CN111398638B - Kelvin probe force microscope system and sample side wall scanning method - Google Patents
Kelvin probe force microscope system and sample side wall scanning method Download PDFInfo
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- CN111398638B CN111398638B CN202010238378.0A CN202010238378A CN111398638B CN 111398638 B CN111398638 B CN 111398638B CN 202010238378 A CN202010238378 A CN 202010238378A CN 111398638 B CN111398638 B CN 111398638B
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- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
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- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
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Abstract
Kelvin probe force microscope system based on orthogonal probe and sample side wall scanning method, belonging to Kelvin probe force microscope measuring technical field. The invention aims to solve the problem that the existing Kelvin probe force microscope cannot realize measurement of the surface morphology and the surface potential of the side wall of the micro-nano three-dimensional structure on the semiconductor component. The method comprises the steps of designing a novel orthogonal probe structure, and measuring the surface morphology and the local surface potential of the side wall of a sample with a micro-nano three-dimensional structure by using a torsion signal of the orthogonal probe; in the method, the first step is to measure the surface morphology of the side wall of the sample, the second and third steps are to measure the surface potential of the side wall of the sample, and the fourth step is to measure the surface of the side wall of the sample by imaging. The invention is used for realizing the measurement of the surface morphology and the local surface potential of the side wall of the sample with the micro-nano three-dimensional structure.
Description
Technical Field
The invention relates to a Kelvin probe force microscope system based on an orthogonal probe and a sample side wall scanning method, and belongs to the technical field of Kelvin probe force microscope measurement.
Background
Kelvin probe force microscopy (Kelvin probe force microscopy, KPFM) is a member of the family of scanning probe microscopes (Scanning probe microscopy, SPM) that combines Kelvin technology with atomic force microscopy (Atomic force microscopy, AFM) to enable characterization of sample surface potential and surface topography. Depending on the detection method, kelvin probe force microscopy KPFM can be divided into two modes of operation: amplitude modulation mode (Amplitude modulation, AM) and frequency modulation mode (Frequency modulation, FM), wherein AM-KPFM is detected based on electrostatic force and FM-KPFM is detected based on electrostatic force gradient.
The surface potential energy of the sample accurately reflects the surface structural characteristics of the material and the physical and chemical changes of the material, and is one of important parameters in the processes of catalyst activity, doping of semiconductors, bending of the belt, charge trapping in dielectrics and corrosion; while the local surface potential is very important for understanding the performance, microbial activity, and functionality of the microelectronic device at the micro-nano scale of the material, it is therefore very interesting to accurately measure the local surface potential of the sample. The measurement of the vertical sidewall surface of a sample is an important means for detecting the processing performance of a sample in the semiconductor industry, so how to scan the vertical sidewall surface of a sample to obtain the electrical performance parameters of the sidewall becomes a key for improving the micro-nano processing technology.
The existing Kelvin probe force microscope measurement system and method based on rectangular beam probe normal signals are very mature and widely applied to the technology of representing the appearance and local surface potential of the horizontal surface of a sample, and the Kelvin probe force microscope measurement system and method can be used for measuring the appearance and the surface potential of the horizontal surface of the sample under the condition that the surface of the sample to be measured is perpendicular to the normal direction of a rectangular beam probe tip. But cannot realize the characterization of the surface morphology and the surface potential of the side wall of the micro-nano three-dimensional structure which are common on the semiconductor component.
At present, aiming at a micro-nano three-dimensional structure on a semiconductor component, only the side wall scanning of the surface morphology can be realized, but the synchronous measurement of the surface potential of the side wall of the micro-nano three-dimensional structure cannot be realized at the same time.
Disclosure of Invention
The invention provides a Kelvin probe force microscope system based on an orthogonal probe and a sample side wall scanning method, which aims to solve the problem that the existing Kelvin probe force microscope can not realize the measurement of the surface morphology and the surface potential of the side wall of a micro-nano three-dimensional structure on a semiconductor component.
The Kelvin probe force microscope system based on the orthogonal probe comprises a probe hand 7, wherein the probe hand 7 comprises a probe hand base 7-1, a probe seat 7-3, an orthogonal probe 7-4, a shielding sheet 7-5, an orthogonal probe fixing plate 7-6 and a wiring terminal 7-7,
the rear end of the probe hand base 7-1 is connected with a wiring terminal 7-7, the lower surface of the front end of the probe hand base 7-1 is connected with a probe seat 7-3, and the lower surface of the probe seat 7-3 is connected with an orthogonal probe 7-4 through an orthogonal probe fixing plate 7-6; a shielding sheet 7-5 is arranged between the orthogonal probe fixing plate 7-6 and the probe seat 7-3; wherein insulating sheets are arranged between the probe hand base 7-1 and the probe seat 7-3 and between the shielding sheet 7-5 and the orthogonal probe fixing plate 7-6;
the probe hand base 7-1, the shielding sheet 7-5 and the orthogonal probe fixing plate 7-6 are respectively and electrically connected with corresponding interfaces of the wiring terminals 7-7; the orthogonal probe fixing plate 7-6 is electrically connected with the orthogonal probes 7-4;
the quadrature probe 7-4 is driven by a driving signal to achieve mechanical vibration at a first order torsional resonance frequency.
The Kelvin probe force microscope system based on the orthogonal probe according to the present invention, the orthogonal probe 7-4 comprises a cross beam 7-4-1, a magnetic ball 7-4-2, a longitudinal beam 7-4-3 and a front convex needle tip 7-4-4,
the cross beam 7-4-1 is connected with the orthogonal probe fixing plate 7-6 through the probe support, the lower surface of the cross beam 7-4-1 is connected with the magnetic ball 7-4-2, the side surface of the magnetic ball 7-4-2 is connected with the longitudinal beam 7-4-3 in the vertical direction, and the outer side surface of the tail end of the longitudinal beam 7-4-3 is connected with the front convex needle point 7-4-4.
The Kelvin probe force microscope system based on the orthogonal probe according to the invention further comprises a Kelvin sample stage 15, wherein the Kelvin sample stage 15 comprises a Kelvin sample stage base 15-1, an inductance coil wiring terminal 15-2, an inductance coil 15-3, a sample holder 15-4, a connecting wire 15-5, a set screw 15-6, a wire harness block 15-7, a copper pressing piece 15-8 and an insulation fixing screw 15-10,
the sample seat 15-4 is arranged on the Kelvin sample stage base 15-1; the upper surface of the sample seat 15-4 is used for placing a sample 15-9, and an insulating sheet is arranged between the sample seat 15-4 and the sample 15-9;
the inductance coil 15-3 is fixed in the hollow inner cavity of the sample holder 15-4, and the inductance coil wiring terminal 15-2 is led out from the inductance coil 15-3 and is used for being electrically connected with corresponding electrical equipment;
the copper pressing sheet 15-8 is fixed on the sample seat 15-4 through an insulating fixing screw 15-10, and the copper pressing sheet 15-8 is electrically connected with the sample 15-9;
the edge of the upper surface of the sample seat 15-4 is also fixed with a wire harness block 15-7, the connecting wire 15-5 passes through the wire harness block 15-7, and the wire harness block 15-7 is in threaded fit with the set screw 15-6 to fix the connecting wire 15-5; the copper pressing sheet 15-8 is electrically connected with the connecting wire 15-5, and the connecting wire 15-5 is used for being electrically connected with corresponding electrical equipment;
the magnetic field generated by the inductance coil 15-3 drives the orthogonal probe 7-4 through the magnetic ball 7-4-2.
The sample side wall scanning method of the Kelvin probe force microscope based on the orthogonal probe is realized based on the Kelvin probe force microscope system based on the orthogonal probe, and comprises the following steps of:
step one: mechanically exciting the quadrature probe 7-4 at a first order torsional resonance frequency to vibrate the quadrature probe 7-4 at a set torsional amplitude; gradually approaching the forward protruding tip 7-4-4 to the sample 15-9 along the Y direction of the XYZ coordinate system until the torsional amplitude of the orthogonal probe 7-4 is attenuated to the torsional amplitude set point; the Z direction of the XYZ coordinate system is the vertical direction;
step two: applying a low-frequency alternating current voltage and a direct current compensation voltage between the quadrature probe 7-4 and the sample 15-9, and changing the magnitude of the direct current compensation voltage to obtain an amplitude relation curve of the direct current compensation voltage and a torsional vibration phase signal of the quadrature probe 7-4 under the first-order torsional resonance frequency, wherein the change frequency of the torsional vibration phase signal is consistent with the frequency of the low-frequency alternating current voltage; according to the relation curve, selecting an amplitude set value of a torsional vibration phase signal of the quadrature probe 7-4;
step three: the DC compensation voltage is regulated through a Kelvin controller, so that the amplitude of the torsional vibration phase signal of the quadrature probe 7-4 is equal to the amplitude set value of the torsional vibration phase signal of the quadrature probe 7-4;
step four: setting a scanning step distance and a scanning test point number of the sample 15-9, wherein the scanning step distance and the scanning test point number comprise an X direction and a Z direction; the position of the quadrature probe 7-4 is kept unchanged, scanning test points of the sample 15-9 are sequentially changed, and the torsional amplitude of the quadrature probe 7-4 is kept equal to a torsional amplitude set value under the mechanical excitation and the electric excitation corresponding to each scanning test point, and the amplitude of a torsional vibration phase signal is kept equal to an amplitude set value of the torsional vibration phase signal; imaging measurements of the surface topography and surface potential of the side walls of the samples 15-9 were achieved.
According to the sample side wall scanning method of the Kelvin probe force microscope based on the orthogonal probe, the imaging measurement of the surface morphology of the side wall of the sample 15-9 comprises the following steps:
fixing a sample 15-9 on a sample seat 15-4, and changing the coordinate position of the sample 15-9 through an XYZ nanometer positioning table 13 connected with a Kelvin sample table base 15-1 to realize the conversion of a sample 15-9 scanning test point; at each scan test point, keeping the Y-direction coordinates of the quadrature probe 7-4 unchanged, and making the torsional amplitude of the quadrature probe 7-4 equal to the torsional amplitude set value by changing the Y position of the Kelvin sample stage base 15-1; and the Y-direction coordinates of the Kelvin sample stage base 15-1 are recorded in sequence when each test point is scanned, so that imaging measurement of the surface morphology of the side wall of the sample 15-9 is realized.
According to the sample side wall scanning method of the Kelvin probe force microscope based on the orthogonal probe, the imaging measurement of the surface potential of the side wall of the sample 15-9 comprises the following steps:
obtaining a local surface potential difference U between the orthogonal probe 7-4 and the sample 15-9 scanning test spot CPD ：
The total potential difference DeltaU between the orthogonal probe 7-4 and the sample 15-9 is:
ΔU＝U DC -U CPD +U AC sin(ω AC t)，
wherein U is DC For the DC compensation voltage, U AC sin(ω AC t) is the low frequency alternating voltage, ω AC The frequency of the low-frequency alternating voltage;
at this time, the gradient F 'of electrostatic force between the orthogonal probe 7-4 and the surface of the sample 15-9' el The method comprises the following steps:
wherein C is the capacitance between the orthogonal probe 7-4 and the sample 15-9, and z is the distance between the orthogonal probe 7-4 and the sample 15-9;
by recording torsional vibrations of the quadrature probe 7-4DC compensation voltage U when amplitude of phase signal is equal to amplitude set value of torsional vibration phase signal DC And determining the local surface potential difference U between the orthogonal probe 7-4 and the sample 15-9 scanning test point by combining the relation curve CPD 。
The invention has the advantages that: the system and the method are used for realizing the characterization of the surface morphology and the local surface potential of the side wall of the sample, a novel orthogonal probe structure is designed in the system, and then the surface morphology and the local surface potential of the side wall of the sample with the micro-nano three-dimensional structure are measured by utilizing the torsion signal of the orthogonal probe.
The invention breaks through the space limitation of the traditional KPFM for carrying out surface potential measurement based on the normal signal of the rectangular beam probe, and can realize the synchronous characterization of the surface morphology and the surface potential of the side wall of the micro-nano three-dimensional structure by utilizing the torsion signal feedback of the orthogonal probe; the method provides a new idea for further researching the surface potential of the side wall of the sample; the front convex needle tip of the orthogonal probe can penetrate into a three-dimensional sample gap with higher density to scan the side wall of the sample, and the additional effect brought by the horn probe used in the traditional side wall morphology scanning can be avoided.
Compared with the traditional KPFM, the method can realize the synchronous characterization of the surface morphology and the potential of the side wall of the sample by taking the torsion signal of the orthogonal probe as feedback, has great significance for the monitoring and control of the device performance, does not need to make any change on a KPFM test system or a Kelvin controller, is compatible with the traditional KPFM test system, and has high practical value in the KPFM test method and system research fields.
Drawings
FIG. 1 is a schematic diagram of the hand structure of a Kelvin probe force microscope system based on orthogonal probes according to the invention;
FIG. 2 is a schematic diagram of the structure of an orthogonal probe;
FIG. 3 is a front view of FIG. 2;
FIG. 4 is a side view of FIG. 2;
FIG. 5 is a schematic structural view of a Kelvin sample stage;
FIG. 6 is a top view of FIG. 5;
FIG. 7 is a schematic diagram of the orthogonal probe scanning position determination process when the height of the side wall of the sample is small;
FIG. 8 is a front view of a scan of an orthogonal probe;
FIG. 9 is a scanning side view of an orthogonal probe;
FIG. 10 is a scanning axonometric view of an orthogonal probe;
FIG. 11 is a block diagram of the overall principle of a control implementation of the method of the present invention;
FIG. 12 is an enlarged view of a portion of the Kelvin sample stage of FIG. 11 in position;
FIG. 13 is a schematic diagram of the overall structure of a Kelvin probe force microscope system based on orthogonal probes according to the invention; in the figure 1: a frame; 2: the four-quadrant position detector adjusts the micro platform in two dimensions; 3: one-dimensional adjustment of the micro platform I;4: a four-quadrant position detector; 5: reflecting the laser convex lens; 6: a laser mirror; 7: a probe hand; 8: an XYZ micron positioning stage; 9: a probe hand support; 10: one-dimensional wide-range adjustment micro-platform; 11: a table top; 12: an XY micron positioning stage; 13: an XYZ nano positioning table; 14: a sample stage support; 15: kelvin scanning of the sample stage; 16: an incident laser focusing convex lens; 17: one-dimensional adjustment of the micro platform II;18: a semiconductor laser generator; 19: an angle adjusting mechanism of the laser generator; 20: an optical microscope;
FIG. 14 is a surface topography obtained by scanning a sample using the method of the present invention;
FIG. 15 is a cross-sectional view corresponding to the marked line in FIG. 14;
FIG. 16 is a plot of the surface potential difference obtained by scanning a sample using the method of the present invention;
fig. 17 is a graph corresponding to the statistical distribution of data in fig. 16 and a fitting result.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The first embodiment is as follows: next, referring to fig. 1 and 13, the kelvin probe force microscope system based on the orthogonal probe according to the present embodiment includes a probe hand 7,
the probe hand 7 comprises a probe hand base 7-1, a probe seat 7-3, an orthogonal probe 7-4, a shielding sheet 7-5, an orthogonal probe fixing plate 7-6 and a wiring terminal 7-7,
the rear end of the probe hand base 7-1 is connected with a wiring terminal 7-7, the lower surface of the front end of the probe hand base 7-1 is connected with a probe seat 7-3, and the lower surface of the probe seat 7-3 is connected with an orthogonal probe 7-4 through an orthogonal probe fixing plate 7-6; a shielding sheet 7-5 is arranged between the orthogonal probe fixing plate 7-6 and the probe seat 7-3; wherein insulating sheets are arranged between the probe hand base 7-1 and the probe seat 7-3 and between the shielding sheet 7-5 and the orthogonal probe fixing plate 7-6;
the probe hand base 7-1, the shielding sheet 7-5 and the orthogonal probe fixing plate 7-6 are respectively and electrically connected with corresponding interfaces of the wiring terminals 7-7; the orthogonal probe fixing plate 7-6 is electrically connected with the orthogonal probes 7-4;
the quadrature probe 7-4 is driven by a driving signal to achieve mechanical vibration at a first order torsional resonance frequency.
Further, as shown in connection with FIGS. 2 to 4, the orthogonal probe 7-4 includes a cross beam 7-4-1, a magnetic ball 7-4-2, a stringer 7-4-3 and a forward protruding tip 7-4-4,
the cross beam 7-4-1 is connected with the orthogonal probe fixing plate 7-6 through the probe support, the lower surface of the cross beam 7-4-1 is connected with the magnetic ball 7-4-2, the side surface of the magnetic ball 7-4-2 is connected with the longitudinal beam 7-4-3 in the vertical direction, and the outer side surface of the tail end of the longitudinal beam 7-4-3 is connected with the front convex needle point 7-4-4.
Still further, as shown in connection with FIGS. 5 and 6, the present embodiment further includes a Kelvin sample stage 15, the Kelvin sample stage 15 including a Kelvin sample stage base 15-1, an inductance coil connection terminal 15-2, an inductance coil 15-3, a sample holder 15-4, a connection wire 15-5, a set screw 15-6, a harness block 15-7, a copper press sheet 15-8, and an insulation set screw 15-10,
the sample seat 15-4 is arranged on the Kelvin sample stage base 15-1; the upper surface of the sample seat 15-4 is used for placing a sample 15-9, and an insulating sheet is arranged between the sample seat 15-4 and the sample 15-9;
the inductance coil 15-3 is fixed in the hollow inner cavity of the sample holder 15-4, and the inductance coil wiring terminal 15-2 is led out from the inductance coil 15-3 and is used for being electrically connected with corresponding electrical equipment, wherein the corresponding electrical equipment comprises an inductance coil controller, as shown in fig. 11;
the copper pressing sheet 15-8 is fixed on the sample seat 15-4 through an insulating fixing screw 15-10, and the copper pressing sheet 15-8 is electrically connected with the sample 15-9;
the edge of the upper surface of the sample seat 15-4 is also fixed with a wire harness block 15-7, the connecting wire 15-5 passes through the wire harness block 15-7, and the wire harness block 15-7 is in threaded fit with the set screw 15-6 to fix the connecting wire 15-5; the copper pressing sheet 15-8 is electrically connected with the connecting wire 15-5, and the connecting wire 15-5 is used for being electrically connected with corresponding electrical equipment, and the corresponding electrical equipment comprises a signal adder for synthesizing signals of the signal generator 2 and the direct current power supply in fig. 11;
the magnetic field generated by the inductance coil 15-3 drives the orthogonal probe 7-4 through the magnetic ball 7-4-2.
The inductance coil 15-3 can generate a uniform magnetic field, and is matched with the magnetic ball 7-4-2 to function, so that the magnetic driving of the orthogonal probe 7-4 is realized.
As shown in fig. 13, the overall structure of the kelvin probe force microscope system based on the orthogonal probe according to the present embodiment further includes: the table top 11, the frame 1, the one-dimensional wide-range adjustment micro-platform 10, the XY micron positioning table 12 and the optical microscope 20 are arranged on the table top 11. The Kelvin sample stage 15 is installed on the XY micrometer positioning stage 12 through a sample stage support 14 and an XYZ nanometer positioning stage 13, the laser force measuring system is installed on the frame 1, and the probe hand 7 is installed on the one-dimensional large-range adjustment micro-platform 10 through a probe hand support 9 and an XYZ micrometer positioning stage 8.
The laser force measuring system is composed of a laser generator angle adjusting mechanism 19, a semiconductor laser generator 18, an incident laser focusing convex lens 16, a laser reflector 6, a reflecting laser convex lens 5, a four-quadrant position detector 4, a one-dimensional adjusting micro-platform II17, a one-dimensional adjusting micro-platform I3 and a two-dimensional adjusting micro-platform 2 of the four-quadrant position detector.
The structure of the probe hand 7 can also comprise piezoelectric ceramics 7-2, wherein the piezoelectric ceramics 7-2 are connected between the probe hand base 7-1 and the probe seat 7-3, insulating sheets are arranged on the upper surface and the lower surface of the piezoelectric ceramics 7-2, and the piezoelectric ceramics 7-2 are electrically connected with corresponding interfaces of the wiring terminals 7-7; the piezoelectric ceramic 7-2 can also realize mechanical driving of the orthogonal probe 7-4.
In fig. 12, B is the electromagnetic field direction, m is the magnetization direction of the magnetic ball, τ is the moment direction of the magnetic ball, and the magnetically driven sample stage is the kelvin sample stage 15; in fig. 11, (1) represents a piezoelectric ceramic-driven wiring scheme and (2) represents a magnetic field-driven wiring scheme, and one of them is optionally used in actual measurement.
The second embodiment is as follows: the following describes a sample sidewall scanning method of a Kelvin probe force microscope based on an orthogonal probe according to the present embodiment with reference to fig. 7 to 12, and the Kelvin probe force microscope system based on an orthogonal probe according to the first embodiment includes the following steps:
step one: mechanically exciting the quadrature probe 7-4 at a first order torsional resonance frequency to vibrate the quadrature probe 7-4 at a set torsional amplitude; gradually approaching the forward tip 7-4-4 to the sample 15-9 along the Y direction shown in FIG. 9 and FIG. 12 of the XYZ coordinate system until the torsional amplitude of the quadrature probe 7-4 decays to the torsional amplitude set point; the Z direction of the XYZ coordinate system is the vertical direction;
step two: applying a low-frequency alternating current voltage and a direct current compensation voltage between the quadrature probe 7-4 and the sample 15-9, and changing the magnitude of the direct current compensation voltage to obtain an amplitude relation curve of the direct current compensation voltage and a torsional vibration phase signal of the quadrature probe 7-4 under the first-order torsional resonance frequency, wherein the change frequency of the torsional vibration phase signal is consistent with the frequency of the low-frequency alternating current voltage; according to the relation curve, selecting an amplitude set value of a torsional vibration phase signal of the quadrature probe 7-4;
step three: setting parameters of a Kelvin controller, and then starting, and adjusting the direct current compensation voltage through the Kelvin controller to enable the amplitude of the torsional vibration phase signal of the quadrature probe 7-4 to be equal to the amplitude set value of the torsional vibration phase signal of the quadrature probe 7-4;
step four: setting a scanning step distance and a scanning test point number of the sample 15-9, wherein the scanning step distance and the scanning test point number comprise an X direction and a Z direction; the position of the quadrature probe 7-4 is kept unchanged, scanning test points of the sample 15-9 are sequentially changed, and the torsional amplitude of the quadrature probe 7-4 is kept equal to a torsional amplitude set value under the mechanical excitation and the electric excitation corresponding to each scanning test point, and the amplitude of a torsional vibration phase signal is kept equal to an amplitude set value of the torsional vibration phase signal; imaging measurements of the surface topography and surface potential of the side walls of the samples 15-9 were achieved. The torsional amplitude of the quadrature probe 7-4 and the amplitude of the torsional vibration phase signal are used as feedback signals to realize displacement control and potential compensation of sample scanning.
In the embodiment, the first step is to measure the surface morphology of the side wall of the sample, the second and third steps are to measure the surface potential of the side wall of the sample, and the fourth step is to measure the surface of the side wall of the sample by imaging. Thanks to the structural characteristics of the orthogonal probe, the torsion signal of the orthogonal probe can well reflect the interaction between the probe tip and the surface of the side wall, so that the surface morphology of the side wall of the sample and the local surface potential can be measured.
The method of the invention works in the frequency modulation mode of the microscope, and drives the probe at two frequencies simultaneously in the measuring process, wherein the method comprises the following steps: 1 mechanical driving of the quadrature probe 7-4 at a first order torsional resonance frequency; 2 low frequency electrical excitation between the quadrature probe 7-4 and the sample 15-9. The displacement control and the potential compensation of the scanning can be realized by taking the torsion signal of the orthogonal probe 7-4 as feedback through the upper computer, so that the simultaneous measurement of the surface morphology and the local surface potential of the sample is realized. The amount of force deflection of the quadrature probe 7-4 can be measured by a laser force measurement system.
In the test of this embodiment, the forward protruding tip 7-4-4 interacts with the three-dimensional sidewall surface of the sample, resulting in torsion of the beam 7-4-1 by the force of the probe stringer 7-4-3, which is detected by the laser force measuring system and used for feedback control of the entire scanning process. The method breaks through the limitation that surface characterization can only be carried out in a horizontal plane based on normal signal measurement of the traditional rectangular beam probe, and synchronous measurement of the surface morphology and the potential of the side wall of the sample can be realized by utilizing the torsion signal of the orthogonal probe.
Further, as shown in connection with fig. 7, the implementation of the imaging measurement of the sidewall surface topography of the sample 15-9 according to the present embodiment includes:
fixing a sample 15-9 on a sample seat 15-4, and changing the coordinate position of the sample 15-9 through an XYZ nanometer positioning table 13 connected with a Kelvin sample table base 15-1 to realize the conversion of a sample 15-9 scanning test point; at each scan test point, keeping the Y-direction coordinates of the quadrature probe 7-4 unchanged, and making the torsional amplitude of the quadrature probe 7-4 equal to the torsional amplitude set value by changing the Y position of the Kelvin sample stage base 15-1; and the Y-direction coordinates of the Kelvin sample stage base 15-1 are recorded in sequence when each test point is scanned, so that imaging measurement of the surface morphology of the side wall of the sample 15-9 is realized.
In FIG. 7, the first diagram shows the orthogonal probe servoing at the highest point of the three-dimensional sidewall structure of the sample; the second panel shows the orthogonal probe servoing at the lowest point of the three-dimensional sidewall structure of the sample; the third panel shows the sample stage Z descending downward by a certain height; the fourth panel shows the orthogonal probe servoing with the sidewall surface at the sidewall location point where the sample is measured.
Still further, the present embodiment enables imaging measurements of the sidewall surface potential of the sample 15-9 comprising:
obtaining a local surface potential difference U between the orthogonal probe 7-4 and the sample 15-9 scanning test spot CPD ：
During the test, the surface potential difference of the orthogonal probe 7-4 and the sample 15-9 is measured by taking as feedback the torsion signal of the probe due to the low frequency electrical excitation.
The total potential difference DeltaU between the orthogonal probe 7-4 and the sample 15-9 is:
ΔU＝U DC -U CPD +U AC sin(ω AC t)，
wherein U is DC For the DC compensation voltage, U AC sin(ω AC t) is the low frequency alternating voltage (electric excitation), ω AC The frequency of the low-frequency alternating voltage;
at this time, the gradient F 'of electrostatic force between the orthogonal probe 7-4 and the surface of the sample 15-9' el The method comprises the following steps:
wherein C is the capacitance between the orthogonal probe 7-4 and the sample 15-9, and z is the distance between the orthogonal probe 7-4 and the sample 15-9; as can be seen from the above, when U DC ＝U CPD When the electrostatic force gradient is omega AC The effect on the quadrature probe 7-4 at frequency will be eliminated. Due to the occurrence of electrostatic force gradients between probe-sample, the effective stiffness of the probe becomes:
k eff ＝k-F′ el ，
where k is the static stiffness of the probe.
Therefore, under the action of the electrostatic force gradient, the change of the resonance frequency of the probe is:
wherein omega is 0 Is the first order torsional resonance frequency of the probe. By recording the DC compensation voltage U at which the amplitude of the torsional vibration phase signal of the quadrature probe 7-4 is equal to the amplitude set point of the torsional vibration phase signal DC And determining the local surface potential difference U between the orthogonal probe 7-4 and the sample 15-9 scanning test point by combining the relation curve CPD 。
In the scanning method, the Z-direction coordinate value of the scanner is recorded when the torsional amplitude is set by the first-order torsional amplitude of the orthogonal probe 7-4, so that the surface topography image of the sample can be obtained;
in practical processing, as shown in connection with fig. 11, the change in resonance frequency of the probe is rarely measured directly by a single lock-in amplifier. Due to the phase of the probeThe amplitude of the signal is equal to zero, with Δω=0. Therefore, two lock-in amplifiers are typically employed to perform KPFM in FM mode: the first is locked to the resonance frequency (omega 0 ) The second one is locked to the frequency (omega AC ) By adjusting U DC Zero the amplitude feedback signal of the phase, then there is U DC ＝U CPD Thereby obtaining a local surface potential difference (U CPD )。
Referring to fig. 11 to 13, the specific test procedure of the method of the present invention is as follows:
1. initializing a system, namely fixing a prepared sample 15-9 on a sample seat 15-4, mounting an orthogonal probe 7-4 on a probe hand 7, then respectively mounting a Kelvin sample stage 15 and the probe hand 7 on a sample stage support 14 and a probe hand support 9, and finally electrically connecting a wiring terminal with corresponding equipment;
2. moving the XY micrometer positioning stage 12, positioning the sample 15-9 initially by the optical microscope 20, selecting a suitable measurement area, and moving the area to the center of the field of view of the optical microscope 20;
3. moving a one-dimensional wide-range adjustment micro platform 10 and an XYZ micrometer positioning platform 8, roughly aligning the orthogonal probe 7-4, placing the probe tip above the proper measurement area selected in the step 2, and adjusting the laser spot of the orthogonal probe 7-4 at the center of the front end of the probe beam;
4. carrying out sweep frequency operation on the orthogonal probe 7-4 through a sweep frequency exciter so as to obtain the first-order torsional resonance frequency of the orthogonal probe 7-4;
5. the scanning position is determined and is mainly divided into two types according to the differences of samples: 1, in a sample with larger side wall height, a needle point does not contact the root of the side wall in the side wall scanning process, the orthogonal probe 7-4 is moved to the front of the Y direction of the side wall of the sample to be detected in a rough adjustment mode through the XYZ micrometer positioning table 8, and the orthogonal probe 7-4 is directly lowered to the Z position to be detected; 2, the needle point 7-4-4 possibly contacts the root of the side wall in the scanning process, so that the side wall is firstly contacted with the top and the bottom of the side wall in a servo manner respectively, the side wall height is obtained according to the Z-direction coordinate of the XYZ nano positioning table 13 during the two servo contacts, then the XYZ nano positioning table 13 is moved to enable the needle point 7-4-4 to be aligned with the Z-direction of the position to be detected, and the Z-direction scanning distance is ensured to be smaller than the rest side wall height;
6. coarse-adjusting the Y-direction distance between the orthogonal probe 7-4 and the sample 15-9, and readjusting the laser spot of the orthogonal probe 7-4 to the center of the front end of the probe beam, so as to prepare to start the upper computer-position servo control;
7. mechanically exciting the probe at its first order torsional resonance frequency (U m ) The present invention may adopt two driving modes, but is not limited to these two driving modes: 1) The piezoelectric ceramic is driven, and the mechanical vibration of the probe under the first-order torsional resonance frequency is realized through the piezoelectric ceramic 7-2 driven by sinusoidal voltage; 2) The magnetic field is driven, and an alternating magnetic field is generated by using an inductance coil 15-3 in the Kelvin sample stage 15 under the driving of a sine voltage signal to drive a magnetic ball 7-4-2 magnetized in a designated direction, so that the mechanical vibration of the probe under the first-order torsional resonance frequency is realized under the action of an electromagnetic moment tau. Detecting a resonance signal generated by the quadrature probe 7-4 by using a laser force measuring system, obtaining a torsion amplitude and a phase signal of the probe by using a lock-in amplifier 1, then starting position servo control, and controlling the XYZ nanometer positioning table 13 to quickly approach the quadrature probe 7-4 in the Y-axis direction so that the torsion amplitude of the quadrature probe 7-4 is equal to a set value;
8. applying a low-rate (4 kHz) electrical excitation (U) between the quadrature probe 7-4 and the sample 15-9 AC ) And obtains the amplitude of the phase signal output by the phase-locked amplifier 1 through the phase-locked amplifier 2, and then obtains U DC A relation curve of the probe torsional vibration phase signal amplitude under the low frequency, and a set value of the probe torsional vibration phase signal amplitude is selected;
9. the Kelvin controller is turned on, and the program controls the DC power supply to output a DC compensation voltage (U DC ) Acts between the quadrature probe 7-4 and the sample 15-9 to compensate for the local potential difference (U) between the quadrature probe 7-4 and the surface of the sample 15-9 CPD ) To ensure that the amplitude of the output of the lock-in amplifier 2 is equal to the set point of the amplitude of the probe torsional vibration phase signal;
10. by passing throughThe above steps can be performed by the voltage (U DC ) And its relation to the torsional amplitude of the probe, to obtain the local potential difference (U) of the orthogonal probe 7-4 and sample 15-9 CPD )；
11. The scanning steps and the number of scanning points are set, and then image scanning is started.
The method is adopted to carry out measurement scanning on the sample with silicon-gold layering distributed on the side wall; obtain fig. 14 to 17; FIGS. 14-17 are sidewall scan images of a silicon-gold interface when placed vertically; in fig. 14, a high-luminance portion is a gold layer, and a low-luminance portion is a silicon substrate; the results in FIG. 15 show that the sample height is 18nm; the results of fig. 17 show that the surface potential difference of the silicon layer and the gold layer on the sample sidewall is 748mV, with a scan range of 2 μm by 2 μm and a scan number of 200 by 200.
Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims. It should be understood that the different dependent claims and the features described herein may be combined in ways other than as described in the original claims. It is also to be understood that features described in connection with separate embodiments may be used in other described embodiments.
Claims (5)
1. A Kelvin probe force microscope system comprising a probe hand (7), characterized in that,
the probe hand (7) comprises a probe hand base (7-1), a probe seat (7-3), an orthogonal probe (7-4), a shielding sheet (7-5), an orthogonal probe fixing plate (7-6) and a wiring terminal (7-7),
the rear end of the probe hand base (7-1) is connected with a wiring terminal (7-7), the lower surface of the front end of the probe hand base (7-1) is connected with a probe seat (7-3), and the lower surface of the probe seat (7-3) is connected with an orthogonal probe (7-4) through an orthogonal probe fixing plate (7-6); a shielding sheet (7-5) is arranged between the orthogonal probe fixing plate (7-6) and the probe seat (7-3); wherein insulating sheets are arranged between the probe hand base (7-1) and the probe seat (7-3) and between the shielding sheet (7-5) and the orthogonal probe fixing plate (7-6);
the probe hand base (7-1), the shielding sheet (7-5) and the orthogonal probe fixing plate (7-6) are respectively and electrically connected with corresponding interfaces of the wiring terminals (7-7); the orthogonal probe fixing plate (7-6) is electrically connected with the orthogonal probes (7-4);
the orthogonal probe (7-4) is driven by a driving signal to realize mechanical vibration at a first-order torsional resonance frequency;
the orthogonal probe (7-4) comprises a cross beam (7-4-1), a magnetic ball (7-4-2), a longitudinal beam (7-4-3) and a front convex needle point (7-4-4),
the cross beam (7-4-1) is connected with the orthogonal probe fixing plate (7-6) through the probe support, the lower surface of the cross beam (7-4-1) is connected with the magnetic ball (7-4-2), the side surface of the magnetic ball (7-4-2) is connected with the longitudinal beam (7-4-3) in the vertical direction, and the outer side surface of the tail end of the longitudinal beam (7-4-3) is connected with the front convex needle point (7-4-4).
2. The Kelvin probe force microscope system of claim 1, further comprising a Kelvin stage (15), the Kelvin stage (15) comprising a Kelvin stage base (15-1), an inductor winding connection terminal (15-2), an inductor winding (15-3), a sample holder (15-4), a connection wire (15-5), a set screw (15-6), a wire harness block (15-7), a copper strap (15-8), and an insulating set screw (15-10),
the sample seat (15-4) is arranged on the Kelvin sample table base (15-1); the upper surface of the sample seat (15-4) is used for placing a sample (15-9), and an insulating sheet is arranged between the sample seat (15-4) and the sample (15-9);
the inductance coil (15-3) is fixed in the hollow inner cavity of the sample seat (15-4), and the inductance coil wiring terminal (15-2) is led out from the inductance coil (15-3) and is used for being electrically connected with corresponding electrical equipment;
the copper pressing sheet (15-8) is fixed on the sample seat (15-4) through an insulating fixing screw (15-10), and the copper pressing sheet (15-8) is electrically connected with the sample (15-9);
the edge of the upper surface of the sample seat (15-4) is also fixed with a wire harness block (15-7), the connecting wire (15-5) passes through the wire harness block (15-7), and the wire harness block (15-7) is in threaded fit with the set screw (15-6) to fix the connecting wire (15-5); the copper pressing sheet (15-8) is electrically connected with the connecting wire (15-5), and the connecting wire (15-5) is used for being electrically connected with corresponding electrical equipment;
the magnetic field generated by the inductance coil (15-3) drives the orthogonal probe (7-4) through the magnetic ball (7-4-2).
3. A method of scanning a sample sidewall of a kelvin probe force microscope based on the kelvin probe force microscope system according to claim 2, characterized by comprising the steps of:
step one: mechanically exciting the quadrature probe (7-4) at a first order torsional resonance frequency to vibrate the quadrature probe (7-4) at a set torsional amplitude; gradually approaching the forward protruding tip (7-4-4) to the sample (15-9) along the Y direction of the XYZ coordinate system until the torsion amplitude of the orthogonal probe (7-4) is attenuated to a torsion amplitude set value; the Z direction of the XYZ coordinate system is the vertical direction;
step two: applying a low-frequency alternating current voltage and a direct current compensation voltage between the quadrature probe (7-4) and the sample (15-9), and changing the magnitude of the direct current compensation voltage to obtain an amplitude relation curve of the direct current compensation voltage and a torsional vibration phase signal of the quadrature probe (7-4) under a first-order torsional resonance frequency, wherein the change frequency of the torsional vibration phase signal is consistent with the frequency of the low-frequency alternating current voltage; according to the relation curve, selecting an amplitude set value of a torsional vibration phase signal of the quadrature probe (7-4);
step three: adjusting the direct current compensation voltage through a Kelvin controller to enable the amplitude of the torsional vibration phase signal of the quadrature probe (7-4) to be equal to the amplitude set value of the torsional vibration phase signal of the quadrature probe (7-4);
step four: setting a scanning step distance and a scanning test point number of the sample (15-9), wherein the scanning step distance and the scanning test point number comprise an X direction and a Z direction; the position of the quadrature probe (7-4) is kept unchanged, scanning test points of the sample (15-9) are sequentially transformed, and the torsional amplitude of the quadrature probe (7-4) is kept equal to a torsional amplitude set value under the action of mechanical excitation and electric excitation corresponding to each scanning test point, and the amplitude of a torsional vibration phase signal is equal to an amplitude set value of the torsional vibration phase signal; imaging measurement of the surface topography and surface potential of the side wall of the sample (15-9) is realized.
4. A sample sidewall scanning method of a kelvin probe force microscope according to claim 3, characterized in that the realization of the imaging measurement of the surface topography of the sidewall of the sample (15-9) comprises:
fixing a sample (15-9) on a sample seat (15-4), and changing the coordinate position of the sample (15-9) through an XYZ nanometer positioning table (13) connected with a Kelvin sample table base (15-1) to realize the conversion of a sample (15-9) scanning test point; at each scan test point, keeping the Y-direction coordinate of the quadrature probe (7-4) unchanged, and enabling the torsion amplitude of the quadrature probe (7-4) to be equal to the torsion amplitude set value by changing the Y-direction position of the Kelvin sample stage base (15-1); and (3) recording Y-direction coordinates of the Kelvin sample stage base (15-1) when each test point is scanned in sequence, and realizing imaging measurement of the surface morphology of the side wall of the sample (15-9).
5. The method of scanning the side wall of a sample in a kelvin probe force microscope according to claim 4, characterized in that the implementation of the imaging measurement of the side wall surface potential of the sample (15-9) includes:
obtaining a local surface potential difference U between the orthogonal probe (7-4) and the sample (15-9) scanning test point CPD ：
The total potential difference DeltaU between the orthogonal probe (7-4) and the sample (15-9) is:
ΔU＝U DC -U CPD +U AC sin(ω AC t)，
wherein U is DC For the DC compensation voltage, U AC sin(ω AC t) is the low frequency alternating voltage, ω AC The frequency of the low-frequency alternating voltage; u (U) AC An electrical excitation applied between the orthogonal probe (7-4) and the sample (15-9);
at this time, the gradient F of electrostatic force between the orthogonal probe (7-4) and the surface of the sample (15-9) e ′ l The method comprises the following steps:
wherein C is the capacitance between the orthogonal probe (7-4) and the sample (15-9), and z is the distance between the orthogonal probe (7-4) and the sample (15-9);
by recording the DC compensation voltage U at which the amplitude of the torsional vibration phase signal of the quadrature probe (7-4) is equal to the amplitude set point of the torsional vibration phase signal DC And determining the local surface potential difference U between the orthogonal probe (7-4) and the sample (15-9) scanning test point by combining the relation curve CPD 。
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| CN114088981B (en) * | 2021-10-21 | 2023-05-23 | 华南理工大学 | Side wall scanning probe and processing method thereof |
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