitation of said lower mode, with respect to the variation of at least one parameter which is influenced by the resonance frequency of a second output signal that is representative of the response of said microlever to said excitation of said higher mode.


[0016] For a preferred embodiment example, said lower mode is the microlever's first natural vibration mode and said higher mode is the microlever's second natural vibration mode.

[0017] Although, preferably, said parameter or parameters are equivalent to the variable whereby they are influenced, in another embodiment example, at least one of said parameters is influenced, in a weighted manner, by at least two variables of, respectively, a first and a second output signal that are representative of the response of said microlever to, respectively, said excitation of said lower mode and said higher mode.

[0018] For another embodiment example, the method comprises exciting one or more higher modes of the microlever, and taking into account, for said analysis or analyses, one or more variables of an output signal obtained by said excitation of said other higher mode.

[0019] The proposed method comprises performing the analyses described to obtain topographic and/or compositional information about said sample, without limiting the use of the variation of the amplitude of the lower mode to obtain topographic information, nor that of the phase of the higher mode to obtain compositional information, as proposed in document WO2007/036591 A1, but any of the variables described above for the different embodiment examples, i.e. the amplitude, the phase or the frequency of any of the modes, with respect to an equivalent parameter or one that is influenced at least in part by the amplitude, the phase or the frequency of another mode, in any order.

[0020] The proposed method also comprises changing said sample to be examined by, at least, a second sample and performing, with said second sample, the same steps that were performed with the sample.

[0021] In order to facilitate the interpretation and presentation of the results of the analyses described, the method comprises performing a cross-representation of the data obtained as a result of said analysis or analyses, for two or more variables of, respectively, two or more output signals that are representative of the response of said microlever to corresponding excitations of said natural vibration modes.

[0022] For an embodiment example, said representations are visual representations, in the form of a graph or a table, some of which are represented in the attached figures, which will be described in a section below.

[0023] The method also comprises recording and classifying the data obtained for a plurality of different samples, as well as comparing the data obtained for an analysis of the sample located under said microlever to said recorded data, and, on the basis of the result of said comparison, establishing a degree of similarity with at least one sample of said plurality of samples.

BRIEF DESCRIPTION OF THE DRAWINGS



[0024] The preceding and other advantages and characteristics will be more fully understood from the following detailed description of some examples that refer to the attached drawings, which are presented for illustrative, non-limiting purposes, and wherein:

Figure 1 shows a block-level description of an atomic force microscope as that proposed by document WO2007/036591 A1, but with a number of added blocks, framed within dotted lines, which are used to perform the method proposed.

Figure 2 is a graph that shows, for two different materials, the variation of the phase displacement of the second oscillation mode of the microlever when it is excited in the first two modes (with free oscillation amplitudes of 10 and 1 nm, respectively), with respect to the amplitude of the first mode.

Figure 3 is a graph that shows, for two different materials, the variation of the phase displacement of the first oscillation mode of the microlever when it is excited in the first two modes (with free oscillation amplitudes of 10 and 1 nm, respectively), with respect to the amplitude of the second mode.

Figure 4 is a graph that shows, for two different materials, the variation of the phase displacement of the first oscillation mode of the microlever when it is excited in the first two modes (with free oscillation amplitudes of 10 and 1 nm, respectively), with respect to the amplitude of the first mode.

Figure 5 is a graph that shows, for two different materials, the variation of the phase displacement of the second oscillation mode of the microlever when it is excited in the first two modes (with free oscillation amplitudes of 10 and 1 nm, respectively), with respect to the amplitude of the second mode; and

Figure 6 is a graph that shows, for two different materials, the variation of the phase displacement of the second oscillation mode of the microlever when it is excited in the first two modes (with free oscillation amplitudes of 10 and 1 nm, respectively), with respect to a parameter that is representative of a weighted sum of amplitudes of both modes.


DETAILED DESCRIPTION OF SOME EMBODIMENT EXAMPLES



[0025] A number of experimental simulations and trials have been performed in order to demonstrate the value of the proposed method, which, amongst others, have offered a number of data that are represented by the graphs illustrated by figures 2 to 6.

[0026] Below we explain a number of concepts and mathematical expressions wherein the above-mentioned simulations have been based, which explain the behaviour of the microscope illustrated by Fig. 1, used in accordance with the proposed method.

[0027] As mentioned above, this invention assumes the multi-mode character of microlever M (see Fig. 1), the simultaneous excitation of several modes of microlever M by mechanical, electrostatic or thermal means, or any combination thereof. This invention specifies that what is relevant to obtain an increase in the sensitivity of the micromechanical device (atomic force microscope or mechanical sensor) to physical interactions in the use of analyses and representations that cross parameters from one mode (amplitude, phase or resonance frequency) with parameters from another mode (cross-representations).

[0028] The feasibility of the method is based on the numerical analysis of the dynamic behaviour of an atomic force microscope, a task that has been performed at the Forces and Tunnel laboratory of the Higher Council for Scientific Research (CSIC).

[0029] In the first place, microlever M is considered to be a continuous system, w(x,t), that is externally excited and interacts with the sample through a long-range interaction (van der Waals force) and a short-range interaction described by the Derjaguin-Muller-Toporov model. Under these conditions, the equation of movement is:

where E is Young's module, l is the moment of inertia formed by microlever M, and L is the length. Fexc , Fmed and Fts are, respectively, the excitation force, the friction force with the medium and the interaction force per unit of length.

[0030] On the other hand, the deflection of microlever M is expressed as:



where,

The total amplitude (rms value) would be calculated as



[0031] The different channels arise naturally when microlever M of an AFM is considered to be a mechanical system that contains many autovibration modes. The excitation of the first mode and the non-linear character of the interaction generate the excitation of higher harmonics of the first mode; however, it has been shown that the amplitude of these components under relevant experimental conditions is approximately four orders of magnitude smaller than the fundamental one, which makes the experimental use thereof very difficult (T.R. Rodriguez, R. Garcia, Appl. Phys. Lett. 80, 1646 (2002)). In order to increase the higher mode components, the simultaneous excitation of several oscillation modes of microlever M has been proposed, which may be two, three, four, etc. (R. Garcia and T.R. Rodríguez, WO2007/036591 A1). The purpose is to establish a relationship between the amplitudes of the lowest frequency mode and the higher mode of approximately 1%-10%. The excitation could also be multi-mode by means of an expression of the type,

where Fi and ωi represent the excitation force and the mode frequency of microlever M. As a consequence of this previous excitation, 2n communication channels with the sample will be generated. For each mode, two channels are provided, one for amplitude A and the other for phases φ. For reasons of brevity and in order to show the concept of multi-mode operation, we will present the two-mode case of the atomic force microscope, i.e. when two vibration modes are simultaneously excited, which may be the first and the second, the first and the third, and so on, or the second and the third, etc., and all the possible combinations between them. The two-mode excitation is as follows:

where ωi and ωj are the frequencies of two normal modes of microlever M that fulfil the condition j>i. Thus, the amplitude of the higher modes will no longer be simply controlled by the excitation caused by the harmonics of the fundamental mode, as is the case with a (dynamic) atomic force microscope, but as a result of a force that may be controlled by the observer.

[0032] The microscope illustrated by Fig. 1 is like that proposed in patent document WO2007/036591 A1, with the corresponding two-mode excitation module, formed by the AFM control unit and the two-mode control unit, already described in said application, as well as a number of added blocks, framed within dotted lines, which are used to perform the method proposed.

[0033] One of said blocks is adapted to perform the analyses described above, at least in part, as well as the cross-representations also described above.

[0034] The other module indicated with dotted lines in Fig. 1 is that pertaining to the feedback of scanner z, i.e. the sample support, which generally consists of a piezoelectric tube controlled by a feedback mechanism designed to adjust the distance between the tip of microlever M and the sample, in order to maintain a constant force between them.

[0035] Said feedback mechanism conventionally only takes into consideration the amplitude of the first mode, i.e. Ai, but the method proposed comprises performing said feedback on the basis not only of the amplitude of the first mode, Ai, but also of the total amplitude, Atot.

[0036] Said Fig. 1 represents the excitation signal of the lower mode as Ficosωit, and that of the higher mode as Fjcosωjt, with j>i.

[0037] For a preferred embodiment example, the proposed method comprises performing both excitations by means of a single excitation signal Ficosωit + Fjcosωjt, composed of the sum of said two excitation signals Ficosωit and Fjcosωjt, and, as indicated by an arrow in Figure 1, applied to microlever M.

[0038] For an embodiment example, the method comprises performing the excitation of the two modes externally, and, for another embodiment example, the method comprises performing the excitation of one of said modes externally, and the excitation of the other mode or modes by self-excitation by harmonics or sub-harmonics of the external excitation.

[0039] Said external excitation may be any of the following excitations: mechanical, thermal, electrostatic or a combination thereof.

[0040] The method also comprises, as shown in Fig. 1, breaking down an output signal Aicos(ωit-φi) + Ajcos(ωjt-φj), which is representative of the response of said microlever M to said excitation by said compound excitation signal Ficosωit + Fjcosωjt, separating the parts of the signal that correspond to the response to each of said two excitations, and subsequently using the variables thereof to perform the above-mentioned analyses.

[0041] Specifically, the method comprises breaking down (as was done in the proposal of document WO2007/036591 A1) the information contained in said output signal Aicos(ωit-φi) + Ajcos(ωjt-φj) into four channels: two channels with information about oscillation amplitude Ai, Aj of said output signal Aicos(ωit-φi) + Ajcos(ωjt-φj) for said two excitation frequencies, and two channels with information about phase φi, φj of said output signal Aicos(ωit-φi) + Ajcos(ωjt-φj) for said two excitation frequencies.

[0042] Said four channels are used to perform the analyses and cross-representations in accordance with the method proposed, some of which are illustrated by Figs. 2 to 6, for some of the possible examples presented in a previous section.

[0043] The numerical simulations presented below illustrate the advantages offered by the analysis and the cross-representation of variables pertaining to different modes, in the particular case of a two-mode excitation that acts on the first and second modes of an AFM.

[0044] Figure 2 shows how the dependency of the phase of the second mode φ2 with respect to the amplitude of the first mode A1 makes it possible to distinguish between two different interaction forces; that is, two different materials (it may be observed that, for A1=5 nm, there is a variation of Δφ2=3 degrees, which the model allows to convert into an increase in interaction forces that in this case is equal to ΔF=3.41 pN), the Hamacker constants whereof are H=4.7x10-20 J and H=9x10-20 J, respectively. This analysis, the result whereof has been graphically represented in said Fig. 2, makes it possible to detect the differences between the materials.

[0045] Figure 3 shows how the dependency of the phase of the first mode φ1 with respect to the oscillation amplitude of the second mode A2 makes it possible to distinguish between two different interaction forces; that is, two different materials (it may be observed that, for A2=0.8 nm, there is a variation of Δφ1=10 degrees, which the model allows to convert into an increase in interaction forces that in this case is equal to ΔF=21.70 pN), which are represented in Fig. 2. This analysis, the result whereof has been graphically represented in said Fig. 3, also makes it possible to detect the differences between the materials.

[0046] Figure 4 shows that the phase of the first mode φ1 is not sensitive to the change in material properties (only elastic interactions are considered) when it is represented with respect to its own amplitude A1. This representation does not make it possible to detect the differences between the materials.

[0047] Figure 5 shows that the phase of the second mode φ2 is not sensitive to the change in material properties (only elastic interactions are considered in the model) when it is represented with respect to its own amplitude A2. This representation does not make it possible to detect the differences between the materials.

[0048] The results shown in Figures 4 and 5 are in contrast with those obtained in Figures 2 and 3.

[0049] The results shown in Figures 2-5 have been obtained with the following parameters L, b, h, E, R and ρ for 255 nm, 40 nm, 1.8 nm, 170 GPa, 20 nm and 2,320 kg/m2; k1=0.9 N/m, k2=35.22 N/m; Q1=255; Q2=1,002; F1=60 pN and F2=20 pN. The two materials used were simulated using Hamacker constants Ha=4.7x10-20 J and Hb=9x10-20 J.

[0050] The preceding figures have allowed to establish that the most genuine way to obtain compositional contrast by attractive elastic interactions is the analysis and cross-representation of variables of both modes. If the phase of one mode is represented with respect to its own amplitude, no contrast is obtained (in the absence of elastic interactions).

[0051] In the examples illustrated by Figures 2 and 3, the abcissa axis represents a pure variable of one mode, specifically, the amplitude (A1 in Fig. 2 and A2 in Fig. 3). These cases are representative of the examples described for which the parameter, or the parameters, with respect to which the variation analysis of a variable is performed (φ2 in Fig. 2 and φ1 in Fig. 3) are equivalent to a single variable, in this case A1 in Fig. 2 and A2 in Fig. 3.

[0052] Other embodiment examples are proposed, also already described, for which said parameters are influenced, in a weighted manner, by two variables of, respectively, a first Aicos(ωit-φj) and a second Ajcos(ωjt-φj) output signals that are representative of the response of microlever M to, respectively, the excitation of the lower mode and of the higher mode.

[0053] Fig. 6 is representative of examples for which said parameters are a weighted sum of amplitudes of both modes. The differences between the graphs of both materials (the same as in Figures 2 to 5), it is also possible to maintain the sensitivity to the change in interaction forces if the variable of one mode (amplitude or phase) is represented with respect to said parameter that is representative of a weighted sum of amplitudes of both modes, which, for said embodiment example illustrated in Fig. 6, are the total amplitude (rms value), but which for other embodiment examples could be any other type of weighted sum.

[0054] The proposed method is equally applicable for those cases wherein microlever M is used as a sensor to determine the adsorption of chemical or biological molecules.

[0055] For an embodiment example of the proposed method, either the amplitude of the lower mode Ai or the total amplitude is used to form an image of the system's topography, whereas the cross signals pertaining to different modes Aj and φj are used to complete the topographic characterisation or to provide information about the material's physical and/or chemical properties, in the form Aj vs. φj, or φj vs. φi, φi vs. Aj, with i≠j. The case φi vs. Atot, where φi is the phase of a mode other than the fundamental one, could also be considered.

[0056] A person skilled in the art could introduce changes and modifications in the embodiment examples described without going beyond the scope of the invention, as defined in the attached claims.


Claims

1. Method of using an atomic force microscope by means of amplitude modulation, of the type that comprises exciting at least one natural lower vibration mode and one natural higher vibration mode of a microlever (M) of said microscope, placed on a sample to be examined, the method comprising:

- analysing at least the variation of the resonance frequency of a first output signal (Ai cos(ωi t-ϕi)) that is representative of the response of said microlever (M) to said excitation of said lower mode, with respect to the variation of at least one parameter which is influenced by the resonance frequency of a second output signal (Aj cos(ωj t-ϕj)) that is representative of the response of said microlever (M) to said excitation of said higher mode.


 
2. Method, as claimed in claim 1, characterised in that at least one of said parameters is equivalent to said variable whereby it is influenced.
 
3. Method, as claimed in claim 1, characterised in that at least one of said parameters is influenced, in a weighted manner, by at least two variables of, respectively, a first (Ai cos(ωi t-ϕi)) and a second (Aj cos(ωj t-ϕj)) output signals that are representative of the response of said microlever (M) to, respectively, said excitation of said lower mode and of said higher mode.
 
4. Method, as claimed in any of the preceding claims, characterised in that said lower mode is the first natural vibration mode of the microlever (M).
 
5. Method, as claimed in any of the preceding claims, characterised in that said higher mode is the second natural vibration mode of the microlever (M).
 
6. Method, as claimed in any of the preceding claims, characterised in that it comprises exciting at least another higher mode of the microlever (M), and taking into consideration, for said analysis or analyses, at least one variable of an output signal obtained by said excitation of said other higher mode.
 
7. Method, as claimed in claim 1, characterised in that it comprises performing said excitation of at least said two modes externally.
 
8. Method, as claimed in claim 1, characterised in that it comprises performing the excitation of one of said modes externally, and the excitation of the other mode or modes by self-excitation by harmonics or sub-harmonics of the external excitation.
 
9. Method, as claimed in claims 7 or 8, characterised in that said external excitation is at least one excitation from the group that includes the following excitations: mechanical, thermal, electrostatic, or a combination thereof.
 
10. Method, as claimed in any of the preceding claims, characterised in that it comprises performing said analysis or analyses to obtain topographic and/or compositional information about said sample.
 
11. Method, as claimed in claim 10, characterised in that it comprises changing said sample to be examined by at least one second sample and performing, with said second sample, the same steps that were performed with the first sample.
 
12. Method, as claimed in any of the preceding claims, characterised in that it comprises performing at least one cross-representation of the data obtained as a result of said analysis or analyses, for two or more variables of, respectively, two or more output signals that are representative of the response of said microlever (M) to the corresponding excitations of said natural vibration modes.
 
13. Method, as claimed in claim 12, characterised in that said representation is a visual representation, in the form of a graph or a table.
 
14. Method, as claimed in claims 11, 12 or 13, when they are dependent on claim 11, characterised in that it comprises recording and classifying the data obtained for a plurality of different samples.
 
15. Method, as claimed in claim 14, characterised in that it comprises comparing the data obtained for an analysis of the sample located under said microlevel (M) to said recorded data, and, on the basis of the result of said comparison, establishing a degree of similarity with at least one sample of said plurality of samples.
 
16. Method, as claimed in any of the preceding claims, characterised in that it comprises performing at least two of said excitations of said natural vibration modes of the microlever (M) simultaneously.
 
17. Method, as claimed in claim 16, characterised in that it comprises performing said excitations, which are at least two, of said natural vibration modes of the microlever (M) by means of a single excitation signal (Fi coswi t + Fj coswj t) composed of the sum of said two excitation signals (Fi coswi t, Fj cosωj t).
 
18. Method, as claimed in claim 13, characterised in that it comprises breaking down an output signal (Ai cos(ωi t-ϕi) + Aj cos(ωj t-ϕj)) that is representative of the response of said microlever (M) to said excitation by means of said compound excitation signal (Fi coswi t + Fj coswj t), separating the parts of the signal that correspond to the response to each of said excitations, which are at least two, and subsequently using the variables thereof to perform at least the above-mentioned analyses.
 


Ansprüche

1. Verfahren zur Verwendung eines Rasterkraftmikroskops mittels Amplitudenmodulation des Typs, das die Anregung mindestens einer niedrigeren Eigenschwingungsmode und einer höheren Eigenschwingungsmode eines Microlevers (M) des Mikroskops umfasst, der auf einer zu untersuchenden Probe angeordnet wird, wobei das Verfahren Folgendes umfasst:

- Analysieren mindestens der Variation der Resonanzfrequenz eines ersten Ausgangssignals (Ai cos(ωi t-ϕi)), das für die Reaktion des Microlevers (M) auf die Anregung der niedrigeren Mode repräsentativ ist, in Bezug auf die Änderung mindestens eines Parameters, der durch die Resonanzfrequenz eines zweiten Ausgangssignals (Aj cos (ωj t-ϕj)) beeinflusst wird, das für die Reaktion des Microlevers (M) auf die Anregung der höheren Mode repräsentativ ist.


 
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass mindestens einer der Parameter äquivalent zu der Variablen ist, durch die er beeinflusst wird.
 
3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass mindestens einer der Parameter in einer gewichteten Weise durch mindestens zwei Variablen von jeweils einem ersten (Ai cos(ωi t-ϕi)) und einem zweiten (Aj cos(ωj t-ϕj)) Ausgangssignal, die für die Reaktion des Microlevers (M) auf jeweils die Anregung der niedrigeren Mode und der höheren Mode repräsentativ sind, beeinflusst wird.
 
4. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die niedrigere Mode die erste Eigenschwingungsmode des Microlevers (M) ist.
 
5. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die höhere Mode die zweite Eigenschwingungsmode des Mikrolevers (M) ist.
 
6. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass es das Anregen mindestens einer weiteren höheren Mode des Microlevers (M) und das Berücksichtigen mindestens einer Variablen eines Ausgangssignals, das durch die Anregung der weiteren höheren Mode erhalten wird, für die Analyse oder Analysen umfasst.
 
7. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass es das Durchführen der externen Anregung von mindestens der zwei Moden umfasst.
 
8. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass es das Durchführen der externen Anregung einer der Moden und die Anregung der anderen Mode oder Moden durch Selbstanregung durch Oberschwingung oder Unterschwingung der externen Anregung umfasst.
 
9. Verfahren nach Anspruch 7 oder 8, dadurch gekennzeichnet, dass die externe Anregung mindestens eine Anregung aus der Gruppe ist, welche die folgenden Anregungen umfasst: mechanische, thermische, elektrostatische oder eine Kombination davon.
 
10. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass es das Durchführen der Analyse oder Analysen umfasst, um topographische und/oder Zusammensetzungsinformationen über die Probe zu erhalten.
 
11. Verfahren nach Anspruch 10, dadurch gekennzeichnet, dass es das Auswechseln der zu untersuchenden Probe durch mindestens eine zweite Probe und das Durchführen der gleichen Schritte, die mit der ersten Probe durchgeführt wurden, mit der zweiten Probe umfasst.
 
12. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass es das Durchführen mindestens einer Vergleichsdarstellung der Daten, die als Ergebnis der Analyse oder Analysen erhalten wurden, für zwei oder mehr Variablen von jeweils zwei oder mehr Ausgangssignalen umfasst, die für die Reaktion des Microlevers (M) auf die entsprechenden Anregungen der Eigenschwingungsmoden repräsentativ sind.
 
13. Verfahren nach Anspruch 12, dadurch gekennzeichnet, dass die Darstellung eine visuelle Darstellung in Form eines Diagramms oder einer Tabelle ist.
 
14. Verfahren nach Anspruch 11, 12 oder 13, wenn sie von Anspruch 11 abhängig sind, dadurch gekennzeichnet, dass es das Aufzeichnen und Klassifizieren der Daten, die für mehrere unterschiedliche Proben erhalten wurden, umfasst.
 
15. Verfahren nach Anspruch 14, dadurch gekennzeichnet, dass es das Vergleichen der Daten, die für eine Analyse der unter dem Microlevel (M) angeordneten Probe erhaltenen wurden, mit den aufgezeichneten Daten und auf der Grundlage des Ergebnisses des Vergleichs das Bestimmen eines Ähnlichkeitsgrades mit mindestens einer Probe der mehreren Proben umfasst.
 
16. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass es das Durchführen von mindestens zwei der gleichzeitigen Anregungen der Eigenschwingungsmoden des Mikrolevers (M) umfasst.
 
17. Verfahren nach Anspruch 16, dadurch gekennzeichnet, dass es das Durchführen der Anregungen, die mindestens zwei sind, der Eigenschwingungsmoden des Mikrolevers (M) mittels eines einzelnen Anregungssignals (Fi cosωi t + Fj cosωj t) umfasst, das aus der Summe der zwei Anregungssignale (Fi cosωi t, Fj cosωj t) gebildet ist.
 
18. Verfahren nach Anspruch 13, dadurch gekennzeichnet, dass es das Zerlegen eines Ausgangssignals (Ai cos(ωi t-ϕi) + Aj cos(ωj t-ϕj)) umfasst, das für die Reaktion des Mikrolevers (M) auf die Anregung repräsentativ ist, mittels des zusammengesetzten Anregungssignals (Fi cosωi t + Fj cosωj t), wobei die Teile des Signals abgetrennt werden, die der Reaktion auf jede der Anregungen entsprechen, die mindestens zwei sind, und anschließend die Variablen davon verwendet werden, um mindestens die oben erwähnten Analysen durchzuführen.
 


Revendications

1. Procédé d'utilisation d'un microscope à force atomique au moyen d'une modulation d'amplitude, du type qui comprend l'excitation d'au moins un mode naturel de vibration inférieur et d'un mode naturel de vibration supérieur d'un microlevier (M) dudit microscope, placé sur un échantillon à examiner, le procédé
comprenant :

- l'analyse d'au moins la variation de la fréquence de résonance d'un premier signal de sortie (Ai cos(ωi t-ϕi)) qui est représentatif de la réponse dudit microlevier (M) à ladite excitation dudit mode inférieur, par rapport à la variation d'au moins un paramètre qui est influencé par la fréquence de résonance d'un deuxième signal de sortie (Aj cos(ωj t-ϕj)) qui est représentatif de la réponse dudit microlevier (M) à ladite excitation dudit mode supérieur.


 
2. Procédé, tel que revendiqué dans la revendication 1, caractérisé en ce qu'au moins l'un desdits paramètres est équivalent à ladite variable selon laquelle il est influencé.
 
3. Procédé, tel que revendiqué dans la revendication 1, caractérisé en ce qu'au moins l'un desdits paramètres est influencé, de façon pondérée, par au moins deux variables, respectivement, d'un premier (Ai cos(ωi t-ϕi)) et d'un deuxième (Aj cos(ωj t-ϕj)) signaux de sortie qui sont représentatifs de la réponse dudit microlevier (M) à, respectivement, ladite excitation dudit mode inférieur et dudit mode supérieur.
 
4. Procédé, tel que revendiqué dans l'une quelconque des revendications précédentes, caractérisé en ce que ledit mode inférieur est le premier mode naturel de vibration du microlevier (M).
 
5. Procédé, tel que revendiqué dans l'une quelconque des revendications précédentes, caractérisé en ce que ledit mode supérieur est le deuxième mode naturel de vibration du microlevier (M).
 
6. Procédé, tel que revendiqué dans l'une quelconque des revendications précédentes, caractérisé en ce qu'il comprend l'excitation d'au moins un autre mode supérieur du microlevier (M), et la prise en considération, pour ladite analyse ou lesdites analyses, d'au moins une variable d'un signal de sortie obtenue par ladite excitation dudit autre mode supérieur.
 
7. Procédé, tel que revendiqué dans la revendication 1, caractérisé en ce qu'il comprend la réalisation de ladite excitation d'au moins lesdits deux modes extérieurement.
 
8. Procédé, tel que revendiqué dans la revendication 1, caractérisé en ce qu'il comprend la réalisation de l'excitation de l'un desdits modes extérieurement, et l'excitation de l'autre mode ou modes par excitation propre par des harmoniques ou sous-harmoniques de l'excitation externe.
 
9. Procédé tel que revendiqué dans les revendications 7 ou 8, caractérisé en ce que ladite excitation externe est au moins une excitation du groupe qui comporte les excitations suivantes : mécanique, thermique, électrostatique, ou une combinaison de ces dernières.
 
10. Procédé, tel que revendiqué dans l'une quelconque des revendications précédentes, caractérisé en ce qu'il comprend la réalisation de ladite analyse ou desdites analyses pour obtenir des informations topographiques et/ou compositionnelles sur ledit échantillon.
 
11. Procédé, tel que revendiqué dans la revendication 10, caractérisé en ce qu'il comprend le changement dudit échantillon à examiner par au moins un deuxième échantillon et la réalisation, avec ledit deuxième échantillon, des mêmes étapes qui ont été réalisées avec le premier échantillon.
 
12. Procédé, tel que revendiqué dans l'une quelconque des revendications précédentes, caractérisé en ce qu'il comprend la réalisation d'au moins une représentation croisée des données obtenues à partir de ladite analyse ou desdites analyses, pour deux ou plusieurs variables, respectivement, de deux ou plusieurs signaux de sortie qui sont représentatifs de la réponse dudit microlevier (M) aux excitations correspondantes desdits modes naturels de vibration.
 
13. Procédé, tel que revendiqué dans la revendication 12, caractérisé en ce que ladite représentation est une représentation visuelle, sous la forme d'un graphique ou d'une table.
 
14. Procédé, tel que revendiqué dans les revendications 11, 12 ou 13, lorsqu'elles sont dépendantes de la revendication 11, caractérisé en ce qu'il comprend l'enregistrement et la classification des données obtenues pour une pluralité de différents échantillons.
 
15. Procédé, tel que revendiqué dans la revendication 14, caractérisé en ce qu'il comprend la comparaison des données obtenues pour une analyse de l'échantillon situé sous ledit microniveau (M) avec lesdites données enregistrées, et, en fonction du résultat de ladite comparaison, l'établissement d'un degré de similarité avec au moins un échantillon de ladite pluralité d'échantillons.
 
16. Procédé, tel que revendiqué dans l'une quelconque des revendications précédentes, caractérisé en ce qu'il comprend la réalisation d'au moins deux desdites excitations desdits modes naturels de vibration du microlevier (M) simultanément.
 
17. Procédé, tel que revendiqué dans la revendication 16, caractérisé en ce qu'il comprend la réalisation desdites excitations, qui sont au moins deux, desdits modes naturels de vibration du microlevier (M) au moyen d'un seul signal d'excitation (Fi cosωi t + Fj cosωj t) composé de la somme desdits deux signaux d'excitation (Fi cosωi t, Fj cosωj t).
 
18. Procédé, tel que revendiqué dans la revendication 13, caractérisé en ce qu'il comprend la décomposition d'un signal de sortie (Ai cos(ωi t-ϕi) + Aj cos(ωj t-ϕj)) qui est représentatif de la réponse dudit microlevier (M) à ladite excitation au moyen dudit signal d'excitation de composé (Fi cosωi t + Fj cosωj t), la séparation des parties du signal qui correspond à la réponse à chacune desdites excitations, qui sont au moins deux, et ultérieurement l'utilisation de leurs variables pour réaliser au moins les analyses susmentionnées.
 




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REFERENCES CITED IN THE DESCRIPTION



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Patent documents cited in the description




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