Method and device of using a scanning probe microscope
11112426 · 2021-09-07
Assignee
Inventors
- Georg Ernest Fantner (Chavannes-près-Renens, CH)
- Jonathan David Adams (Lausanne, CH)
- Adrian Pascal Nievergelt (Préverenges, CH)
Cpc classification
G01Q10/065
PHYSICS
International classification
Abstract
A scanning probe microscope for high-speed imaging and/or nanomechanical mapping including a scanning probe comprising a cantilever with a tip at the distal end, and means for modulating a tip-sample distance separating the tip from an intended sample to be viewed with the microscope, the means for modulating being adapted to provide a direct cantilever actuation.
Claims
1. A method for characterising a surface of a sample using atomic force microscopy with a cantilever acting as both actuator and sensor, the method comprising the steps of: generating an oscillating motion between a tip of the cantilever of the atomic force microscope and the surface of the sample by deforming at least a part of the cantilever to bring the tip of the cantilever in contact with the surface of the sample for a tip-sample interaction; recording a deflection of the cantilever resulting from the tip-sample interaction as a first signal; extracting the tip-sample interaction as a second signal from the first signal by removing a background signal; determining a peak force from the extracted second signal; comparing the peak force to a predetermined setpoint force to determine an error signal; generating a control signal from the error signal; and actuating a z-actuator using the control signal to maintain the peak force at the predetermined setpoint force, wherein the cantilever includes an actuation coating and a detection coating, each of the coatings made of a different material, and each of the coatings is arranged at a different location on the cantilever.
2. The method of claim 1, wherein the background signal includes a signal of the deflection resulting from the tip-sample interaction caused by the cantilever deformation to generate tip-sample distance modulation.
3. The method of claim 1, wherein the step of recording the cantilever signal includes a step of reading a light beam.
4. The method of claim 3, wherein the step of generating the oscillating motion caused by the deformation of at least a part of the cantilever uses a photothermal device as a modulation, and both a device generating the light beam and the photothermal device include a single laser.
5. The method of claim 1, wherein the step of generating the oscillating motion caused by the deformation of at least a part of the cantilever is performed by a modulation device configured to provide a deformation of an entirety of the cantilever.
6. The method of claim 1, wherein the step of generating the oscillating motion caused by the deformation of at least a part of the cantilever is performed by a modulation device configured to provide a partial deformation of the cantilever.
7. The method of claim 1, wherein the step of generating the oscillating motion caused by the deformation of at least a part of the cantilever is configured to achieve a predefined motion.
8. The method of claim 7, wherein the predefined motion compensates for the background signal.
9. The method of claim 1, further comprising the step of: thermally bending the cantilever to provide a feedback motion.
10. The method of claim 9, wherein the step of thermally bending is configured to enable the feedback motion using a combination of a piezo scanner and the bending of the cantilever.
11. An atomic force microscope configured to perform the method of claim 1.
12. The method of claim 1, wherein the detection coating is arranged at a free end of the cantilever, and the actuation coating is arranged at a base of the cantilever.
13. The method of claim 1, wherein the detection coating is arranged to cover an entire side of the cantilever.
14. The method of claim 1, wherein the step of recording is performed by strain sensing of the cantilever, and the detection coating includes a piezoresistive, electrothermal, or piezoelectric device.
Description
BRIEF DESCRIPTION OF THE FIGURES
(1) The invention will be better understood through the description of example preferred embodiments and in reference to the drawings, wherein
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DESCRIPTION OF EXAMPLE EMBODIMENTS OF THE INVENTION
(19) The invention makes use of direct cantilever actuation to perform the tip-sample distance modulation. In this case, the tip sample distance is preferably modulated through a deformation of the whole or part of the cantilever. In contrast, in conventional methods either the cantilever as a whole is displaced or the sample is displaced to modulate the tip-sample distance.
(20) Here, we refer to “cantilever” as the probe consisting of a cantilever with tip at the distal end as is commonly used in the field, as well as other cantilever structures or MEMS devices that could be usable in scanning probe microscopy, such as but not limited to a membran.sup.11 or a dual stage cantilever.sup.12,13. In a preferred embodiment a photothermal actuation of the cantilever is used.
(21) Cantilever Motion and Photothermal Peak Force Deflection Signal
(22) In Photothermal actuation, a laser beam is focused preferably on the base of the cantilever, which results in local heating. If the cantilever is asymmetric (for example through a metal coating), the local heating will result in a deflection of the cantilever through the bi-morph effect, see
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(24) Using this technique only the cantilever itself can be actuated, without having to move any larger mechanical components. This is easily possible to 100 kHz and beyond.
(25) The resulting cantilever deflection signal from photothermally actuated PF-QNM (PT-PF-QNM) which is different from the standard PF-QNM signal, since in the PT-PF-QNM the cantilever is both actuator and displacement/force sensor—see
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(27) The fact that only the cantilever itself can be actuated is not a problem, since PF-QNM uses a method to subtract parasitic cantilever motion such as viscous drag forces. This background subtraction incidentally also removes the actuator-sensor cross-talk in PT-PF-QNM, and the resulting measurement data is equally valid for PT-PF-QNM as for traditional PF-QNM.
(28) In
(29) Use of Photothermally Actuated PF-QNM for High-Speed AFM Operation
(30) In recent years two main trends have pushed the AFM market:
(31) 1) high-speed AFM, and
(32) 2) Nanomechanical characterization.
(33) The development of PF-QNM has added a third trend, which is towards ease of use with the goal of fully automated AFM imaging. Peak force-QNM (and the simplified version peak force tapping—PF-tapping or PFT) has gained popularity due to the much simple feedback situation in PF-QNM than in conventional tapping-mode AFM (which is currently the most widely used AFM mode). Many users are willing to trade the imaging speed for ease of use. The herein described devices and methods according to the invention allow to increase the imaging speed of PF-tapping by one order of magnitude, and potentially surpass the imaging speeds of current generations of general purpose high-speed AFMs (HS-AFMs).
(34) The invention will be better understood through the following description of example illustrated by Figures as appropriate.
(35) The invention is of course not limited to this example.
(36) A review of the peak force tapping mode of imaging is described in US patent publications U.S. Pat. No. 8,646,109 B2 and U.S. Pat. No. 8,650,660 B2 and is incorporated by reference herein.
(37) During operation, probe deflection is measured by bouncing a light beam “L” off the back of the probe and toward a detector 114, such as a four quadrant photodetector. The deflection signal is then transmitted to an analog to digital converted 103. The digitized signal is used for maintaining the tip-sample force low while operating the AFM at high speed.
(38) In the embodiment shown in
(39) For generating the tip-sample distance modulation, the synchronization signal from Block 127 is converted to analog with converter 136 and applied to laser drive circuit 141 which modulates the intensity of the light beam “DL”.
(40) In the embodiment shown in
(41) For generating the tip-sample distance modulation, the synchronization signal from Block 227 is converted to analog with converter 236 and applied to laser drive circuit 241 which modulates the intensity of the light beam “DL”.
(42) The embodiment in
(43) In
(44) Motion of the probe is then detected; in particular, probe deflection is detected and transmitted to the converter for further processing. In Block 306, the method then operates to recover probe-sample interaction as described above, preferably performing subtraction of both the actuation and hydrodynamic background using either lock-in amplification, or more preferably, synchronous averaging of the deflection. After filtering the output in Block 308 (e.g. selecting a number of cycles of ringdown to process), the method detects the force (peak force detection/gated averaging), preferably using the repulsive region of the force curve, in Block 310. In Block 312, the force is then compared to the setpoint force, set according to the user's desired interaction force. The Z-actuator responds to the control signals in Block 316 to adjust tip-sample separation and maintain the setpoint force, with the control signals being used to generate an image of the sample.
(45) The method of setting the desired peak force tapping amplitude is shown in
(46) Reconstruction of Force Distance Curve Taking into Account the Different Deflection Sensitivities when the Cantilever Tip is in Free Air and when it is in Contact.
(47) Since in PT-PFT the cantilever acts as sensor and as actuator, the actuation of the cantilever is inherently embedded in the deflection signal. In addition, since the actuation of the tip motion occurs at a different place (the base of the cantilever) than the detection of the tip (detected through the measurement of the cantilever angle at the tip) the coupling of the actuation into the detection signal is not always constant. In particular it depends on if the tip touches the surface or not. When the tip is in free air, the cantilever follows the bending profile of a single sided cantilever beam with induced asymmetric stress. Once the surface is in contact, the cantilever bending line is that of a beam supported on one side with a fixed support and on the other with a sliding pin support.
(48) This additional correction can be performed as an additional step or as part of block 306 in
(49) Alternatively to the commonly used optical lever deflection system an interferometric detection scheme could be used. This would enable the absolute measurement of the cantilever deflection due to cantilever actuation or cantilever-sample interaction. The photothermal actuation can be either coupled through the interferometer or via a different light path.
(50) Alternatively to optical detection methods to measure the cantilever deflection one can also use other methods such as strain sensing methods (including but not limited to piezoresistive, piezoelectric, etc). The above described correction may or may not be applicable to these situations. Depending on the situation a different correction procedure may be required before or as part of block 306.
(51) Optimization of Cantilevers for PT-PFT
(52) Cantilevers can be made with dedicated coatings for high bimorph effect and large heat dissipation for high-bandwidth actuation. For the current tests, we used commercial cantilevers that are not specifically optimized for photothermal actuation. This limits the actuation efficiency and thereby the ultimate bandwidth that can be achieved. Optimization of the cantilever could focus on aspects such as:
(53) 1) improving the actuation efficiency when the laser is on,
(54) 2) ensuring sufficiently fast heat dissipation when the laser is off, and
(55) 3) optimize the spring constant for specific applications.
(56) A high photothermal drive efficiency requires a combination of a high bimorph effect (for example by using materials with very different thermal expansion coefficients, or by optimizing the relative layer thicknesses) with a coating that absorbs sufficient amounts of light to locally heat the cantilever. To achieve high bandwidth the stored thermal energy in the cantilever has to dissipate quickly for the cantilever to return again to its original position. The amount of cantilever deflection that can be achieved due to the photothermally induced stress depends on the elastic modulus of the material and the spring constant of the beam.
(57) Optimization of cantilever properties for PT-PFT performance could take place via strategies such as those illustrated in
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(59) Physical Implementation and Practical Testing
(60) The inventors have tested the concept using a home built AFM-head with photo-thermal actuation.sup.14 in conjunction with a custom Nanoscope PF-QNM workspace provided by Bruker Nano Inc. The schematic of the experimental setup is shown in
(61) Advantageously two laser beams are focused on the cantilever, one to detect the cantilever deflection (focused near the tip end of the cantilever) and one to perform the actuation (focused near the base of the cantilever). The detection laser is either powered continuously or with a frequency much higher than the first resonance frequency of the cantilever. The actuation laser is powered with a varying intensity corresponding to the trajectory used for the PF-modulation. This modulation can either be done in current control mode or in power control mode, with or without an additional high frequency modulation. By simple rerouting the signal that is originally intended for the Z-modulation Piezo into the modulation power input of our photothermal head the cantilever can be modulated to frequencies of around 100 kHz (see
(62) The reflected light from the actuation laser is blocked from entering the detector (position sensitive device, PSD) by an optical filter. The readout laser passes that filter and the position at which the readout laser hits the PSD is transformed into an electronic signal. This signal is then used for the deflection input into the peak-force AFM controller.
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(64) The concept of a unified optics block and the basic optical architecture are described in U.S. Pat. No. 6,871,527 B2. The use of a secondary housing on an adjustable kinematic mount for photothermal actuation is described in reference.sup.14.
(65) Results
(66) Several standard AFM samples were imaged to demonstrate the performance of the technique.
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(76) To demonstrate the improved speed performance through the use of PT-PFT we imaged Celgard 2400 membranes in air and water at different line-rates (surface speeds), see
(77) In
(78) Other Embodiments
(79) Instead of using a laser to heat and actuate the cantilever other direct cantilever actuation signals can be used, such as: Piezoelectric.sup.13, Electrothermal.sup.15,16, Magnetic.sup.17, Electrostatic.sup.18.
(80) With respect to photothermal actuation, instead of using two lasers (one for detection and one for actuation) only one laser to perform both tasks can be used. Here the peak force actuation signal is used to modulate the intensity of the readout laser. This however also changes the intensity of the laser beam that hits the PSD. In this case it is essential to subtract the background of changing intensity. This may be done using a normalization of the deflection signal to the PSD output using a divider circuit as is commonly done in the art, or using a readout technique such as that described in reference.sup.19 that provides a normalized signal output. The background subtraction could also be performed using the background generator and subtraction circuit described in
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