CN113325021A - In-situ testing method and sample platform capable of carrying micro-nano-scale sample - Google Patents
In-situ testing method and sample platform capable of carrying micro-nano-scale sample Download PDFInfo
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- CN113325021A CN113325021A CN202110596603.2A CN202110596603A CN113325021A CN 113325021 A CN113325021 A CN 113325021A CN 202110596603 A CN202110596603 A CN 202110596603A CN 113325021 A CN113325021 A CN 113325021A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
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Abstract
The invention discloses a sample stage capable of carrying a micro-nano scale sample, which comprises a base, a sealing cover and a metal wire, wherein the base is in a cube shape, six faces of the cube are respectively provided with a threaded hole, the sealing cover is fixedly connected with the upper surface of the base through screws, the middle part and the bottom of the metal wire are positioned between the sealing cover and the base, the middle part and the bottom of the metal wire are clamped by the sealing cover and the base, the top end of the metal wire is a plane, and the micro-nano scale sample is fixed on the plane of the top end of the metal wire through a micro-deposition welding process. A micro-nano scale sample is fixed at the top end of a metal wire in the sample table, and the sample table is clamped on a micro mechanical tester to carry out in-situ test on the micro-nano scale sample. The in-situ test method and the sample platform capable of carrying the micro-nano scale sample can be used for conveniently preparing, transferring and testing the micro-nano scale sample.
Description
Technical Field
The invention relates to the technical field of micro-nano mechanics and micro-electro-mechanical systems, in particular to an in-situ testing method and a sample table capable of carrying micro-nano scale samples.
Background
The scanning electron microscope is a large-scale precision instrument used for high-resolution micro-area morphology analysis, and has the characteristics of large depth of field, high resolution, visual imaging, strong stereoscopic impression, wide magnification range, capability of rotating and inclining a sample to be detected in a three-dimensional space and the like. The secondary electron imaging principle is one of various scanning electron microscopes with the widest application and the strongest resolving power. The electron beam emitted from the electron gun is narrowed and focused by the condenser lens and the objective lens to form an electron beam on the surface of the sample, and secondary electrons are excited due to the difference of the surface structure of the sample. The secondary electron collector can collect the secondary electrons emitted from all directions, and the secondary electrons are processed into optical signals by the scintillator, the optical signals are converted into electric signals by the photomultiplier tube, and the electric signals are transmitted to the grid of the kinescope by the video amplifier, so that a secondary electron scanning image of the surface appearance of the sample is presented on the screen.
The focused ion beam system uses an electric lens to accelerate ion beams generated by an ion source through an ion gun, the ion beams are focused and then act on the surface of a sample to generate secondary electronic signals to obtain electronic images, and the surface atoms are stripped by a strong current ion beam to finish micro-nano surface topography processing, or a physical sputtering mode is matched with chemical gas reaction to selectively strip metals, silicon oxide layers or deposit metal layers. After the focused ion beam system and the scanning electron microscope are coupled into a focused ion beam-scanning electron microscope double-beam system, the sample in the scanning electron microscope cabin can be subjected to micro-cutting or micro-deposition welding with extremely small size.
In the micro-nano scale mechanical test process, a micro-nano scale sample cut by a focused ion beam is often extracted from a bulk sample, and then in-situ mechanical test is further carried out, while a common sample table, whether being a cylindrical sample table or a prefabricated inclined sample table, faces to the bulk sample and can only be manually loaded outside a scanning electron microscope cabin. For a micro-nano-scale sample, the existing method is to perform inclined observation through the self-contained inclination function of equipment, and has the angle limitation of scanning electron microscope equipment, but the inclination function of the current scanning electron microscope bearing table base is only-30-90 degrees, and the sample table may impact a probe in the large-angle inclination process, so that the equipment is damaged, the micro-scale sample is difficult to directly operate, and the method is not fast and convenient and has low fault-tolerant rate.
The existing scanning electron microscope equipment cannot observe and prepare a sample in multiple dimensions in a self-inclined function transfer mode, cannot be operated outside a cabin, needs to be applied to the transfer, rotation and re-arrangement processes of a mechanical arm, is long in operation process consumption and low in fault tolerance rate, cannot be combined with the subsequent preparation and test processes of the sample, and can only be carried out in the scanning electron microscope cabin.
Disclosure of Invention
The invention aims to provide an in-situ testing method and a sample platform capable of carrying a micro-nano scale sample, so as to solve the problems in the prior art and facilitate the transfer and testing of the micro-nano scale sample.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a sample stage capable of carrying a micro-nano scale sample, which comprises a base, a sealing cover and a metal wire, wherein the base is in a cube shape, threaded holes are respectively formed in six faces of the cube, the sealing cover is fixedly connected with the upper surface of the base through screws, the middle part and the bottom of the metal wire are positioned between the sealing cover and the base, the middle part and the bottom of the metal wire are clamped by the sealing cover and the base, the top end of the metal wire is a plane, and the micro-nano scale sample is fixed on the plane of the top end of the metal wire through a micro-deposition welding process.
Preferably, a groove is formed between the cover and the base, the groove is arranged on the upper surface of the base, and the middle part and the bottom part of the metal wire are inserted into the groove.
Preferably, a conductive adhesive is filled between the metal wire and the groove.
Preferably, the groove is semi-cylindrical.
Preferably, a right-angle notch is formed in one edge of the base, which is close to the top end of the metal wire.
The invention also provides an in-situ test method, which comprises the following steps:
(1) cutting a micro-nano scale sample with a right-angled trapezoid cross section from the surface of a bulk sample by using a focused ion beam-scanning electron microscope dual-beam system, and keeping the connection of one side of the micro-nano scale sample and the bulk sample;
(2) combining the micro-nano scale sample with a built-in mechanical arm by using a micro-deposition welding technology, and cutting off the connection between the micro-nano scale sample and the bulk sample by using a focused ion beam;
(3) fixing the micro-nano scale sample on a plane at the top end of a metal wire clamped by a sample stage by using a micro-deposition welding technology, and cutting off the connection between the micro-nano scale sample and the mechanical arm by using a focused ion beam;
(4) taking the sample stage out of the scanning electron microscope, namely manually completing three-dimensional rotation outside a cabin of the scanning electron microscope, then placing the sample stage into the scanning electron microscope at different angles, cutting the micro-nano scale sample positioned at the top end of the metal wire by using a focused ion beam, and performing a preparation process of a micro-nano material complex structure required by mechanical testing;
(5) after the preparation is finished, clamping the sample stage on a micro mechanical tester, and aligning the top end surface of the metal wire by adjusting the position of the sample stage, so that a probe of the micro mechanical tester is exactly aligned with a complex structure acting point of the micro-nano scale sample;
(6) and then, the mechanical properties of the micro-nano scale sample under various stress conditions are tested under in-situ observation by operating the micro mechanical tester.
Compared with the prior art, the invention has the following technical effects:
the in-situ test method and the sample platform capable of carrying the micro-nano scale sample can be used for conveniently preparing, transferring and testing the micro-nano scale sample. The in-situ testing method and the sample platform capable of carrying the micro-nano-scale sample provide a concept of 'controlling the size by the size', the top end of the metal wire is used as a platform for bearing the micro-nano-scale sample, and the micro-nano-scale sample which can not be seen by naked eyes can be manually operated by clamping the metal wire by the sample platform provided by the invention to perform directional movement and rotation of a three-dimensional angle, so that the preparation, transfer and testing processes of the micro-nano-scale complex sample can be conveniently performed by utilizing a focused ion beam-scanning electron microscope dual-beam system. The invention has reasonable design, compact structure and convenient operation, and is convenient for the calibration process of the probe and the loading end with the same axis in the subsequent mechanical test. The sample stage provided by the invention is not provided with a rotating shaft, so that the problem of poor conductivity is avoided. For metal wires with different diameters, the conducting adhesive or the double-sided conducting adhesive tape can be used for fixing, and meanwhile, three-dimensional directional rotation is convenient to carry out. The micro-nano scale sample is stably and reliably placed, the complex operations of large-angle inclination and rotation of the sample stage of the device are avoided, meanwhile, the sample stage of the device is prevented from impacting a receiving probe, and the safe use of the scanning electron microscope is ensured.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments 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 it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a sample stage capable of carrying a micro-nano-scale sample according to the invention;
FIG. 2 is a schematic diagram I of a partial structure of a sample stage capable of carrying a micro-nano-scale sample according to the invention;
FIG. 3 is a schematic diagram of a partial structure of a sample stage capable of carrying a micro-nano-scale sample according to the invention;
FIG. 4 is a schematic diagram of a part of a structure of a sample stage capable of carrying a micro-nano-scale sample according to the invention;
wherein: 100. the sample stage can carry a micro-nano scale sample; 1. a base; 2. a metal wire; 3. sealing the cover; 4. a threaded hole; 5. a right-angle opening; 6. a groove; 7. and (4) screws.
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 obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
The invention aims to provide an in-situ testing method and a sample platform capable of carrying a micro-nano scale sample, so as to solve the problems in the prior art and facilitate the transfer and testing of the micro-nano scale sample.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in fig. 1 to 4: the embodiment provides a sample stage 100 capable of carrying a micro-nano scale sample, which comprises a base 1, a sealing cover 3 and a metal wire 2, wherein the base 1 is in a cube shape, six faces of the cube are respectively provided with a threaded hole 4, the sealing cover 3 is fixedly connected with the upper surface of the base 1 through a screw 7, and the threaded holes 4 on the other five faces of the base 1 except the upper surface are used for being connected with bayonet screws of an SEM (scanning electron microscope).
A groove 6 is formed between the cover 3 and the base 1, the groove 6 is arranged on the upper surface of the base 1, the groove 6 is semi-cylindrical, and the middle part and the bottom part of the upper metal wire 2 are inserted into the groove 6. In practical application, the number of the grooves 6 can be increased; the middle part and the bottom of the metal wire 2 are positioned between the sealing cover 3 and the base 1, the sealing cover 3 and the base 1 clamp the middle part and the bottom of the metal wire 2, the top end of the metal wire 2 is a plane, and the micro-nano scale sample is fixed on the plane at the top end of the metal wire 2 through a micro-deposition welding process.
Conductive adhesive is filled between the metal wire 2 and the groove 6, so that the conductivity between the metal wire 2 and the groove 6 is improved, and the condition that the sample stage is poor in conductivity is avoided; the conductive adhesive can also prevent the metal wire from slipping, and besides the conductive adhesive, the metal wire can also be fixed through the conductive adhesive tape. A right-angle opening 5 is formed in one edge, close to the top end of the metal wire 2, of the base 1, and the top of the metal wire can be observed conveniently due to the fact that the right-angle opening 5 is formed.
The base 1 and the cover 3 are both made of metal materials, preferably aluminum materials, and the metal aluminum has good conductivity, low cost and simple processing, so the material is an ideal material for processing a sample stage of a scanning electron microscope. After the base 1 and the cover 3 are combined, the total height of the base 1 and the cover 3 does not exceed 20 mm. The metal wire is preferably a highly conductive metal wire such as a gold wire, a silver wire, or a copper wire.
The invention also provides an in-situ test method, which comprises the following steps:
(1) cutting a micro-nano scale sample with a right-angled trapezoid cross section from the surface of the bulk sample by using a focused ion beam-scanning electron microscope dual-beam system, and keeping the connection of one side of the micro-nano scale sample with the bulk sample;
(2) combining the micro-nano scale sample with a built-in mechanical arm by using a micro-deposition welding technology, and cutting off the connection between the micro-nano scale sample and the bulk sample by using a focused ion beam;
(3) fixing the micro-nano-scale sample on a plane at the top end of a metal wire clamped by a sample stage by using a micro-deposition welding technology, and cutting off the connection between the micro-nano-scale sample and a mechanical arm by using a focused ion beam;
(4) taking the sample stage out of the scanning electron microscope, namely manually completing three-dimensional rotation outside a cabin of the scanning electron microscope, then placing the sample stage into the scanning electron microscope at different angles, cutting a micro-nano scale sample positioned at the top end of a metal wire by using a focused ion beam, and performing a preparation process of a micro-nano material complex structure required by mechanical testing;
(5) after the preparation is finished, clamping the sample table on a micro mechanical tester, and aligning the top end surface of the metal wire by adjusting the position of the sample table, so that the probe of the micro mechanical tester is exactly aligned with the force application point of the complex structure of the micro-nano scale sample;
(6) then, the mechanical properties of the micro-nano scale sample under various stress conditions are tested under in-situ observation by operating a micro mechanical tester; specifically, a micro loading device is adopted to perform stress relaxation test on the micro-nano scale sample. The wedge probe loads the free end of the cantilever beam of the sample structure, the piezoelectric actuator in the capacitive transducer realizes the collection of force-displacement data, and the morphological evolution process of the micro-cantilever beam in the bending process is observed and recorded in real time in a scanning electron microscope, so that the further research is realized; by using the sample stage 100 capable of carrying the micro-nano-scale sample and the in-situ testing method provided by the embodiment, the micro-nano-scale sample processed by the focused ion beam can be fixed at the top end of the metal wire at the edge of the sample stage, so that the in-situ mechanical test can be further performed by using the in-situ scanning electron microscope technology in cooperation with a nano-indenter such as Pi-88. It should be noted that, for the steps of placing, grasping and finally transferring the sample stage holder in the sem to the sample chamber for observation, the present invention does not refer to the in-situ sem observation method in the prior art for the bulk sample.
In the description of the present invention, it should be noted that the terms "top", "bottom", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, which are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
The principle and the implementation mode of the present invention are explained by applying specific examples in the present specification, and the above descriptions of the examples are only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (6)
1. The utility model provides a can carry on sample platform of receiving a little yardstick sample which characterized in that: the device comprises a base, a sealing cover and a metal wire, wherein the base is in a cube shape, threaded holes are formed in six faces of the cube respectively, the sealing cover is fixedly connected with the upper surface of the base through screws, the middle part and the bottom of the metal wire are located between the sealing cover and the base, the sealing cover and the base clamp the middle part and the bottom of the metal wire tightly, the top end of the metal wire is a plane, and a micro-nano scale sample is fixed on the plane of the top end of the metal wire through a micro-deposition welding process.
2. The sample stage capable of carrying the micro-nano-scale sample according to claim 1, wherein: a groove is formed between the sealing cover and the base, the groove is formed in the upper surface of the base, and the middle and the bottom of the metal wire are inserted into the groove.
3. The sample stage capable of carrying the micro-nano-scale sample according to claim 2, wherein: and conductive adhesive is filled between the metal wire and the groove.
4. The sample stage capable of carrying the micro-nano-scale sample according to claim 2, wherein: the groove is semi-cylindrical.
5. The sample stage capable of carrying the micro-nano-scale sample according to claim 1, wherein: and a right-angle notch is arranged on one edge of the base, which is close to the top end of the metal wire.
6. An in-situ testing method, comprising the steps of:
(1) cutting a micro-nano scale sample with a right-angled trapezoid cross section from the surface of a bulk sample by using a focused ion beam-scanning electron microscope dual-beam system, and keeping the connection of one side of the micro-nano scale sample and the bulk sample;
(2) combining the micro-nano scale sample with a built-in mechanical arm by using a micro-deposition welding technology, and cutting off the connection between the micro-nano scale sample and the bulk sample by using a focused ion beam;
(3) fixing the micro-nano scale sample on a plane at the top end of a metal wire clamped by a sample stage by using a micro-deposition welding technology, and cutting off the connection between the micro-nano scale sample and the mechanical arm by using a focused ion beam;
(4) taking the sample stage out of the scanning electron microscope, namely manually completing three-dimensional rotation outside a cabin of the scanning electron microscope, then placing the sample stage into the scanning electron microscope at different angles, cutting the micro-nano scale sample positioned at the top end of the metal wire by using a focused ion beam, and performing a preparation process of a micro-nano material complex structure required by mechanical testing;
(5) after the preparation is finished, clamping the sample stage on a micro mechanical tester, and aligning the top end surface of the metal wire by adjusting the position of the sample stage, so that a probe of the micro mechanical tester is exactly aligned with a complex structure acting point of the micro-nano scale sample;
(6) and then, the mechanical properties of the micro-nano scale sample under various stress conditions are tested under in-situ observation by operating the micro mechanical tester.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110596603.2A CN113325021A (en) | 2021-05-31 | 2021-05-31 | In-situ testing method and sample platform capable of carrying micro-nano-scale sample |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110596603.2A CN113325021A (en) | 2021-05-31 | 2021-05-31 | In-situ testing method and sample platform capable of carrying micro-nano-scale sample |
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| Publication Number | Publication Date |
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| CN113325021A true CN113325021A (en) | 2021-08-31 |
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| CN202110596603.2A Pending CN113325021A (en) | 2021-05-31 | 2021-05-31 | In-situ testing method and sample platform capable of carrying micro-nano-scale sample |
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| CN (1) | CN113325021A (en) |
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- 2021-05-31 CN CN202110596603.2A patent/CN113325021A/en active Pending
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