CN112557702A

CN112557702A - Chromatography detection device and method based on atomic force microscope and ion beam

Info

Publication number: CN112557702A
Application number: CN202011321337.4A
Authority: CN
Inventors: 陈庚亮; 吴森
Original assignee: Shenzhen Mingrui Instrument Co ltd
Current assignee: Shenzhen Mingrui Instrument Co ltd
Priority date: 2020-11-23
Filing date: 2020-11-23
Publication date: 2021-03-26

Abstract

The invention provides a chromatography detection device and a chromatography detection method based on an atomic force microscope and an ion beam, wherein the chromatography detection device comprises an equipment shell, the atomic force microscope, the ion beam device, a control device and a sample bearing device, wherein the equipment shell is used for forming a vacuum environment inside; the sample bearing device and the atomic force microscope are both arranged in the vacuum environment, and the ion beam device is fixedly arranged on the equipment shell; the atomic force microscope comprises a probe and a probe driving structure for driving the probe to move; the sample bearing device comprises a sample table for bearing a sample, and a sample table driving structure for driving the sample table and the sample thereon to move; and the control device controls the probe driving structure and the sample stage driving structure through signals respectively. The chromatography detection is realized by the in-situ alternate use or the simultaneous use of an ion beam device and an atomic force microscope.

Description

Chromatography detection device and method based on atomic force microscope and ion beam

Technical Field

The invention relates to the field of object detection, in particular to a chromatography detection device and method based on an atomic force microscope and an ion beam.

Background

When the object is subjected to nanoscale detection, the three-dimensional shape of the object can be detected in an atomic force probe mode, and the shape of the object can also be detected through a sensor, so that corresponding shape information and physical properties are obtained. However, the existing detection method can only detect the surface shape of the object, and cannot obtain the internal information (such as the internal shape and physical properties) of the object.

Therefore, in the related art, the diamond knife may be used to strip the object to be measured layer by layer, and then the object to be measured is sent to the image acquisition device after each stripping, and the image acquisition device may acquire the image of the current surface to be measured, and further, based on the acquired image, the related information of the object may be analyzed and determined.

However, the information covered by the image is limited, and it is difficult to fully reflect the actual physical properties of the surface to be measured (for example, the image is difficult to effectively reflect the fluctuation of the surface to be measured).

Disclosure of Invention

The invention provides a chromatography detection device and method based on an atomic force microscope and an ion beam, and aims to solve the problems that detected information is single and cannot meet requirements.

According to a first aspect of the present invention, there is provided a chromatography detection apparatus based on an atomic force microscope and an ion beam, comprising an equipment housing for forming a vacuum environment inside, the atomic force microscope, an ion beam apparatus, a control apparatus, and a sample carrying apparatus; the sample bearing device and the atomic force microscope are both arranged in the vacuum environment, and the ion beam device is fixedly arranged on the equipment shell;

the atomic force microscope comprises a probe and a probe driving structure for driving the probe to move; the sample bearing device comprises a sample table for bearing a sample, and a sample table driving structure for driving the sample table and the sample thereon to move; the control device controls the probe driving structure and the sample stage driving structure through signals respectively;

the control device is used for:

controlling the sample to be at a stripping position through the sample stage driving structure, wherein the stripping position is matched with an ion beam incidence direction of the ion beam device;

controlling the ion beam device to emit ion beams to the sample at the stripping position so as to strip one layer of surface of the sample to obtain the current surface to be measured;

controlling the probe and the current surface to be measured to be in an interaction position through the sample stage driving structure and/or the probe driving structure at the same time of stripping or after stripping, controlling the probe to perform scanning motion relative to the sample through the probe driving structure, and performing physical property measurement on the current surface to be measured by using the probe; wherein, the physical signal change of the scanning movement of the plurality of measuring points forms a physical map of the current surface to be measured, and the center of the ion beam and the needle point of the probe act on the same position of the sample;

the above procedure was repeated to peel off the sample surface again, and the surface physical property measurement and scanning were repeated using an atomic force microscope.

Optionally, the chromatography detection apparatus further includes an optical device, the optical device is mounted on the apparatus housing, the optical device faces to the region where the sample stage belongs, and the sample is located between the sample stage and the optical device; the interaction location matches a focal plane of the optical device;

the optical device is used for:

collecting a real-time image within the coverage range of the real-time image and sending the real-time image to the control device;

the control device is further configured to:

when the probe makes the scanning movement, determining probe position information of the probe tip relative to the sample at different time according to the real-time image;

when the control device uses the probe to measure the physical property of the current surface to be measured, the control device is specifically configured to:

and determining the physical map of the current surface to be measured according to the probe position information and the physical signals at different times.

Optionally, the stripping position is matched with the intersection of the ion beam incidence direction and the focal plane of the optical device;

when the control device controls the sample to be in the peeling position, the control device is specifically configured to: controlling the sample to be at the stripping position according to the corresponding real-time image;

the control device is used for controlling the probe and the current surface to be detected to be in the interaction position according to the corresponding real-time image when controlling the probe and the current surface to be detected to be in the interaction position.

Optionally, the optical device is further configured to introduce first auxiliary light, and guide the first auxiliary light to the current surface to be measured, so as to form a first light spot on the current surface to be measured;

the first auxiliary light is configured to enable:

in the current image, the probe tip section of the probe shows spectral information which is different from spectral information of other areas in the area range covered by the first light spot, and the size range of the probe tip section is smaller than 20 nm.

Optionally, the optical device is further configured to introduce second auxiliary light, and guide the second auxiliary light to the current surface to be measured, so as to form a second light spot on the current surface to be measured;

the second auxiliary light is configured to enable:

and in the current surface to be measured, the second light spot is deformed within the covered area range.

Optionally, the chromatography detection apparatus further comprises an electrical measurement device, the electrical measurement device electrically connects the probe and the sample to form a loop between the probe and the sample; the electrical measuring device is also electrically connected with the control device to acquire the probe position information at different times;

the electrical measurement device is configured to:

acquiring electrical parameters of the loop at different times;

determining the surface electrical information of the current surface to be detected according to the electrical parameters at different times and the probe position information at different times, wherein the surface electrical information represents the change of the electrical parameters when the needle point of the probe reaches different positions relative to the sample;

and after the sample is stripped for N times and the corresponding surface electrical information is acquired after each stripping, integrating N groups of surface electrical information corresponding to the N times of stripping.

Optionally, the chromatography detection apparatus further includes a laser assembly, the laser assembly includes a laser and a detector, and the control device is electrically connected to the laser and the detector respectively; the probe comprises a cantilever and a contact part, and the cantilever is connected between the contact part and the probe driving structure;

the position of the laser and the detector relative to the device housing is fixed, the position of the interaction location, the position of the laser and the detector match such that: when the probe makes the scanning movement, the laser of the laser can be incident to a cantilever of the probe;

the control device is further configured to:

when the probe makes the scanning movement, controlling the laser to emit laser to the cantilever and acquiring a signal of return light received by the detector;

the physical signal is determined from the signal of the corresponding return light.

Optionally, the laser and the detector are directly or indirectly mounted on the device housing, a heat conduction structure is arranged between the laser and the device housing, and a heat conduction structure is also arranged between the detector and the device housing.

Optionally, the laser and the detector are mounted on an optical device.

Optionally, the control device is further configured to:

after the stripping of the sample is completed for N times and corresponding physical property maps are obtained, constructing corresponding three-dimensional chromatographic images based on the N physical property maps; wherein N is an integer greater than or equal to 2.

Optionally, the probe comprises a cantilever, a contact part, and a sensing part, and the cantilever is connected between the contact part and the probe driving structure;

the sensing component is used for detecting the deformation and/or deformation stress of the cantilever to obtain a corresponding sensing signal;

the induction component is electrically connected with the control device so as to feed the induction signal back to the control device;

the physical signal is determined from the corresponding sensing signal.

Optionally, the control device is further configured to:

controlling the probe to be in a probe tip cleaning position through the probe driving structure; wherein the tip cleaning position matches the ion beam incident direction;

and controlling the ion beam device to inject an ion beam to the probe at the point cleaning position so as to clean the object to be cleaned on the probe.

Optionally, the chromatography detection apparatus further comprises a probe changing table, the probe driving structure is provided with a probe installation part, the probe is detachably installed on the probe installation part through a probe holder, and the probe changing table is provided with at least two probe containing positions;

if the at least two probe accommodating positions comprise an empty first accommodating position and a second accommodating position which already accommodates the standby probe and the probe holder thereof, then:

the control device is further configured to:

controlling the probe and the probe clamp thereof to enter the first containing position through the probe driving structure;

controlling the probe mounting part to be separated from the corresponding probe clamp so that the probe and the probe clamp thereof can be left at the first accommodating position;

the probe mounting part is controlled to move to the outer side of the second accommodating position through the probe driving structure;

controlling the probe mounting section to interface with a probe holder of the back up probe to enable the back up probe to be a currently used probe.

Optionally, after the control device controls the sample to be in the peeling position, the control device is further configured to:

and controlling the sample stage and the sample to deflect towards the ion beam device through the sample stage driving structure.

Optionally, the probe driving structure includes a probe driving assembly and a scanner, the probe is directly or indirectly mounted on the scanner, and the scanner is mounted on the probe driving assembly;

the probe driving component is electrically connected with the control device so as to change the positions of the scanner and the probe under the control of the control device;

the scanner is electrically connected with the control device so as to drive the probe to perform the scanning motion under the control of the control device.

Optionally, the initial vacuum degree of the vacuum environment is higher than 1 mPa; the working air pressure controlled by the ion beam is at least 10 times larger than the initial vacuum degree.

According to a second aspect of the present invention, there is provided a chromatography detection method based on an atomic force microscope and an ion beam, which employs a chromatography detection apparatus based on an atomic force microscope and an ion beam, the chromatography detection apparatus includes an equipment housing for forming a vacuum environment inside, an atomic force microscope, an ion beam apparatus, a control apparatus, and a sample carrying apparatus; the sample bearing device and the atomic force microscope are both arranged in the vacuum environment, and the ion beam device is fixedly arranged on the equipment shell;

the chromatography detection method is applied to the control device and comprises the following steps:

repeating the above process, after completing the stripping of the sample for N times and acquiring corresponding N physical property maps, constructing a corresponding three-dimensional chromatographic image based on the physical property maps, wherein N is greater than or equal to 2.

In the chromatography detection device and method based on the atomic force microscope and the ion beam, the probe of the atomic force microscope is controlled to interact with the current surface to be detected, and the probe is controlled to perform scanning motion, so that a physical property map number representing the physical property of the surface to be detected can be obtained. Meanwhile, the invention also adopts the ion beam to realize the stripping of the surface of the object, which is beneficial to realizing the uniform stripping of the surface of the object.

Because the atomic force microscope is usually applied to the atmospheric environment, the invention further contemplates forming a vacuum environment under the condition of using the atomic force microscope and the ion beam, and further realizing the detection of the atomic force microscope and the stripping of the ion beam at the same position in the same vacuum environment, thereby avoiding the pollution of impurities (gas molecules, water vapor and the like) in the atmosphere to the detection and stripping effects, and further effectively improving the stripping effect, the detection effect and the stripping and detection efficiency.

Furthermore, the invention is different from the stripping and detection processes in the atmospheric environment, and aims at the vacuum environment, and controls the probe driving structure and the sample stage driving structure through the control device, thereby realizing the precise control of the ion beam, the probe and the sample stage in the stripping and detection processes and ensuring the accurate implementation of the stripping and detection.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.

FIG. 1 is a first schematic structural diagram of an atomic force microscope and ion beam based tomography apparatus according to an embodiment of the present invention;

FIG. 2 is a schematic structural diagram of a tomography apparatus based on an atomic force microscope and an ion beam according to an embodiment of the present invention;

FIG. 3 is a schematic structural diagram of the chromatographic detection device with the sample stage in the peeling position according to an embodiment of the present invention;

FIG. 4 is a schematic diagram of a chromatographic detection device with a probe in an interaction position with a current surface to be detected according to an embodiment of the present invention;

FIG. 5 is a schematic diagram of a first embodiment of a tomographic detection apparatus employing a laser assembly in accordance with the present invention;

FIG. 6 is a schematic structural diagram of a tomography apparatus employing a laser assembly in an embodiment of the present invention;

FIG. 7 is a schematic view of the structure of the chromatography detection apparatus when the probe is cleaned according to an embodiment of the present invention;

FIG. 8 is a schematic view of the chromatographic detection device with probe replaced according to an embodiment of the present invention;

FIG. 9 is a third schematic structural diagram of an atomic force microscope and ion beam based tomography apparatus according to an embodiment of the present invention;

FIG. 10 is a flow chart illustrating an AFM and ion beam based tomography method according to an embodiment of the present invention.

Description of reference numerals:

1-an ion beam device;

11-an ion source;

12-an accelerator;

13-an electrostatic lens;

14-a diaphragm;

15-ion beam;

2-equipment housing;

21-a housing body;

22-an electrical interface;

23-a viewing window;

24-a housing door panel;

25-an optical interface;

3-a sample carrier;

31-sample stage;

32-a sample stage drive structure;

33-needle changing table;

34-an active vibration isolation table;

4-atomic force microscopy;

41-a probe;

42-a probe drive structure;

421-a probe drive assembly;

422-a scanner;

43-a probe holder;

5-a control device;

6-sample;

7-an optical device;

71-extra-cavity optical structures;

72-an optical window;

73-objective lens;

8-a laser assembly;

81-laser;

82-a detector;

83-thermally conductive structures;

9-an electrical measuring device;

10-vibration isolation platform.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The terms "first," "second," "third," "fourth," and the like in the description and in the claims, as well as in the drawings, if any, are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.

The technical solution of the present invention will be described in detail below with specific examples. The following several specific embodiments may be combined with each other, and details of the same or similar concepts or processes may not be repeated in some embodiments.

Referring to fig. 1, the chromatography detection apparatus based on the afm and the ion beam includes an equipment housing 2 for forming a vacuum environment therein, an afm 4, an ion beam apparatus 1, a control apparatus 5, and a sample holder 3. The sample bearing device 3 and the atomic force microscope 4 are both arranged in the vacuum environment, and the ion beam device 1 is fixedly arranged on the equipment shell 2.

The atomic force microscope includes a probe 41, and a probe driving structure 42 for driving the probe 41 to move.

The probe drive structure 42 may be any structure or combination of structures that can drive the movement of the probe 41, which may include three degrees of freedom of movement, and may also include one or more degrees of freedom of rotation. In the following further alternatives, the probe drive structure 42 may be further configured to the motion requirements of the probe 41, no matter how configured, without departing from the scope of embodiments of the present invention.

The sample bearing device 3 comprises a sample table 31 for bearing the sample 6, and a sample table driving structure 32 for driving the sample table 31 and the sample 6 thereon to move;

the stage driving structure 32 may be any structure or combination of structures capable of driving the stage 31 to move, where the movement may include movement in three degrees of freedom, and may also include rotation in one or more degrees of freedom. In the following further alternatives, the stage driving structure 32 may be further configured according to the motion requirement of the stage 31, and no matter how configured, the present invention is not departing from the scope of the present invention.

In the embodiment of the present invention, the control device 5 controls the probe driving structure 42 and the sample stage driving structure 32 through signals, referring to fig. 1 and fig. 2, the control device 5 may electrically connect the probe driving structure 42 and the sample stage driving structure 32; in turn, the probe driving structure 42 and the stage driving structure 32 can be controlled to perform corresponding movements by corresponding electrical signals.

The optional processing of the control device 5 can be understood as steps of the detection method based on the afm and the ion beam provided by the embodiment of the present invention, please refer to fig. 1 and fig. 10, wherein the control device 5 is configured to implement the following steps:

s101: controlling the sample to be in a stripping position through the sample stage driving structure;

s102: and controlling the ion beam device to emit ion beams to the sample at the stripping position so as to strip one layer of surface of the sample to obtain the current surface to be measured.

Referring to fig. 3, which can be regarded as a structural state when the sample 6 is in the stripping position and is further stripped by the ion beam, it can be seen that the stripping position can be matched with the incident direction of the ion beam 15 of the ion beam apparatus, wherein the matching can be understood as: when the sample 6 is at the peeling position, the ion beam 15 incident by the ion beam apparatus 1 may be incident on the surface of the sample 6.

The control sample 6 is in the peeling position, which may include a case where the control sample 6 is moved to the peeling position, and a case where the control sample 6 is kept in the peeling position without position change.

In one embodiment, if the ion beam apparatus 1 is not located on the upper side of the sample support apparatus 3: the control means 5, after controlling the sample 6 in the peeling position, are further configured to: the sample stage 31 and the sample 6 are controlled to deflect towards the ion beam device 1 by the sample stage driving structure 32. Further, the sample 6 can be made to receive the ion beam 15 efficiently and accurately.

The control device 5 is also configured to implement the following steps:

s103: controlling the probe and the current surface to be measured to be in an interaction position through the sample stage driving structure and/or the probe driving structure at the same time of stripping or after stripping, controlling the probe to perform scanning motion relative to the sample through the probe driving structure, and performing physical property measurement on the current surface to be measured by using the probe;

and the change of the physical signals of the plurality of measuring points of the scanning movement forms a physical map of the current surface to be measured, and the center of the ion beam and the needle point of the probe act on the same position of the sample. .

The same positions therein are to be understood as: the same positions in nanometer scale may specifically be, for example: when the probe is not in scanning motion, the center of the ion beam can be exactly aligned with the position of the probe (for example, several nanometers) in the nanometer space.

The interaction may be, for example, a repulsive force (contact or non-contact) generated between the probe tip atoms and the sample surface atoms, and in one example, the tip of the probe 41 may be made to fluctuate with the surface to be measured by controlling the force to be constant during scanning. If the sample 6 is arranged horizontally or is understood to be arranged laterally, then: the undulation is to be understood as vertical or vertical.

The physical property map may represent any information related to the physical properties of the surface.

Wherein, controlling device passes through the control of signal to probe drive structure, sample platform drive structure, can understand as: the same (or a certain range of) force between the probe and the sample surface is controlled and in this case scanned based on a corresponding feedback loop, which may for example be acquired by measurement of the cantilever (e.g. induced signals from detection of the cantilever deformation stress as referred to hereinafter), and based on the result of this acquisition may be controlled such that the force is maintained. On the basis, physical property measurement and physical property diagram construction can be realized.

For example, the control device acquires a sensing signal (also understood as a force deformation signal) of the deformation stress of the probe in real time, performs processing such as filtering on the signal, and controls signals such as vibration excitation of the probe, three-dimensional displacement driving of the scanner, bias voltage between the probe tip and the sample, and illumination according to the signal and a specific scanning strategy, so as to obtain physical properties (such as surface morphology and physical and chemical property information) of the sample.

Further, a physical property map can be obtained based on the physical signal when the probe is scanned to a different position.

Wherein the measured physical properties may be, for example, three-dimensional morphology, roughness, adhesion, elastic modulus, hardness, conductivity, work function, piezoelectric response, charge distribution, magnetic domain distribution, thermal distribution, and the like.

The physical signal may be a signal itself directly obtained by detecting the probe (for example, a signal of an induced signal and a signal of return light described later), or may be arbitrary information obtained based on the signal.

Further, where the number of layers stripped (also understood as the number of times of stripping) N may be greater than or equal to 2, the thickness of each layer may be, for example, 0.1 nm to 1 μm, where the ion beam employed may be focused or unfocused (e.g., defocused), the energy of the ion beam may be, for example, 100eV to 10keV, the type of ion beam may be, for example, Ar, the angle of incidence of the ion beam may be, for example, 3 to 30 degrees, and the degree of vacuum of the vacuum environment formed may be, for example, 1E to 4 torr-1E-11.

Wherein the initial vacuum degree of the vacuum environment can be higher than 1 mPa; the working air pressure controlled by the ion beam is at least 10 times larger than the initial vacuum degree.

As mentioned above, in step S103, in some embodiments, the physical property measurement of the atomic force microscope can be realized while peeling, that is: at the same time, physical properties were measured by an atomic force microscope as well as by ion beam stripping. In another embodiment, the physical property measurement of the surface of the layer may be performed by an atomic force microscope after each layer is peeled by an ion beam microscope. In any way, without departing from the scope of the embodiments of the present invention.

If the ion beam is used for stripping and the atomic force microscope is used for measuring the physical property at the same time, the measured physical property can be ensured to be more timely, and the influence of surface adsorbed atoms and molecules on the surface physical property after stripping is avoided, so that the interference of the influence on the measurement result is avoided. Meanwhile, in the specific implementation process of the scheme, in order to avoid the interference of residues generated by stripping, the ion beam can be stripped at a smaller incident angle, a focused ion beam can be used for stripping, and a corresponding collecting device can be configured for collecting the residues. Further, after step S103 (or after steps S101-S103 are understood to be repeatedly performed), the method may further include:

s104: whether the stripping of the sample is finished for N times or not is judged, and a corresponding physical property diagram is obtained after each stripping; wherein N is an integer greater than or equal to 2.

If the determination result in step S104 is yes, step S105 may be implemented: based on the N physical property maps, a corresponding three-dimensional tomographic image is constructed, and further, a detection result for the sample can be obtained.

In the specific implementation of step S105, taking two physical property diagrams as an example, the three-dimensional tomographic images of the two physical property diagrams can be constructed using the spatial coherence of the first physical property diagram and the second physical property diagram, and further, the three-dimensional tomographic images of at least two physical property diagrams can be constructed based on the spatial coherence of the N physical property diagrams for the N physical property diagrams.

In some embodiments, step S104 and step S105 may be implemented by the control device 5, and in other embodiments, step S104 and step S105 may be implemented by other devices.

Therefore, in the above scheme, by controlling the probe of the atomic force microscope to interact with the current surface to be detected and controlling the probe to perform scanning motion, the physical property map representing the physical property of the surface to be detected can be obtained. Meanwhile, the embodiment of the invention also adopts the ion beam to realize the stripping of the surface of the object, which is beneficial to realizing the uniform stripping of the surface of the object.

Wherein, the chromatography detection is realized by the in-situ alternate use or the simultaneous use of an ion beam device and an atomic force microscope.

Because the atomic force microscope is generally applied to an atmospheric environment, in the embodiment of the invention, under the condition of using the atomic force microscope and the ion beam, a vacuum environment is further formed, so that the detection of the atomic force microscope and the stripping of the ion beam are realized at the same position in the same vacuum environment, the pollution of impurities (gas molecules, water vapor and the like) in the atmosphere on the detection and stripping effects is avoided, and the stripping effect, the detection effect and the stripping and detection efficiency are effectively improved.

Further, different from the stripping and detection processes in the atmospheric environment, the embodiment of the invention aims at the vacuum environment, and controls the probe driving structure and the sample stage driving structure through the control device, thereby realizing the precise control of the ion beam, the probe and the sample stage in the stripping and detection processes and ensuring the accurate implementation of the stripping and detection.

In order to integrate the physical signals when the probe scans to different positions, it is required to know which position the acquired physical signals correspond to. Therefore, in one embodiment, referring to fig. 2 to 8, the tomography apparatus further includes an optical device 7, the optical device 7 is mounted on the apparatus housing 2, the optical device 7 faces the area to which the sample stage 31 belongs, and the sample 6 is located between the sample stage 31 and the optical device 7, in an example, a coverage area of the optical device 7 for acquiring an image may cover various moving positions of the sample stage 31 and the sample 6, meanwhile, a focusing distance of the optical device 7 may be fixed, and further, in an actual use process, an image to be acquired may specifically refer to an image in a focal plane.

Wherein the interaction position matches the focal plane of the optical device 7; furthermore, the optical device 7 can accurately and clearly observe the actual position of the probe scanning movement during scanning because the probe is located in the focal plane.

The optical device 7 is configured to:

and acquiring a real-time image within the coverage range of the real-time image, and sending the real-time image to the control device.

Correspondingly, the control device 5 is further configured to:

and when the probe makes the scanning movement, determining probe position information of the probe tip relative to the sample at different time according to the real-time image.

Further, in the detection method, after step S104, the above process may also be implemented.

When the control device uses the probe to measure the physical property of the current surface to be measured, the control device is specifically configured to: (that is, the partial process of step S103 may specifically include:.)

The probe position information can be understood as any information capable of representing the position of the probe tip. For example, the position of the probe tip in the image can be identified in a real-time image, and as can be seen, the accuracy of the identification depends on the resolution of the optical device, and the higher the resolution, the more accurate the identified position of the probe tip can be made.

In one embodiment, based on the optical device 7, a basis is provided for the stripping of the sample 6, and further, the stripping position is matched with the intersection of the ion beam incident direction and the focal plane of the optical device;

the control device 5 is specifically configured to (i.e., the step S101 specifically includes): and controlling the sample to be at the stripping position according to the corresponding real-time image.

The control device 5 is specifically configured to, when controlling the probe and the current surface to be measured to be in the interaction position (that is, part of the process of step S103 specifically includes: and controlling the probe and the current surface to be detected to be in the interaction position according to the corresponding real-time image.

For example, the positions of the sample, the probe, and the like may be identified based on the real-time image, and the sample 6 and the probe 41 may be brought to the peeling position and the interaction position based on the identified positions.

Taking fig. 3 and 4 as an example, when the sample 6 is in the peeling position, it is already at a position corresponding to the focal plane of the optical device, and then the probe 41 can be mainly controlled to make horizontal and vertical movements, so as to reach the corresponding interaction position, and at this time, the sample 6 may not move.

In addition, for convenience of description, the horizontal direction may be regarded as the motion of the XY plane, the vertical direction may be regarded as the motion of the Z axis, and the XY plane may be regarded as the motion of the X axis and the motion of the Y axis. Correspondingly, the scanning movement referred to in the foregoing can be understood as a wobble about the Z-axis.

Therefore, the sample 6 can be stripped and detected by the probe in situ, and the movement of the sample 6 is prevented from influencing the movement and detection accuracy.

The motion control in step S101 and step S103 may be automatically performed by the control device 5, or may be manually controlled by the control device 5.

Further, in order to identify the position of the probe tip more accurately, the accuracy of the motion control (e.g., the control accuracy of step S101 and step S103) and the accuracy of the position matching during the probe detection (e.g., the more accurate probe position information is matched for the physical signals at each time in step S103) are improved. In one example, the optical device 7 is further configured to introduce a first auxiliary light (the light obliquely incident to the sample shown in fig. 7 may be, for example, the first auxiliary light) and guide the first auxiliary light to the current surface to be measured to form a first light spot on the current surface to be measured;

the first auxiliary light is configured to enable:

In one example, the first auxiliary light may be auxiliary light capable of forming raman light, for example.

The tip section can be understood as a part in a length range of the tip end, and therefore, the identification precision of the optical device can be effectively improved based on the length smaller than 20nm, so that the scanning position of the tip can be accurately determined, a more accurate position can be matched for a physical signal, and the physical map has higher resolution.

In one embodiment, in order to be able to learn the nature of the change of the physical property of the sample, a second auxiliary light may be introduced, and specifically, the optical device 7 is further configured to introduce the second auxiliary light (the light obliquely incident to the sample shown in fig. 7 may be, for example, the second auxiliary light) and guide the second auxiliary light to the current surface-to-be-measured so as to form a second light spot on the current surface-to-be-measured;

the second auxiliary light is configured to enable:

In one example, the second auxiliary light may be, for example, infrared light, and when the infrared light is irradiated, the temperature in the coverage area of the second light spot may change, and accordingly, the area may be deformed, and when the probe scans the area, the corresponding physical signal may indicate the deformation.

It can be seen that when infrared light is used as the second auxiliary light, the change in surface morphology can be known when the temperature of the sample changes.

Referring to fig. 3, in one embodiment, the ion beam apparatus 1 may include: the ion source 11, the accelerator 12, the electrostatic lens 13, and the diaphragm 14, wherein the ion beam 15 emitted from the ion source 11 can be accelerated by the accelerator 12 and then incident on the surface of the sample 6 through the guidance of the electrostatic lens 13 and the diaphragm 14.

The ion beam apparatus 1 according to the embodiment of the present invention is not limited to the above examples, and any ion beam apparatus 1 existing or modified in the art may be applied to the embodiment of the present invention.

Referring to fig. 2 and 3, in one embodiment, the optical device 7 may include an extra-cavity optical structure 71, an optical window 72 and an objective lens 73, and the optical signals of the captured image may enter the extra-cavity optical structure 71 through the objective lens and the optical window 72, so that the optical signals of the captured image form the current image mentioned above.

The optical window 72 may be opened in the device housing 2, the extra-cavity optical structure 71 may be disposed outside the device housing 2 and connected to the device housing 2, and the objective lens 73 may be disposed inside the device housing 2 and connected to the device housing 2.

The extra-cavity optical structure 71 may collect the optical signal and emit the optical signal, including the first auxiliary light, the second auxiliary light, and the illumination light, etc. mentioned above.

Referring to fig. 4, in one embodiment, the probe driving structure 42 may include a probe driving assembly 421 and a scanner 422. The probe 41 is directly or indirectly mounted to the scanner 422, and the scanner 422 is mounted to the probe driving assembly 421; the probe driving assembly 421 is electrically connected to the control device 5 to change the positions of the scanner 422 and the probe 41 under the control of the control device 5; the scanner 422 is electrically connected to the control device 5, so as to drive the probe 41 to perform the scanning motion under the control of the control device 5.

The probe driving assembly 421 can be used to drive the probe to move, for example, to move in at least one of three degrees of freedom, i.e., X-axis, Y-axis, and Z-axis, and further, the probe driving assembly 421 can further realize the rotation around at least one of the X-axis, Y-axis, and Z-axis, and meanwhile, the probe driving assembly 421 without realizing the rotation can also be used in this embodiment.

In a specific example, the probe driving assembly 421 may be driven by a motor, and further, the probe driving assembly 421 may be, for example, a measuring head motor assembly, a driving motor which may have at least one degree of freedom, and a corresponding transmission member, and any scheme in the art which can achieve movement in at least one degree of freedom may be applied to the probe driving assembly according to the embodiment of the present invention. The probe drive assembly 421 may be mounted to the device housing 2.

Control of the scanning motion may be achieved by the scanner 422, which may be a piezo ceramic scanner, for example. Meanwhile, the embodiment of the invention does not exclude the scheme of adopting other forms of scanners.

Specifically, the probes 41 can be fixedly connected to the probe holders 43 (e.g., the probe holders 43 can fixedly hold the probes 41), the probe holders 43 can be mounted on the scanner 422 so as to perform scanning motions under the driving of the scanner 422, and the scanner 422 can be mounted on the probe driving assembly 421 so that the scanner 422, the probe holders 43 mounted on the scanner 422, and the probes 41 can be driven to move together by the probe driving assembly 421.

The sample stage driving structure 32 may, for example, be capable of realizing a movement of at least one degree of freedom among three degrees of freedom of an X axis, a Y axis, and a Z axis, and further, if a deflection needs to be realized, the sample stage driving structure 32 may also further realize a rotational movement around at least one of the X axis, the Y axis, and the Z axis, and meanwhile, the sample stage driving structure 32 that does not realize the rotational movement may also be adopted in this embodiment.

In a specific example, the sample stage driving structure 32 may be driven by a motor, and further, the sample stage driving structure 32 may be, for example, a sample stage motor structure, in which a driving motor with at least one degree of freedom and a corresponding transmission member may be provided, and any scheme that can achieve movement with at least one degree of freedom in the art may be applied to the probe driving assembly according to the embodiment of the present invention. The sample stage drive structure 32 may be mounted directly or indirectly to the apparatus housing 2.

In order to obtain the undulation information of the probe 41, the laser unit 8 may be used as shown in fig. 5 and 6, or a sensing member provided in the probe may be used.

In one embodiment, referring to fig. 5 and fig. 6, the tomography apparatus further includes a laser assembly 8, the laser assembly 8 includes a laser 81 and a detector 82, and the control device 5 is electrically connected to the laser 81 and the detector 82 respectively; the probe 41 comprises a cantilever and a contact portion, the cantilever being connected between the contact portion and the probe actuation structure, in particular connectable between the contact portion and a probe holder 43; the cantilever and the contact part can be integrated or assembled together.

The position of the laser 81 and the detector 82 relative to the device housing 2 is fixed, the position of the interaction position, the position of the laser 81 and the detector 82 matching such that: while the probe 41 performs the scanning movement, the laser light of the laser 81 can be incident on the cantilever of the probe 41.

Correspondingly, the control device 5 is further configured to:

controlling the laser 81 to enter laser light into the cantilever and acquiring a signal of return light received by the detector 82 when the probe 41 performs the scanning motion;

the physical signal may be determined from the signal of the corresponding return light.

In an example, as shown in fig. 5, the laser 81 and the detector 82 are directly or indirectly installed on the device housing 2, at this time, the laser 81 and the detector 82 generate a large amount of heat energy in a vacuum environment, so that light emitting and detecting effects of the laser and the detector are affected, and a temperature in the vacuum environment may be raised, so that a detection effect is affected, therefore, a heat conduction structure 83 is disposed between the laser 81 and the device housing 2, and a heat conduction structure 83 may also be disposed between the detector 82 and the device housing 2. The heat conducting structure 83 may be any material and structure capable of conducting heat to the device housing 2.

In another example, as shown in fig. 6, the laser and the detector may also be mounted to the optical device 7, and may be specifically mounted to an extra-cavity optical structure 71 of the optical device 7, so as to prevent heat accumulation of the laser and the detector 82 from affecting the vacuum environment.

In another embodiment, not shown, the probe 41 includes a cantilever, a contact portion, and a sensing component, the cantilever being connected between the contact portion and the probe driving structure, wherein the cantilever and the contact portion can be understood by referring to the related description.

The sensing component can be used for detecting the deformation and/or deformation stress of the cantilever to obtain a corresponding sensing signal; for example: the sensing component may be, for example, a component capable of changing the resistance of the component under the action of a strain, and the corresponding sensing signal may change in response to the change in the resistance.

The induction component is electrically connected with the control device 5 so as to feed the induction signal back to the control device 5; the physical signal may be determined from the corresponding sensing signal.

Referring to fig. 2, in one embodiment, the chromatography detection apparatus further includes an electrical measurement device 9, wherein the electrical measurement device 9 electrically connects the probe 41 and the sample 6 to form a loop between the probe 41 and the sample 6; the electrical measuring device 9 is also electrically connected with the control device 5 to acquire the probe position information at different times; furthermore, the synchronization of the probe position information and the electrical parameters can be realized.

Specifically, the electrical measurement device 9 is configured to:

acquiring electrical parameters of the loop at different times; the electrical parameter can be any one of the parameters of current, voltage, power, temperature and the like of the loop;

In the solution shown in fig. 2, the above procedure can be implemented with the electrical measuring device 9, in other solutions the above procedure can also be implemented with the control device 5, i.e.: the above process may also be used as a step of the detection method.

Referring to fig. 2, and with reference to the configurations shown in fig. 1 and fig. 3 to fig. 6, for the configuration described above, the control device 5 can control the laser to emit laser light by the laser control signal S-1, and acquire the signal of the return light by the photodetector signal S-2.

If the probe driving assembly 421 adopts a probe motor assembly, then: the control means 5 may control the probe drive assembly by means of a side motor control signal S-3.

If the scanner 422 is a piezo-ceramic scanner, then: the control device 5 can control the scanner 422 to perform the scanning motion by the piezoelectric scanner control signal S-4.

The control means 5 may also control the interaction force between the probe 41 and the sample 6 by means of the cantilever vibration excitation signal S-5, e.g. the interaction force may be controlled to be kept consistent such that: the tip of the probe 41 may undulate with the surface of the sample 6 during the scanning movement.

The control device 5 may also be electrically connected to a temperature control member provided on the sample stage 31, so as to control the temperature of the sample stage and the sample 6 thereon by means of the stage temperature control signal S-6.

If the sample stage driving structure 32 adopts a sample stage motor structure, the control device 5 can control the sample stage driving structure 32 through a sample stage motor control signal S-7.

The control device 5 and the optical device 7 can also acquire a real-time image through an optical system synchronous control signal S-8, so that the probe position information is determined based on the real-time image.

The probe position information can also be synchronized between the control means 5 and the electrical measuring means 9 by means of the electrical measuring unit control signal S-9, so that the electrical parameters can be integrated on the basis of the probe position information.

The electrical measuring device 9 can also collect corresponding electrical parameters through the probe electrical signal S-10 and the sample electrical signal S-11.

In addition to the functions described above, the probe may be cleaned and replaced during the implementation based on the vacuum environment.

Referring to fig. 7, the control device 5 is further configured to:

controlling the probe 41 to be in a tip cleaning position by the probe driving structure 42; wherein the needle tip cleaning position is matched with the ion beam incidence direction, and further can be matched at the intersection of the ion beam incidence direction and the focal plane of the optical device;

the ion beam apparatus 1 is controlled to inject an ion beam to the probe 41 at the tip cleaning position to clean an object to be cleaned on the probe.

In the actual use process, whether the probe 41 has the object to be cleaned can be judged based on the real-time image acquired by the optical device 7, if so, the cleaning process can be automatically controlled, and the cleaning prompt can also be output externally, so that the cleaning process can be realized under manual control.

Referring to fig. 8, the detecting apparatus further includes a probe changing table 33, which can be disposed on the sample table driving structure 32 or disposed independently of the sample table driving structure 32, the probe driving structure is provided with a probe mounting portion (for example, an absorption member capable of generating absorption), the probe 41 is detachably mounted on the probe mounting portion (for example, absorbed on the probe mounting portion) by a probe holder 43, and the probe changing table 33 is provided with at least two probe accommodating positions.

The probe 41 on the needle changing table 33 shown in fig. 8 can be regarded as a backup probe.

the control device 5 is further configured to:

controlling the probe 41 and the probe holder 43 thereof to enter the first containing position through the probe driving structure 42;

controlling the probe mounting part to be separated from the corresponding probe clamp so that the probe and the probe clamp thereof can be left at the first accommodating position; wherein the separation can be achieved, for example, by controlling the adsorption member to no longer adsorb;

controlling the probe mounting section to interface with a probe holder of the back-up probe to enable the back-up probe to be a currently used probe; wherein the docking can be realized by controlling the suction of the suction member, for example.

Through the processes shown in fig. 7 and 8, the probe can be cleaned and replaced in a vacuum environment, and further, the probe can be cleaned and replaced by avoiding opening the shell of the device, and the working efficiency in the detection process is guaranteed.

In addition to the above description, referring to fig. 9, the chromatography detection apparatus may further include a vibration isolation platform 10, the apparatus housing 2 may be disposed on the vibration isolation platform 10, the sample holder 3 may further include an active vibration isolation platform 34, the sample stage driving structure 32 and the sample stage 31 may be directly or indirectly mounted on the active vibration isolation platform 34, and the active vibration isolation platform 34 may receive the apparatus housing 2.

Referring to fig. 9, the apparatus housing 2 may include a housing body 21 and a housing door 24 disposed on an opening side of the housing body 21, a vacuum environment may be formed in the housing body 21 and the housing door 24, and the ion beam device 1 may be disposed on the housing door 24.

The top of the equipment housing 2 can be provided with a viewing window 23, the side wall of the equipment housing 2 can be provided with an electrical interface 22 and an optical interface 24, and the electrical interface 22 can be used for realizing the electrical signal transmission between each internal structure and the control device 5 and the electrical measurement device 9.

The side wall of the device housing 2 can also be provided with an optical interface 25, whereby the optical means 7 can act in the vacuum environment via the optical interface 25.

In summary, in the chromatography detection apparatus and method based on the atomic force microscope and the ion beam provided by the embodiment of the invention, the probe of the atomic force microscope is controlled to interact with the current surface to be detected, and the probe is controlled to perform scanning motion, so that the physical signal representing the physical property of the surface to be detected can be obtained. Meanwhile, the invention also adopts the ion beam to realize the stripping of the surface of the object, which is beneficial to realizing the uniform stripping of the surface of the object.

Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A chromatography detection device based on an atomic force microscope and an ion beam is characterized by comprising an equipment shell, the atomic force microscope, the ion beam device, a control device and a sample bearing device, wherein the equipment shell is used for forming a vacuum environment inside; the sample bearing device and the atomic force microscope are both arranged in the vacuum environment, and the ion beam device is fixedly arranged on the equipment shell;

the control device is used for:

2. The chromatography detection apparatus according to claim 1, further comprising an optical device mounted to the apparatus housing, the optical device facing the region to which the sample stage belongs, and the sample being between the sample stage and the optical device; the interaction location matches a focal plane of the optical device;

the optical device is used for:

the control device is further configured to:

3. The chromatography detection apparatus according to claim 2, wherein the peeling position is matched to an intersection of the ion beam incident direction and a focal plane of the optical apparatus;

4. The chromatography detection apparatus according to claim 2, wherein the optical device is further configured to guide a first auxiliary light and guide the first auxiliary light to the current surface-to-be-detected to form a first light spot on the current surface-to-be-detected;

the first auxiliary light is configured to enable:

5. The apparatus according to claim 2, wherein the optical device is further configured to guide a second auxiliary light and guide the second auxiliary light to the current surface-to-be-measured to form a second light spot on the current surface-to-be-measured;

the second auxiliary light is configured to enable:

6. The chromatography detection apparatus according to any one of claims 2 to 5, further comprising an electrical measurement device electrically connecting the probe and the sample to form a loop between the probe and the sample; the electrical measuring device is also electrically connected with the control device to acquire the probe position information at different times;

the electrical measurement device is configured to:

acquiring electrical parameters of the loop at different times;

7. The chromatography detection apparatus according to any one of claims 1 to 5, further comprising a laser assembly, wherein the laser assembly comprises a laser and a detector, and the control device is electrically connected to the laser and the detector respectively; the probe comprises a cantilever and a contact part, and the cantilever is connected between the contact part and the probe driving structure;

the control device is further configured to:

the interaction of the probe with the sample surface is controlled by the signal of the returned light.

8. The chromatography detection apparatus according to claim 7, wherein the laser and the detector are directly or indirectly mounted on the device housing, and a heat conduction structure is provided between the laser and the device housing, and a heat conduction structure is also provided between the detector and the device housing.

9. The apparatus according to claim 7, wherein the laser and the detector are mounted to an optical device.

10. The chromatography detection apparatus according to any one of claims 1 to 5, wherein the control apparatus is further configured to:

after the stripping of the sample is completed for N times and the corresponding physical property diagram is obtained, constructing a corresponding three-dimensional chromatographic image based on the N physical property diagrams; wherein N is an integer greater than or equal to 2.

11. The chromatography detection apparatus according to any one of claims 1 to 5, wherein the probe comprises a cantilever, a contact portion, and a sensing member, the cantilever being connected between the contact portion and the probe driving structure;

the physical signal is determined from the corresponding sensing signal.

12. The chromatography detection apparatus according to any one of claims 1 to 5, wherein the control apparatus is further configured to:

13. The chromatography detection apparatus according to any one of claims 1 to 5, further comprising a probe changing table, wherein the probe driving structure is provided with a probe mounting portion, the probe is detachably mounted on the probe mounting portion through a probe holder, and the probe changing table is provided with at least two probe accommodating positions;

the control device is further configured to:

14. The chromatography detection apparatus according to any one of claims 1 to 5, wherein the control device controls the sample to be in the peeling position and further functions to:

15. The chromatography detection apparatus according to any one of claims 1 to 5, wherein the probe driving mechanism comprises a probe driving assembly and a scanner, the probe is directly or indirectly mounted on the scanner, and the scanner is mounted on the probe driving assembly;

16. A chromatography detection apparatus according to any one of claims 1 to 5, wherein the initial vacuum level of the vacuum environment is higher than 1 mPa; the working air pressure controlled by the ion beam is at least 10 times larger than the initial vacuum degree.

17. A chromatography detection method based on an atomic force microscope and an ion beam is characterized in that a chromatography detection device based on the atomic force microscope and the ion beam is adopted, and the chromatography detection device comprises an equipment shell, the atomic force microscope, the ion beam device, a control device and a sample bearing device, wherein the equipment shell is used for forming a vacuum environment inside; the sample bearing device and the atomic force microscope are both arranged in the vacuum environment, and the ion beam device is fixedly arranged on the equipment shell;

repeating the above process, and after completing the stripping of the sample for N times and acquiring corresponding N physical property maps, constructing a corresponding three-dimensional chromatographic image based on the N physical property maps, wherein N is greater than or equal to 2.