CN108717130B - Detection device, copper sheet and detection method for fixing AFM probe - Google Patents
Detection device, copper sheet and detection method for fixing AFM probe Download PDFInfo
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- CN108717130B CN108717130B CN201810433434.9A CN201810433434A CN108717130B CN 108717130 B CN108717130 B CN 108717130B CN 201810433434 A CN201810433434 A CN 201810433434A CN 108717130 B CN108717130 B CN 108717130B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q10/00—Scanning or positioning arrangements, i.e. arrangements for actively controlling the movement or position of the probe
Abstract
The invention discloses a detection device, a copper sheet and a detection method for fixing an AFM probe, wherein the detection device comprises: the shape of the copper sheet is characterized by a semicircular sheet with a preset thickness and a preset diameter, and a trapezoidal opening is arranged at the central axis position of the semicircular sheet so as to generate an inclined plane-shaped opening which is concave inwards to the copper sheet; an optical microscope; and the controller is used for coating the adhesive on a preset position on the copper sheet through the cantilever beam without the needle point under the optical microscope, contacting the probe of the AFM to be detected with the position of the adhesive on the copper sheet through the optical microscope, gradually pressurizing until the cantilever beam of the probe of the AFM to be detected is broken, and lifting the silicon substrate without the cantilever beam after the silicon substrate and the cantilever beam are separated, so that the cantilever beam and the needle point of the probe of the AFM to be detected are remained on the copper sheet for transmission electron microscope detection. The detection device has the advantages of simple structure, portability and extremely low cost.
Description
Technical Field
The invention relates to the technical field of microscope detection, in particular to a detection device, a copper sheet and a detection method for detecting a fixed AFM (Atomic force microscope) probe in a TEM (Transmission electron microscope).
Background
The tribology research is not limited to the experiment under a macroscopic friction instrument, and in recent 10 years, with the development and application of instruments such as an Atomic Force Microscope (AFM) and the like, the tribology research plays a great promoting role in the research of the ultra-smooth microscopic mechanism. Meanwhile, because the area of the contact area is greatly reduced, how to analyze the friction process becomes a very important problem. Since the contact area cannot be analyzed qualitatively, the detection of the tip of an Atomic Force Microscope (AFM) probe after the test becomes an important means for determining the rubbing process. Transmission Electron Microscopy (TEM) is an important tool for analyzing Atomic Force Microscopy (AFM) tips.
At present, two modes can assist a Transmission Electron Microscope (TEM) to detect the tip of an Atomic Force Microscope (AFM) probe, one mode is to fix the probe by adopting a specific clamp, the cost of the clamp is as high as fifteen thousand RMB, and the cost of a Transmission Electron Microscope (TEM) detection experiment is greatly improved. Secondly, FIB (Focused ion beam) is adopted to strip the surface layer of the needle tip surface, the method has low cost but long experiment time consumption and damages the needle tip surface, so that the needle tip cannot be repeatedly detected.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
Therefore, an object of the present invention is to provide a detection device for fixing an AFM probe, which has a simple structure, is portable, is extremely low in cost, is convenient to manufacture a sample, has a short operation time, and does not damage a tip.
It is another object of the present invention to provide a copper sheet for use in immobilizing an AFM probe.
It is a further object of the present invention to provide a detection method for a fixed AFM probe.
In order to achieve the above object, an embodiment of the present invention provides a detection apparatus for fixing an AFM probe, including: the copper sheet is characterized by being a semicircular sheet with a preset thickness and a preset diameter in shape, and a trapezoidal opening is formed in the central axis of the semicircular sheet so as to generate an inclined plane-shaped opening which is concave inwards towards the copper sheet; an optical microscope; and the controller is used for smearing the adhesive at a preset position on the copper sheet through the cantilever beam without the needle point under the optical microscope, contacting the probe of the AFM to be detected with the position of the adhesive on the copper sheet through the optical microscope, gradually pressurizing until the cantilever beam of the probe of the AFM to be detected is broken, and lifting the silicon substrate without the cantilever beam after the silicon substrate is separated from the cantilever beam, so that the cantilever beam and the needle point of the probe of the AFM to be detected are remained on the copper sheet for transmission electron microscope detection.
According to the detection device for fixing the AFM probe, disclosed by the embodiment of the invention, the adhesive is coated at the specific position of the fixing device by using the AFM cantilever beam without the tip, the AFM tip to be detected is fixed at the position of the adhesive through the adhesive so as to be detected by a transmission electron microscope, a simple and efficient means can be provided for the analysis of the probe property in a microscopic tribology experiment, research conditions are provided for the analysis of a friction mechanism and the research and development of novel materials, the structure is simple, the detection device is light and portable, the cost is extremely low, the sample is convenient to manufacture, the operation time is short, and the tip cannot be damaged.
In addition, the detection device for fixing the AFM probe according to the above embodiment of the present invention may further have the following additional technical features:
further, in one embodiment of the present invention, the predetermined position on the copper sheet is a 45 ° sharp point of the copper sheet.
Further, in an embodiment of the present invention, the predetermined thickness is 0.1mm, and the predetermined diameter is 3 mm.
Further, in an embodiment of the present invention, the method further includes: the fixed probe is used for dipping a preset amount of adhesive and smearing the preset amount of adhesive on the sharp 45-degree angle part of the copper sheet.
In order to achieve the above object, according to another aspect of the present invention, a copper sheet for fixing an AFM probe is provided, wherein the copper sheet has a shape characterized by a semicircular sheet with a preset thickness and a preset diameter, and a trapezoidal opening is provided at a central axis of the semicircular sheet to generate a bevel-shaped opening that is concave towards the copper sheet. The copper sheet is convenient to process, simple in structure, portable and extremely low in cost.
In order to achieve the above object, an embodiment of another aspect of the present invention provides a detection method for fixing an AFM probe, including the following steps: coating an adhesive on a preset position on the copper sheet through a cantilever beam without a needle point under the optical microscope, and contacting a probe of an Atomic Force Microscope (AFM) to be detected with the position of the adhesive on the copper sheet through the optical microscope; gradually pressurizing until the cantilever beam of the probe of the AFM to be detected is broken; and after the silicon substrate is separated from the cantilever beam, lifting the silicon substrate without the cantilever beam, so that the cantilever beam and the needle point of the probe of the AFM to be detected are left on the copper sheet for transmission electron microscope detection.
According to the detection method for fixing the AFM probe, disclosed by the embodiment of the invention, the adhesive is coated at the specific position of the fixing device by using the AFM cantilever beam without the tip, the AFM tip to be detected is fixed at the position of the adhesive through the adhesive so as to be detected by a transmission electron microscope, a simple and efficient means can be provided for the analysis of the probe property in a microscopic tribology experiment, research conditions are provided for the analysis of a friction mechanism and the research and development of novel materials, the structure is simple, the detection method is light and portable, the cost is extremely low, the sample is convenient to manufacture, the operation time is short, and the tip cannot be damaged.
In addition, the detection method for fixing the AFM probe according to the above embodiment of the present invention may further have the following additional technical features:
further, in one embodiment of the present invention, the predetermined position on the copper sheet is a 45 ° sharp point of the copper sheet.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic structural diagram of a detection device for immobilizing an AFM probe according to one embodiment of the present invention;
FIG. 2 is a schematic diagram of an apparatus and inspection of a transmission electron microscope according to one embodiment of the present invention;
FIG. 3 is a schematic view of a copper sheet used to secure an AFM probe according to one embodiment of the present invention;
FIG. 4 is a schematic diagram of the manner of use of a probe for immobilizing an AFM in accordance with one embodiment of the present invention;
FIG. 5 is a flow chart of a detection method for immobilizing an AFM probe according to one embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
The detection apparatus, the copper sheet and the detection method for fixing the AFM probe according to the embodiment of the present invention will be described below with reference to the accompanying drawings, and first, the detection apparatus for fixing the AFM probe according to the embodiment of the present invention will be described with reference to the accompanying drawings.
FIG. 1 is a schematic structural diagram of a detection device for immobilizing an AFM probe according to one embodiment of the present invention.
As shown in fig. 1, the inspection apparatus 10 for fixing an AFM probe includes: copper sheet 100, optical microscope 200 and controller 300.
The shape of the copper sheet 100 is characterized by a semicircular sheet with a preset thickness and a preset diameter, and a trapezoidal opening is formed in the central axis of the semicircular sheet to form an inclined opening which is concave towards the copper sheet. An optical microscope 200. The controller 300 is configured to apply an adhesive to a preset position on the copper sheet through the cantilever without the tip under the optical microscope, contact the probe of the AFM to be detected with the position of the adhesive on the copper sheet through the optical microscope, gradually pressurize the probe until the cantilever of the AFM probe to be detected is broken, and lift the silicon substrate without the cantilever after the silicon substrate and the cantilever are separated, so that the cantilever and the tip of the AFM probe to be detected are left on the copper sheet for transmission electron microscope detection. The detection device provided by the embodiment of the invention has the advantages of simple structure, portability, extremely low cost, convenience in sample preparation, short operation time and no damage to the needle point.
Further, in one embodiment of the present invention, the predetermined position on the copper sheet may be a 45 ° acute position of the copper sheet.
It will be appreciated that embodiments of the present invention use a cantilever beam without a needle tip to apply adhesive to specific locations on the fixation device, such as a 45 ° sharp point on a piece of copper.
Further, in one embodiment of the present invention, the predetermined thickness may be 0.1mm, and the predetermined diameter may be 3 mm.
It can be understood that in the embodiment of the invention, the copper sheet is manufactured by adopting a copper sheet, the copper sheet is processed into a specific shape by adopting means such as wire cutting, and the like, the copper sheet is used for fixing the probe tip of an Atomic Force Microscope (AFM) to carry out Transmission Electron Microscope (TEM) detection, the shape of the copper sheet is characterized by a semicircular sheet with the thickness of 0.1mm and the diameter of 3mm, a trapezoidal opening is arranged on the axis of the sheet, the shape of the miniature copper sheet is commonly characterized by an inward concave inclined plane-shaped opening, the size is explained by the example but not limited to the example, the copper sheet is suitable for carrying out Transmission Electron Microscope (TEM) detection on the AFM probes of all models, and the copper sheet is characterized by simplicity, easiness in manufacturing, low cost and no damage to the structure of the probe tip. In the embodiment of the present invention, the copper sheet may also be referred to as a micro copper sheet. The setup and examination of a Transmission Electron Microscope (TEM) is shown in fig. 2.
Specifically, as shown in FIG. 3, the embodiment of the present invention was fabricated by machining a 0.1mm thick copper sheet. A3 mm diameter wafer was first cut from a copper sheet and then cut into two semicircles. Taking one semicircle, marking two points at 0.5mm positions on two sides of the central axis of the semicircle, cutting the semicircle along the direction away from the central axis at the two points along the direction of 45 degrees, wherein the cutting depth is 0.5mm along the direction of the central axis, then buckling the whole shearing part, and finishing the manufacturing of the fixing device.
Further, in an embodiment of the present invention, the method further includes: and (4) fixing the probe. The fixed probe is used for dipping a preset amount of adhesive and smearing the preset amount of adhesive on a sharp 45-degree angle part of the copper sheet.
It can be understood that the embodiment of the invention needs to coat an adhesive on the surface of the micro copper sheet, and the preparation experiments before the detection of the Transmission Electron Microscope (TEM) are all carried out under an optical microscope, and a small amount of adhesive is dipped by a pinpoint-free Atomic Force Microscope (AFM) cantilever beam firstly, and then the cantilever beam is contacted with a specific position of the micro copper sheet, and the adhesive is coated on the position.
Furthermore, the needle point is fixed on the micro copper sheet, firstly, with the help of an optical microscope, the probe of the Atomic Force Microscope (AFM) to be detected is contacted with the position of the adhesive on the micro copper sheet, then, the pressure is gradually applied until the cantilever beam of the probe of the Atomic Force Microscope (AFM) is pressed off, the silicon substrate is separated from the cantilever beam, then, the silicon substrate without the cantilever beam is lifted, and at the moment, the cantilever beam and the needle point of the probe of the Atomic Force Microscope (AFM) are remained on the micro copper sheet and cannot cause any damage to the needle point, so that the truth and credibility of the detection result of the transmission electron microscope are ensured.
Specifically, as shown in fig. 4, the usage of the device according to the embodiment of the present invention is described, wherein the entire usage process is performed under an optical microscope. In addition to the probe to be immobilized (probe A), a cantilever without a tip (probe B) is required in the immobilization process. The fixing process is divided into three steps:
first, dip in a small amount of gluing agent with probe B, notice holding the quantity of gluing agent, too much or too little will all cause harmful effects to the fixed process, and the technical staff in the art can hold the quantity according to particular case, does not do the specific limit here.
And secondly, coating the adhesive on a 45-degree sharp position of the fixing device by using the probe B, wherein care needs to be taken not to break the probe B, otherwise, the fixation of the tip of the probe A is influenced.
The third step, press probe A and scribble gluing agent department in last step, add power gradually, keep away from the sharp-ended fracture of needle until probe A cantilever beam, probe A's cantilever beam is fixed on gluing agent and the needle point is unsettled this moment, and this one step of need is noticed the position of pressing probe A, and too outer can make fixed not firm, and too can lead to the unsettled position of needle point to be too close to fixing device by the lining, is unfavorable for the detection.
In summary, embodiments of the present invention are directed to a simple apparatus for fixing a probe tip of an Atomic Force Microscope (AFM) for a Transmission Electron Microscope (TEM) detection, and the apparatus of the embodiments of the present invention has the following advantages:
(1) firstly, the cost is low, only a piece of copper sheet with the thickness of 0.1mm needs to be processed, and only one Atomic Force Microscope (AFM) cantilever beam without a needle point needs to be adopted in the process of fixing the needle point to be detected.
(2) Secondly, the experiment time is short, if a method of stripping the surface layer by using a Focused Ion Beam (FIB) needs about ten hours, and under the condition of skillfully using the device, the time for fixing the needle point on the device only needs a few minutes, so the experiment efficiency is greatly improved.
(3) Finally, the device provided by the embodiment of the invention does not damage the needle tip part, so that on one hand, the truth and credibility of the detection result are ensured, and on the other hand, the possibility of carrying out multiple detections on the same needle tip is provided.
According to the detection device for fixing the AFM probe, provided by the embodiment of the invention, the adhesive is coated at the specific position of the fixing device by using the AFM cantilever without the tip, the AFM tip to be detected is fixed at the position of the adhesive through the adhesive so as to be detected by the transmission electron microscope, a simple and efficient means can be provided for the analysis of the probe property in a microscopic tribology experiment, research conditions are provided for the analysis of a friction mechanism and the research and development of novel materials, the structure is simple, the detection device is light and portable, the cost is extremely low, the sample is convenient to manufacture, the operation time is short, and the tip cannot be damaged.
In addition, the embodiment of the invention also provides a copper sheet for fixing the AFM probe, wherein the shape of the copper sheet is characterized by a semicircular sheet with a preset thickness and a preset diameter, and a trapezoidal opening is arranged at the central axis position of the semicircular sheet so as to generate an inclined plane-shaped opening which is concave towards the copper sheet. The copper sheet is convenient to process, simple in structure, portable and extremely low in cost.
Next, a description will be given of a detection method for fixing an AFM probe according to an embodiment of the present invention with reference to the accompanying drawings.
FIG. 5 is a flow chart of a detection method for immobilizing an AFM probe in accordance with one embodiment of the present invention.
As shown in fig. 5, the detection method for fixing the AFM probe includes:
in step S501, an adhesive is coated on a preset position on the copper sheet through a cantilever beam without a needle point under the optical microscope, and a probe of the atomic force microscope AFM to be detected is contacted with the position of the adhesive on the copper sheet through the optical microscope.
In step S502, the pressure is gradually applied until the cantilever of the probe of the AFM to be tested is broken.
In step S503, after the silicon substrate and the cantilever beam are separated, the silicon substrate without the cantilever beam is lifted, so that the cantilever beam and the tip of the probe of the AFM to be detected are left on the copper sheet for transmission electron microscope detection.
Further, in one embodiment of the present invention, the predetermined position on the copper sheet is a 45 ° sharp point of the copper sheet.
It should be noted that the foregoing explanation of the embodiment of the detection apparatus for fixing the AFM probe is also applicable to the detection method for fixing the AFM probe of the embodiment, and details are not repeated herein.
According to the detection method for fixing the AFM probe, provided by the embodiment of the invention, the adhesive is coated at the specific position of the fixing device by using the AFM cantilever without the tip, the AFM tip to be detected is fixed at the position of the adhesive through the adhesive so as to be detected by the transmission electron microscope, a simple and efficient means can be provided for the analysis of the probe property in the micro tribology experiment, research conditions are provided for the analysis of a friction mechanism and the research and development of novel materials, the structure is simple, the detection method is light and portable, the cost is extremely low, the sample is convenient to manufacture, the operation time is short, and the tip cannot be damaged.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (6)
1. A test device for immobilizing an AFM probe, comprising:
the copper sheet is characterized by being a semicircular sheet with a preset thickness and a preset diameter in shape, and a trapezoidal opening is formed in the central axis of the semicircular sheet so as to generate an inclined plane-shaped opening which is concave inwards towards the copper sheet;
an optical microscope; and
and the controller is used for smearing the adhesive on a preset position on the copper sheet through the cantilever beam without the tip under the optical microscope, contacting the probe of the AFM to be detected with the position of the adhesive on the copper sheet through the optical microscope, gradually pressurizing until the cantilever beam of the probe of the AFM to be detected is broken, and lifting the silicon substrate without the cantilever beam after the silicon substrate is separated from the cantilever beam, so that the cantilever beam and the tip of the probe of the AFM to be detected are remained on the copper sheet for transmission electron microscope detection, wherein the preset position is on the cross sections of two ends of the trapezoidal opening of the copper sheet, and the tip of the probe of the AFM to be detected is positioned on the upper part of the trapezoidal opening.
2. The detecting device for fixing the AFM probe as claimed in claim 1, wherein the predetermined position on the copper sheet is a 45 ° sharp point of the copper sheet, wherein the sharp point is a sharp angle formed by a cross section and a slope of a trapezoid opening.
3. The probing apparatus for immobilizing an AFM probe according to claim 1, wherein the predetermined thickness is 0.1mm and the predetermined diameter is 3 mm.
4. The probing apparatus for immobilizing an AFM probe according to claim 2, further comprising:
the fixed probe is used for dipping a preset amount of adhesive and smearing the preset amount of adhesive on the sharp 45-degree angle part of the copper sheet.
5. A detection method for fixing an AFM probe is characterized by comprising the following steps:
coating an adhesive at a preset position on a copper sheet through a cantilever beam without a needle point under an optical microscope, and contacting a probe of an AFM to be detected with the position of the adhesive on the copper sheet through the optical microscope, wherein the shape of the copper sheet is characterized by a semicircular sheet with a preset thickness and a preset diameter, a trapezoidal opening is arranged at the central axis position of the semicircular sheet to generate an inclined plane-shaped opening which is concave towards the copper sheet, the preset position is on the cross sections of two ends of the trapezoidal opening of the copper sheet, and the needle point of the probe of the AFM to be detected is positioned at the upper part of the trapezoidal opening;
gradually pressurizing until the cantilever beam of the probe of the AFM to be detected is broken;
and after the silicon substrate is separated from the cantilever beam, lifting the silicon substrate without the cantilever beam, so that the cantilever beam and the needle point of the probe of the AFM to be detected are left on the copper sheet for transmission electron microscope detection.
6. The detecting method for fixing the AFM probe as claimed in claim 5, wherein the predetermined position on the copper sheet is a 45 ° sharp point of the copper sheet, wherein the sharp point is a sharp angle formed by a cross section and a slope of a trapezoid opening.
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| JPH07113634A (en) * | 1993-10-18 | 1995-05-02 | Matsushita Electric Ind Co Ltd | Probe for scanning probe microscope, manufacture thereof, recording reproducer using probe and fine machining device |
| JP2002062253A (en) * | 2000-08-21 | 2002-02-28 | Hidehiro Kamiya | Method and device for manufacturing colloid probe |
| US7348570B2 (en) * | 2005-12-14 | 2008-03-25 | University Of Washington | Unsupported, electron transparent films and related methods |
| DE102010032894B4 (en) * | 2010-07-30 | 2013-08-22 | Carl Zeiss Microscopy Gmbh | Tem lamella, process for its preparation and apparatus for carrying out the process |
| EP2755226B1 (en) * | 2013-01-15 | 2016-06-29 | Fei Company | Sample carrier for an electron microscope |
| CN104792583B (en) * | 2014-01-17 | 2018-06-26 | 中芯国际集成电路制造(上海)有限公司 | A kind of preparation method of TEM sample |
| CN104360107B (en) * | 2014-11-12 | 2016-11-30 | 苏州大学 | A kind of graphene coated atomic force microscope probe and preparation method thereof, purposes |
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