CN112630247A - Frozen sample platform of scanning electron microscope - Google Patents
Frozen sample platform of scanning electron microscope Download PDFInfo
- Publication number
- CN112630247A CN112630247A CN202011639710.0A CN202011639710A CN112630247A CN 112630247 A CN112630247 A CN 112630247A CN 202011639710 A CN202011639710 A CN 202011639710A CN 112630247 A CN112630247 A CN 112630247A
- Authority
- CN
- China
- Prior art keywords
- scanning electron
- electron microscope
- water cooling
- semiconductor
- frozen sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
Abstract
The invention discloses a scanning electron microscope frozen sample stage which comprises a water cooling stage, a semiconductor refrigeration piece and a sample carrying platform, wherein the semiconductor refrigeration piece is arranged on the water cooling stage, and a heat dissipation surface of the semiconductor refrigeration piece is attached to the surface of the water cooling stage; the sample carrying platform is arranged on the semiconductor refrigerating sheet, and the bottom surface of the sample carrying platform is attached to the refrigerating surface of the semiconductor refrigerating sheet. The frozen sample stage of the scanning electron microscope provided by the invention utilizes the refrigeration effect of the semiconductor refrigeration piece, and is miniaturized through reasonable structural design, so that the frozen sample stage can be placed below the scanning electron microscope to directly freeze a sample, and can provide a low temperature lower than-60 ℃, thereby meeting the low temperature requirement of the sample and simplifying experimental operation.
Description
Technical Field
The invention relates to the field of scanning electron microscopes, in particular to a frozen sample table of a scanning electron microscope.
Background
In the field of scanning electron microscopes, a high-pressure freezing method and a liquid nitrogen mud rapid freezing method are generally adopted for a scanning electron microscope frozen sample stage, a sample is inserted into a refrigerant, generally liquid nitrogen, and then is transferred to a cold stage of a sample preparation room of a frozen scanning electron microscope preparation system under vacuum, so that the experiment is complicated in operation, complex in structure and high in price.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a frozen sample stage for a scanning electron microscope, which can be placed under the scanning electron microscope to directly freeze the sample, so as to simplify the experimental operation.
In order to achieve the aim, the invention provides a scanning electron microscope frozen sample stage which comprises a water cooling stage, a semiconductor refrigeration piece and a sample carrying stage,
the semiconductor refrigeration piece is arranged on the water cooling table, and a heat dissipation surface of the semiconductor refrigeration piece is attached to the surface of the water cooling table;
the sample carrying platform is arranged on the semiconductor refrigerating sheet, and the bottom surface of the sample carrying platform is attached to the refrigerating surface of the semiconductor refrigerating sheet.
Furthermore, a temperature sensor is arranged between the bottom surface of the sample carrying platform and the refrigerating surface of the semiconductor refrigerating sheet, and the temperature sensor is attached to the bottom surface of the sample carrying platform.
Furthermore, the semiconductor refrigeration piece is of a multilayer structure, the area of the bottom layer of the semiconductor refrigeration piece and the bottom layer of the water cooling platform attaching surface is largest, then the area is gradually reduced upwards, and the size of the top layer of the semiconductor refrigeration piece is equivalent to that of the sample carrying platform; and between the layers of the semiconductor refrigerating sheets, the refrigerating surface of the next layer is attached to the radiating surface of the previous layer.
Furthermore, the water cooling platform adopts ethylene glycol as a water cooling medium.
Furthermore, a pipeline of the water cooling table is led out from the side edge of the frozen sample table.
Further, the frozen sample stage further comprises a water-cooling pedestal, the bottom surface and the side surface of the water-cooling stage are wrapped in the water-cooling pedestal, and a heat-insulating material is arranged in the water-cooling pedestal.
Furthermore, the frozen sample stage further comprises a shell for fixing the semiconductor refrigeration piece, the water cooling stage, the water cooling pedestal and the sample stage.
Furthermore, an aviation plug is arranged on the side of the shell and provides power supply connection for the semiconductor refrigeration piece.
Furthermore, the frozen sample stage further comprises a sample stage mounting seat, and the sample stage mounting seat is connected with the bottom of the shell.
The invention realizes the following technical effects: the frozen sample stage of the scanning electron microscope provided by the invention utilizes the refrigeration effect of the semiconductor refrigeration piece, and is miniaturized through reasonable structural design, so that the frozen sample stage can be placed below the scanning electron microscope to directly freeze a sample, and can provide a low temperature lower than-60 ℃, thereby meeting the low temperature requirement of the sample and simplifying experimental operation.
Drawings
FIG. 1 is a block diagram of a frozen sample stage according to a preferred embodiment of the present invention;
FIG. 2 is an expanded view of a frozen sample stage according to an embodiment of the present invention;
fig. 3 is a cross-sectional view of a frozen sample stage according to an embodiment of the present invention.
Detailed Description
To further illustrate the various embodiments, the invention provides the accompanying drawings. The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the embodiments. Those skilled in the art will appreciate still other possible embodiments and advantages of the present invention with reference to these figures. Elements in the figures are not drawn to scale and like reference numerals are generally used to indicate like elements.
The invention will now be further described with reference to the accompanying drawings and detailed description.
As shown in fig. 1-3, the invention discloses a specific embodiment of a frozen sample stage for a scanning electron microscope, which comprises a sample stage mounting base 1, a shell 2, an aviation socket 3, a water-cooling pedestal 4, a water-cooling stage 5, a semiconductor refrigeration sheet 6, a temperature sensor 7, a sample stage 8, a panel 9 and an upper cover 10.
Wherein, the shell 2, the panel 9 and the upper cover 10 form a shell of the scanning electron microscope frozen sample stage. The water-cooling pedestal 4 is sleeved inside the shell 2; the sample stage mounting seat 1 is connected with the water-cooling pedestal 4 below the shell 2 and fixes the shell 2 in the middle; the aviation plug 3 is arranged on the side edge of the shell 2 and used for supplying power to the semiconductor chilling plate 6; the water cooling table 5 is arranged in the water cooling table seat 4, the bottom surface and the periphery of the water cooling table seat are wrapped in the water cooling table seat 4, and the water cooling table seat 4 provides heat preservation and insulation measures for the water cooling table 5; the heat dissipation surface of the semiconductor refrigeration piece 6 is attached to the surface of the water cooling table 5, the temperature sensor 7 is fixed below the carrier 8, and the carrier 8 is attached to the refrigeration surface of the semiconductor refrigeration piece 6. The panel 9 is arranged on the water-cooling pedestal 4 and is matched with the water-cooling pedestal 4 to fix the positions of the sample carrier 8, the semiconductor refrigeration sheet 6 and the water-cooling platform 5. The upper cover 10 is mounted on the housing 2.
In this embodiment, semiconductor refrigeration piece 6 is multilayer structure, and the layer area of the contact with water cooling platform 5 is the biggest, then reduces step by step, and top layer and microscope carrier 8 laminating.
The working principle is as follows:
the semiconductor refrigerating sheet 6 utilizes the Peltier effect of semiconductor materials, when direct current passes through a couple formed by connecting two different semiconductor materials in series, heat can be absorbed and released at two ends of the couple respectively, and the purpose of refrigeration can be achieved.
Under certain conditions, the temperature difference between two ends of the couple of the semiconductor refrigerating sheet can reach 200 ℃ (the temperature range is-130 ℃ plus 90 ℃); the temperature difference between the refrigerating surface and the radiating surface of the semiconductor refrigerating sheet 6 can achieve the effect of ultra-low temperature sample freezing.
In this embodiment, the cooling surface of the semiconductor chilling plate 6 is cooled by the water cooling table 5, so as to ensure the stable long-time operation of the semiconductor chilling plate 6. In order to ensure the heat dissipation effect, glycol with the temperature of minus 10 ℃ or lower is introduced into the water cooling table 5.
In this embodiment, the semiconductor cooling plate 6 has a multilayer structure, which can provide sufficient cooling capacity and concentrate the cooling area on the sample carrier 8, and can realize accurate temperature control by controlling the layered power of the semiconductor cooling plate 6. Meanwhile, the semiconductor refrigerating sheet 6 is of a multilayer structure and can have high refrigerating efficiency, and the size of the frozen sample stage can be reduced as far as possible by combining the low-temperature water cooling stage 5 using ethylene glycol as a medium, so that the size of the frozen sample stage meets the requirement of application below a scanning electron microscope.
In this application, the minimum refrigeration temperature required for the sample is-60 ℃. And the refrigerating speed of the semiconductor refrigerating sheet is higher, and the required temperature can be reached within a few seconds according to the temperature control requirement of the application. Therefore, in the application, the semiconductor refrigeration piece, especially the multilayer refrigeration piece is adopted, so that the requirement of sample refrigeration of the application can be met.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. The utility model provides a frozen sample platform of scanning electron microscope which characterized in that: the semiconductor refrigeration piece is arranged on the water cooling table, and a heat dissipation surface of the semiconductor refrigeration piece is attached to the surface of the water cooling table; the sample carrying platform is arranged on the semiconductor refrigerating sheet, and the bottom surface of the sample carrying platform is attached to the refrigerating surface of the semiconductor refrigerating sheet.
2. The scanning electron microscope frozen sample stage according to claim 1, characterized in that: and a temperature sensor is arranged between the bottom surface of the sample carrying platform and the refrigerating surface of the semiconductor refrigerating sheet, and the temperature sensor is attached to the bottom surface of the sample carrying platform.
3. The scanning electron microscope frozen sample stage according to claim 1, characterized in that: the semiconductor refrigeration piece is of a multilayer structure, the area of the bottom layer, attached to the water cooling platform, of the semiconductor refrigeration piece is largest, then the area of the bottom layer is reduced upwards step by step, and the sizes of the top layer of the semiconductor refrigeration piece and the sample carrying platform are equivalent; and between the layers of the semiconductor refrigerating sheets, the refrigerating surface of the next layer is attached to the radiating surface of the previous layer.
4. The scanning electron microscope frozen sample stage according to claim 1, characterized in that: the water cooling platform is a water cooling platform adopting ethylene glycol as a water cooling medium.
5. The scanning electron microscope frozen sample stage according to claim 1, characterized in that: the frozen sample stage further comprises a water-cooling pedestal, the bottom surface and the side surface of the water-cooling stage are wrapped in the water-cooling pedestal, and a heat-insulating material is arranged in the water-cooling pedestal.
6. The scanning electron microscope frozen sample stage according to claim 1, characterized in that: the frozen sample stage further comprises a shell, the semiconductor refrigerating sheet, the water cooling stage and the water cooling pedestal are arranged in the shell, and the sample stage is arranged on a panel of the shell.
7. The scanning electron microscope frozen sample stage according to claim 6, characterized in that: the freezing sample platform still is provided with the circular connector, the circular connector set up in the side of casing for provide the power supply connection of semiconductor refrigeration piece.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011639710.0A CN112630247A (en) | 2020-12-31 | 2020-12-31 | Frozen sample platform of scanning electron microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011639710.0A CN112630247A (en) | 2020-12-31 | 2020-12-31 | Frozen sample platform of scanning electron microscope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112630247A true CN112630247A (en) | 2021-04-09 |
Family
ID=75290169
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011639710.0A Pending CN112630247A (en) | 2020-12-31 | 2020-12-31 | Frozen sample platform of scanning electron microscope |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112630247A (en) |
-
2020
- 2020-12-31 CN CN202011639710.0A patent/CN112630247A/en active Pending
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