CN101493397B - Electrostatic force microscope and measurement method thereof - Google Patents
Electrostatic force microscope and measurement method thereof Download PDFInfo
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- CN101493397B CN101493397B CN200910037448XA CN200910037448A CN101493397B CN 101493397 B CN101493397 B CN 101493397B CN 200910037448X A CN200910037448X A CN 200910037448XA CN 200910037448 A CN200910037448 A CN 200910037448A CN 101493397 B CN101493397 B CN 101493397B
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- 238000000691 measurement method Methods 0.000 title abstract 2
- 239000000523 sample Substances 0.000 claims abstract description 137
- 238000000034 method Methods 0.000 claims description 15
- 238000005259 measurement Methods 0.000 claims description 10
- 239000013068 control sample Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 2
- 238000012876 topography Methods 0.000 description 9
- 239000010931 gold Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000003384 imaging method Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 3
- 238000004667 electrostatic force microscopy Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 230000004936 stimulating effect Effects 0.000 description 2
- 206010021703 Indifference Diseases 0.000 description 1
- 238000004630 atomic force microscopy Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
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Abstract
The invention provides an electrostatic microscope and a measurement method. The electrostatic microscope consists of a scan head, a low frequency voltage signal generator, a high frequency voltage signal generator, a low frequency vibration signal detector, a high frequency vibration signal detector and a controller; and the scan head comprises a probe, a probe location inductor, a piezoelectric vibration exciter and a piezoelectric scanner. Based on an existing electrostatic force microscope, a higher order eigenvibration mode of the probe is adopted to measure electrostatic force. As interaction of the probe and the sample is different in different vibration modes, the corresponding performance is different in aspects such as resolution, sensitivity, stability and the like. The electrostatic microscope can help significantly improve spatial resolution of the electrostatic force microscope in atmospheric environment.
Description
Technical field
The invention belongs to the electrostatic force microscope field, particularly relate to a kind of electrostatic force microscope and measuring method thereof.
Technical background
(Electrostatic force microscopy, (it can measure two electrostatic interaction power and Two dimensional Distribution thereof between the object to electrostatic force microscope for Atomic force microscopy, technology AFM) EFM) to be based on atomic force microscope.Electrostatic force microscope obtains the electric charge of sample surfaces or the local distributed image of electromotive force by the kinetic measurement to electrostatic force, has become the important characterization method of material microstructure and character.
Electrostatic force microscope need obtain the surface topography image of sample by atomic force microscope.Electrostatic force microscope and atomic force microscope adopt the micro-cantilever probe to come ergometry.Under the atmospheric environment, electrostatic force microscope and atomic force microscope need excite the eigenvibration pattern of probe with raising sensitivity, and " amplitude modulation(PAM) " mode of employing measuring probe Oscillation Amplitude.Electrostatic force microscope resolution is higher under vacuum environment, but for sample certain requirement is arranged, and for example can not be used for measuring the samples such as device in biomolecule, the work.Electrostatic force microscope under the atmospheric environment does not have these restrictions, but the spatial resolution that present method is reached is relatively low, the highest 100-200 nanometer that is about.
The micro-cantilever probe has multiple eigenvibration pattern, as for the first time, for the second time, vibration mode for the third time etc., its eigenvibration frequency uprises successively.Existing electrostatic force microscope has only utilized the eigenvibration pattern first time of micro-cantilever probe, do not utilize other than the high order vibration mode, cause relatively limiting in the use.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of utilize the micro-cantilever probe come the electrostatic force microscope of measurement of electrostatic power than the high order vibration mode.
Another object of the present invention is to provide the measuring method of this electrostatic microscope.
In order to realize goal of the invention one, the technical scheme of employing is as follows:
A kind of electrostatic force microscope, be made up of scanner head, low-frequency voltage signal generator, high-frequency voltage signal generator, low-frequency vibration signal detecting device, high-frequency vibration signal detecting device, controller, described scanner head comprises conduction micro-cantilever probe, probe location inductor, piezoelectric vibration exciter, piezoelectric scanner; Described low-frequency voltage signal generator is connected with piezoelectric vibration exciter and provides voltage signal to excite the probe vibration, described high-frequency voltage signal generator is connected with probe and provides voltage signal to it, described probe location inductor is connected with the high-frequency vibration signal detecting device with the low-frequency vibration signal detecting device respectively, to transmit the vibration information of its probe of sensing, described low-frequency vibration signal detecting device is connected with controller respectively with the high-frequency vibration signal detecting device, and described controller is connected and controls by output voltage signal the running of piezoelectric scanner with piezoelectric scanner.
In the technique scheme, described high-frequency voltage signal generator is connected with measuring samples on being positioned at piezoelectric scanner with probe respectively and provides voltage signal to them.
The voltage signal that described high-frequency voltage signal generator produces is an AC signal, or direct current signal adds AC signal.
Described probe is provided with vibration frequency multiple vibration mode from low to high, and minimum its voltage signal of vibration mode of frequency provides by the low-frequency voltage signal generator, and the voltage signal of the vibration mode of other frequency is provided by the high-frequency voltage signal generator.
Measuring principle of the present invention is as follows:
When probe and sample room had applied direct current with the voltage signal that exchanges, its electrostatic force can be expressed as:
D is probe-sample interval in the following formula (1), and C ' is the gradient that probe and sample room equivalent capacity are adjusted the distance, and Δ φ is the electric potential difference between probe when not applying the voltage signal of direct current and interchange and the sample, U
DcThe expression d. c. voltage signal, U
AcBe the amplitude of sinusoidal ac signal, f is its frequency, and t is the time.
The component of electrostatic force on frequency f is:
F
f(D)＝-C′[(Δφ-U
dc)U
acSin(2πf·t)] (2)
If the d. c. voltage signal U that applies at probe-sample room
DcBe 0, the amplitude F of detected radio-frequency signal then
f(D) be directly proportional with the electric potential difference of probe-sample room, therefore the image that obtains has reflected that the surface potential of sample distributes.If the d. c. voltage signal U that applies at probe-sample room
Dc, the electric potential difference Δ φ that this DC voltage is just equaled between probe and the sample by the 6-controller also uses this voltage imaging simultaneously, then can obtain the measured value and the distribution thereof of the surface potential of sample.
Described probe is conducting electricity near the needle point of measuring samples one side, according to formula (1), and square being directly proportional of electrostatic force and probe and the sample surface electrical potential difference between the two.For nonconducting probe tip, its surface potential is determined by the static charge of piling up, thereby is difficult to control.For the ease of measuring, must make the value of surface potential for determining of probe, otherwise the result who measures there is not physical significance.In addition, for nonconducting probe tip, high frequency excitation voltage signal used during measurement also can't apply up, thereby can't excite the vibration of probe.Therefore, in electrostatic force was measured, probe tip must conduct electricity.
In order to realize goal of the invention two, the technical scheme of employing is as follows:
A kind of measuring method of electrostatic force microscope comprises the steps:
1), by scanner head, low-frequency voltage signal generator, low-frequency vibration signal detecting device, controller coordinate running, by the shape appearance figure of low frequency voltage signal measuring samples;
2) by scanner head, high-frequency voltage signal generator, high-frequency vibration signal detecting device, controller coordinate running, the shape appearance figure that obtains according to step 1) by the high-frequency voltage signal further measures the electrostatic force image of sample.
In the technique scheme, described step 1) is specific as follows:
Sample is fixed on the piezoelectric scanner, piezoelectric scanner drives sample at X under the voltage signal effect of controller output, Y, the Z three-dimensional space position changes, thereby the relative position of control sample and probe tip, produce low-frequency voltage signal by the low-frequency voltage signal generator, and be applied on the piezoelectric vibration exciter, thereby excite the eigenvibration pattern first time of probe, the probe location inductor is sensed this vibration and it is sent to the low-frequency vibration signal detecting device, measure its amplitude and phase signal, obtain shape appearance figure on sample thereby utilize this signal controlling piezoelectric scanner that probe is scanned by controller at last.
Described step 2) specific as follows:
Produce high-frequency voltage signal by the high-frequency voltage signal generator, be applied on the probe or on the sample (, or be applied on probe and the sample (this sentence of red word removes) simultaneously), to excite the eigenvibration pattern of probe than high order, the probe location inductor is sensed this vibration and it is sent on the high-frequency vibration signal detecting device, measure its amplitude and phase signal, utilize this signal to draw the electrostatic force distribution two dimensional image of sample by controller at last.
Described step 2) can send the voltage signal of a plurality of different frequencies by the high-frequency voltage signal generator simultaneously, thereby excite a plurality of eigenvibration patterns of probe simultaneously, and the high-frequency vibration signal detecting device also detects a plurality of corresponding vibration signals simultaneously, and finally is controlled to picture by controller.
Described step 2) voltage signal that high-frequency voltage signal generator (3) produces is an AC signal, or direct current signal adds AC signal.
Described step 2) probe when carrying out the electrostatic force image measurement is lifted certain height with respect to sample and makes probe and sample be in discontiguous state, keeps that probe-sample interval is constant to be convenient to scanning and to obtain long-range electrostatic force image.
The present invention is on existing electrostatic force microscope basis, and that utilizes probe comes measurement of electrostatic power than the high order vibration mode.Because in the different vibration modes, the interaction of probe and sample is different, its corresponding performance also can there are differences, as at aspects such as resolution, sensitivity and stability.The present invention can significantly improve the spatial resolution of the electrostatic force microscope under the atmospheric environment.
Probe and the residing environment of sample are atmospheric environment, special atmosphere environment or liquid environment during operate as normal of the present invention.Overcome existing electrostatic force microscope because the scanning of its pattern adopts is " frequency modulation (PFM) ", so can not be used for the defective that atmospheric environment can only be worked under vacuum, and invention is because pattern scanning adopts is " amplitude modulation(PAM) ", promptly, can under atmospheric environment, accurately measure the result by measuring its amplitude and phase signal.
Description of drawings
Fig. 1 is an electrostatic microscope structural representation of the present invention, wherein 1 is scanner head, and 1-1 is conduction micro-cantilever probe, and 1-2 is the probe location inductor, 1-3 is a piezoelectric vibration exciter, 1-4 is a measuring samples, and 1-5 is a piezoelectric scanner, and 2 is the low-frequency voltage signal generator, 3 is the high-frequency voltage signal generator, 4 is the low-frequency vibration signal detecting device, and 5 is the high-frequency vibration signal detecting device, and 6 is controller;
Fig. 2 is the image of the gold grain that is dispersed in silicon face that adopts measuring method provided by the invention and obtain simultaneously, and wherein (A) is the surface topography image, (B) is the electrostatic force image.
Embodiment
The present invention is described further below in conjunction with accompanying drawing.
Structural representation of the present invention as shown in Figure 1, the present invention does not influence the original measurement function of quiet atomic force microscope.Before scanning electrostatic force image, need to use earlier the surface topography of afm scan sample.Atomic force microscope adopts progressive scan mode to obtain shape appearance figure.Atomic force microscope is operated in " Intermittent Contact " pattern of conduction micro-cantilever probe 1-1 and sample 1-4.Sample 1-4 is fixed on the piezoelectric scanner 1-5, and piezoelectric scanner 1-5 drives sample 1-4 under the voltage signal effect of controller 6 outputs changes at X, Y, Z three-dimensional space position, thus the relative position of control sample 1-4 and probe 1-1 needle point.Pattern scanning utilizes the eigenvibration pattern first time (its eigenfrequency frequency for the high order vibration mode is lower) of probe 1-1.The ac voltage signal identical or approaching with first eigenfrequency produced by low-frequency voltage signal generator 2, is applied on the piezoelectric vibration exciter 1-3 that closely links to each other with probe 1-1, excites probe 1-1 to vibrate on the eigenvibration pattern in the first time thereby make.Probe location inductor 1-2 senses this vibration and it is sent to low-frequency vibration signal detecting device 4, measures its amplitude and phase signal.Thereby controller 6 utilizes this signal controlling piezoelectric scanner 1-5 that probe 1-1 is scanned on sample 1-4 and obtains sample topography figure.
Electrostatic force microscope adopts " lifting pattern ".So-called " lifting pattern " is that a kind of every capable image all scans twice imaging mode: first pass obtains surface topography with the said method of atomic force microscope by measuring interatomic force earlier, second time scanning the time is then lifted certain height with probe 1-1, and the information that rises and falls according to the sample topography that obtains before keeps the constant and scanning of probe-sample interval to obtain long-range electrostatic force image.
When carrying out electrostatic force image scanning, utilized higher intrinsic vibration mode (its eigenfrequency frequency for first time vibration mode is higher) of conduction micro-cantilever probe 1-1.The ac voltage signal identical or approaching with its eigenfrequency produced by high-frequency voltage signal generator 3, be applied on the probe 1-1, and the voltage that is applied on the sample 1-4 is zero.The voltage signal that high-frequency voltage signal generator 3 produces can also include DC component except AC signal, its direct current and AC signal all are applied on the probe 1-1.Because the electrostatic force between probe 1-1 and sample 1-4 interacts, can excite the vibration of probe 1-1 on higher intrinsic vibration mode.Probe location inductor 1-2 senses this vibration and it is sent to high-frequency vibration signal detecting device 5, measures its amplitude and phase signal.Controller 6 utilizes this signal to draw the electrostatic force distribution two dimensional image of sample.
When carrying out electrostatic force image scanning, can excite a plurality of eigenvibration patterns of probe simultaneously.These vibration modes can be high orders for the second time or more.At this moment, high-frequency voltage signal generator 3 produces a plurality of excitation signals simultaneously, and high-frequency vibration signal detecting device 5 also detects a plurality of corresponding vibration signals and simultaneously by controller 6 imagings.
When electrostatic force image scanning or under the state of lifting, the vibration mode first time that was used for topography measurement originally can be excited simultaneously by original mode.The amplitude of this vibration or phase place can be noted and imaging simultaneously.
The concrete measuring method of the present invention is as follows:
(1) determines eigenfrequency.Excite the vibration mode of probe 1-1, as for the first time, for the second time, eigenvibration pattern for the third time etc., obtain the eigenfrequency of each time vibration mode.Select first eigenfrequency or near the frequency it stimulating frequency, the stimulating frequency of selecting one or more higher eigenfrequencies to measure as electrostatic force as pattern scanning.
(2) two dimensional image scanning.The scanning earlier of every provisional capital obtains the pattern curve of sample surfaces, again probe 1-1 is lifted certain height, to be used for electrostatic force measurement higher-frequency voltage signal applies up, repeat the change curve that this line scanning obtains electrostatic force or surface potential then, line by line scan at last and obtain several entire image simultaneously.
(3) electrostatic force spectrometry.Select different measurement points on shape appearance figure or static are tried hard to, 1-1 lifts certain height with probe, measures electrostatic force on the high order eigenfrequency with the relation curve of direct current that is applied or ac voltage signal, or with the relation curve of probe raising height.
Fig. 2 has provided sample topography figure and the surface potential figure that utilizes said apparatus to record.Used probe is a rectangle silicon micro-cantilever probe, its for the first time, for the second time and for the third time eigenfrequency be respectively: 23.096kHz, 119.565kHz and 146.711KHz.Specimen in use is for being dispersed in gold (Au) particle on silicon (Si) surface.First eigenfrequency is adopted in shape appearance figure scanning, and the 3rd eigenfrequency is then adopted in electrostatic force image scanning, and raising height is 30nm.Adding DC voltage between sample and the probe is 0, and the amplitude of eigenfrequency voltage signal is 1V for the third time, puts on the probe.Sweep limit is 1 μ m * 1 μ m, and sweep velocity is 0.2Hz.
From the result of Fig. 2, this method simultaneously surface topography map (A) of measuring samples and static is tried hard to (B).On the shape appearance figure, gold grain and by crystallization silicon grain and indifference.Then shown the details different on the electrostatic force image with shape appearance figure.Several less dark spaces have appearred in the lower left corner in this electrostatic force image, and several bigger dark spaces have appearred in the centre and the lower right corner, and these features do not occur in shape appearance figure.Because the surface potential of gold grain and silicon grain there are differences, and can cause the variation of electrostatic force, so these characteristics of image are caused by electrostatic force.These dark spaces are likely gold grain institute corresponding region.Size according to these zones judges that the spatial resolution of the electrostatic force image that this method obtains has reached 30 nanometers at least.
Claims (4)
1. electrostatic force microscope, it is characterized in that being made up of scanner head (1), low-frequency voltage signal generator (2), high-frequency voltage signal generator (3), low-frequency vibration signal detecting device (4), high-frequency vibration signal detecting device (5), controller (6), described scanner head (1) comprises conduction micro-cantilever probe (1-1), probe location inductor (1-2), piezoelectric vibration exciter (1-3), piezoelectric scanner (1-5); Described low-frequency voltage signal generator (2) is connected with piezoelectric vibration exciter (1-3) and provides voltage signal to excite probe (1-1) vibration, described high-frequency voltage signal generator (3) is connected with measuring samples (1-4) on being positioned at piezoelectric scanner (1-5) with probe (1-1) respectively and provides voltage signal to them, high-frequency voltage signal generator (3) is applied between probe (1-1) and the measuring samples (1-4) voltage signal to excite probe (1-1) vibration, the voltage signal that high-frequency voltage signal generator (3) produces is an AC signal, or direct current signal adds AC signal, described probe location inductor (1-2) is connected with high-frequency vibration signal detecting device (5) with low-frequency vibration signal detecting device (4) respectively, to transmit the vibration information of its probe of sensing (1-1), described low-frequency vibration signal detecting device (4) is connected with controller (6) respectively with high-frequency vibration signal detecting device (5), described controller (6) is connected and controls by output voltage signal the running of piezoelectric scanner (1-5) with piezoelectric scanner (1-5), described probe (1-1) is provided with vibration frequency multiple eigenvibration pattern from low to high, and its voltage signal of eigenvibration pattern that frequency is minimum is provided by low-frequency voltage signal generator (2), and the voltage signal of the eigenvibration pattern of other frequency is provided by high-frequency voltage signal generator (3), described probe (1-1) can conduct electricity at the needle point near measuring samples (1-4) side, thereby so that the surface potential of control probe tip produces measurable electrostatic force.
2. a measuring method that adopts the described electrostatic force microscope of claim 1 is characterized in that comprising the steps:
1), by scanner head (1), low-frequency voltage signal generator (2), low-frequency vibration signal detecting device (4), controller (6) coordinate operation, shape appearance figure by low frequency voltage signal measuring samples (1-4), sample (1-4) is fixed on the piezoelectric scanner (1-5), piezoelectric scanner (1-5) drives sample (1-4) at X under the voltage signal effect of controller (6) output, Y, the Z three-dimensional space position changes, thereby the relative position of control sample and probe tip, produce low-frequency voltage signal by low-frequency voltage signal generator (2), and be applied on the piezoelectric vibration exciter (1-3), thereby excite the eigenvibration pattern first time of probe (1-1), probe location inductor (1-2) is sensed this vibration and it is sent to low-frequency vibration signal detecting device (4), measure its amplitude and phase signal, at last by controller (6) utilize this signal controlling piezoelectric scanner (1-5) make probe (1-1) at sample (1-4) thus going up scanning obtains shape appearance figure;
2) by scanner head (1), high-frequency voltage signal generator (3), high-frequency vibration signal detecting device (5), controller (6) coordinate operation, the shape appearance figure that obtains according to step 1) by the high-frequency voltage signal further measures the electrostatic force image of measuring samples (1-4), specifically produce high-frequency voltage signal by high-frequency voltage signal generator (3), be applied to that probe (1-1) is gone up or sample (1-4) on, excite the eigenvibration pattern of probe (1-1) than high order, probe location inductor (1-2) is sensed this vibration and it is sent on the high-frequency vibration signal detecting device (5), measure its amplitude and phase signal, utilize this signal to draw the electrostatic force distribution two dimensional image of sample (1-4) by controller (6) at last.
3. the measuring method of electrostatic force microscope according to claim 2, it is characterized in that described step 2) can send the voltage signal of a plurality of different frequencies by high-frequency voltage signal generator (3) simultaneously, thereby excite a plurality of eigenvibration patterns of probe (1-1), and high-frequency vibration signal detecting device (5) also detects a plurality of corresponding vibration signals simultaneously, and finally is controlled to picture by controller (6).
4. the measuring method of electrostatic force microscope according to claim 2 is characterized in that described step 2) probe when carrying out the electrostatic force image measurement (1-1) is lifted certain height with respect to sample makes probe and sample be in discontiguous state.
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| CN102507986A (en) * | 2011-10-13 | 2012-06-20 | 中山大学 | Intermittent contact type measuring method for electrostatic force microscopy |
| CN102749480A (en) * | 2012-07-10 | 2012-10-24 | 上海交通大学 | Method for improving vibration amplitude of electrostatic force driven atomic force microscope probe cantilever |
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| CN102749480A (en) * | 2012-07-10 | 2012-10-24 | 上海交通大学 | Method for improving vibration amplitude of electrostatic force driven atomic force microscope probe cantilever |
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