CN113447513A - Long-acting vacuum transfer sample stage for X-ray photoelectron spectrometer and transfer method - Google Patents
Long-acting vacuum transfer sample stage for X-ray photoelectron spectrometer and transfer method Download PDFInfo
- Publication number
- CN113447513A CN113447513A CN202110730216.3A CN202110730216A CN113447513A CN 113447513 A CN113447513 A CN 113447513A CN 202110730216 A CN202110730216 A CN 202110730216A CN 113447513 A CN113447513 A CN 113447513A
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- vacuum
- sample
- sample stage
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000001681 protective effect Effects 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000002390 adhesive tape Substances 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000012780 transparent material Substances 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
Images
Classifications
-
- 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
- G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
- G01N23/2273—Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]
-
- 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
Abstract
The invention relates to a long-acting vacuum sample transferring table and a transferring method for an X-ray photoelectron spectrometer, in particular to a long-acting vacuum sample transferring table and a transferring method for an electron spectrometer, aiming at solving the problems that the effective time for keeping the vacuum degree is short and the long-acting vacuum environment cannot be realized. The invention is used in the field of vacuum sample transfer.
Description
Technical Field
The invention relates to a sample transfer table and a transfer method for an electron energy spectrometer, in particular to a long-acting vacuum sample transfer table and a transfer method for an X-ray photoelectron spectrometer.
Background
At present, an X-ray photoelectron spectrometer is widely applied to various fields and used for analyzing the physicochemical characteristics of a tested sample, such as chemical composition, element state, work function and the like. However, the analysis depth of the x-ray photoelectron spectrometer is very thin (10 nm), when the sample is exposed to the atmosphere, the sample is polluted by the surrounding gas environment, the surface of the sample can adsorb pollutants such as oxygen, carbon and the like, and even the surface characteristics of the sample can be changed sharply.
Therefore, the in-situ detection without exposure to the atmospheric environment is applicable to almost all samples to be detected. However, for most tests, purchasing custom XPS equipment to implement in-situ testing is very expensive and inefficient.
At present, only a team related to the chemical institute of Chinese academy of sciences develops a semi-in-situ transfer sample stage, but the effective time for maintaining the vacuum degree is short (the leakage rate is high), and the long-acting vacuum environment cannot be realized, so that a transfer sample stage system for maintaining the long-acting high vacuum environment for an X-ray photoelectron spectrometer is urgently needed.
Disclosure of Invention
The invention aims to solve the problems that the effective time for keeping the vacuum degree is short and the long-acting vacuum environment cannot be realized in the prior art, and further provides a long-acting vacuum transfer sample table and a transfer method for an X-ray photoelectron spectrometer.
The technical scheme adopted by the invention for solving the problems is as follows:
the battery unit and the sample stage unit are fixedly mounted on the upper end face of the base, the protective cover is buckled on the base, and the battery unit is connected with the sample stage unit and supplies power to the sample stage unit.
The method is realized according to the following steps:
the method comprises the following steps: cleaning each part of the long-acting vacuum transfer sample table and ensuring that each part of the long-acting vacuum transfer sample is clean and has no obvious dust on the surface, placing a sample to be tested on a sample placing support, adhering the sample to be tested on the sample placing support by using a double-sided adhesive tape or a conductive adhesive tape, and ensuring that the battery unit and the sample table unit are fixedly arranged on the base;
step two: placing the long-acting vacuum transfer sample table in a glove box, wherein inert gas filled in the glove box is an atmosphere;
step three: starting a micro vacuum pump to perform vacuum pumping for 15 minutes, and ensuring that a cavity between a vacuum cover of the sample table unit and the sample placing support is in a stable vacuum state;
step four: covering the protective cover, and transferring the sample table unit out of the glove box;
step five: the vacuum of a sample introduction chamber of the X-ray photoelectron spectrometer is discharged, and a sample introduction chamber door is opened;
step six: the power of the long-acting vacuum transfer sample stage system is turned off, the transfer sample stage is quickly placed on the magnetic force transmission rod of the sample chamber,
step seven: and vacuumizing the sample chamber.
The invention has the beneficial effects that:
the sample stage unit 3 is used for protecting the sample stage and the battery unit from being damaged and polluted by the outside in the transferring process of the system. The battery pack unit is used for providing electric energy required by the micro vacuum pump on the sample platform. The sample stage unit is used for protecting the vacuum state of the sample and ensuring that the sample is prevented from being influenced by the outside air. The sample stage unit can be sleeved on the vacuum cover, is not easy to loosen from the vacuum cover after being tightly sleeved, and an iron patch is arranged at the top end of the lifting frame and used for automatically releasing the vacuum cover when being transferred to the XPS vacuum bin body. The micro vacuum pump is connected with the vacuum cover and is electrified to realize the vacuum pumping of the inner chamber of the vacuum cover, and the air release valve is fixed on the vacuum cover to realize the air release function under the atmospheric pressure; the vacuum cover limiting sleeve is matched with the vacuum cover base, so that the vacuum cover, the sealing rubber ring and the vacuum cover base are accurately positioned, the vacuum cover is stably pressed, a vacuum cavity is formed to be matched with the sealing rubber ring and the vacuum cover base for use, and the sealing rubber ring is positioned in an inner groove of the vacuum cover base; the sample placing support is used for placing a tested sample; the vacuum cover base is connected with the sample transferring table; and the sample transferring table can be placed on a magnetic force transmission rod of a sample chamber of the X-ray photoelectron spectrometer in the transferring process.
The invention can solve the problems that the effective time for keeping the vacuum degree is short and the long-acting vacuum environment can not be realized in the prior art, and further needs to provide a long-acting vacuum transfer sample stage and a transfer method for an X-ray photoelectron spectrometer.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
Fig. 2 is a schematic structural view of the sample stage unit 3 of the present invention.
Fig. 3 is a schematic view of the sample stage unit 3 according to the present invention before installation.
Fig. 4 is a schematic diagram of the cover-removing of a sample transfer table in a sample chamber of an X-ray photoelectron spectrometer, wherein a is a molecular pump, b is the sample chamber, c is an analyst, d is a magnetic force transmission rod, and f is a magnet.
Detailed Description
The first embodiment is as follows: the embodiment is described with reference to fig. 1 to fig. 3, and the long-acting vacuum transfer sample stage for an X-ray photoelectron spectrometer in the embodiment includes a protective cover 1, a battery unit 2, a sample stage unit 3 and a base 4, wherein the battery unit 2 and the sample stage unit 3 are fixedly mounted on the upper end surface of the base 4, the protective cover 1 is buckled on the base 4, and the battery unit 2 is connected with the sample stage unit 3 and supplies power to the sample stage unit 3.
The second embodiment is as follows: the long-acting vacuum transfer sample stage for the X-ray photoelectron spectrometer is described by combining the figures 1-3, the sample stage unit 3 comprises a self-suction lifting frame 5, a micro vacuum pump 6, a deflation valve 7, a vacuum cover locking nut 8, a vacuum cover 9, a sealing rubber ring 10, a sample placing support 11, a vacuum cover locking bolt 12 and a transfer sample stage 13, the sample placing support 11 is fixedly arranged on the transfer sample stage 13, the vacuum cover 9 and the sealing rubber ring 10 are arranged on the sample placing support 11, the vacuum cover 9 is pressed on the sealing rubber ring 10, the vacuum cover locking nut 8 is sleeved on the vacuum cover 9 and is in threaded connection with the sample placing support 11, the micro vacuum pump 6 and the deflation valve 7 are both arranged on the top end of the vacuum cover 9, the micro vacuum pump 6 and the deflation valve 7 are both communicated with the vacuum cover 9, the bottom end of the self-suction lifting frame 5 is fixedly arranged on the upper end face of the vacuum cover locking nut 8, the battery unit 2 is connected with the micro vacuum pump 6 and supplies power to the micro vacuum pump 6, and other methods are the same as those of the first embodiment.
The third concrete implementation mode: the long-acting vacuum transfer sample stage for the X-ray photoelectron spectrometer is described with reference to fig. 1 and 2, wherein an annular iron sheet is installed at the bottom edge of a vacuum cover 9, a top pressing plate of a vacuum cover locking nut 8 is pressed on the annular iron sheet of the vacuum cover 9, the vacuum cover locking nut 8 is in threaded connection with a sample placing support 11, and other methods are the same as those in the second embodiment.
The fourth concrete implementation mode: referring to fig. 1 and 2, the present embodiment is described, and the long-acting vacuum transfer sample stage for an X-ray photoelectron spectrometer according to the present embodiment is characterized in that a battery unit 2 and a sample stage unit 3 are fixedly mounted on a base 4 through a bolt connection. The other methods are the same as those in the first embodiment.
The fifth concrete implementation mode: referring to fig. 1 and 2, the long-acting vacuum transfer sample stage for an X-ray photoelectron spectrometer according to the present embodiment is described, in which a protective cover 1 is a cover body made of a transparent material, and the protective cover 1 is mounted on a base 4 in a sealing and buckling manner. The protective cover 1 is made of transparent acrylic material. The other methods are the same as those in the first embodiment.
The sixth specific implementation mode: the embodiment is described with reference to fig. 1 to 4, and the method for transferring the long-acting vacuum transfer sample stage for the X-ray photoelectron spectrometer is implemented according to the following steps:
the method comprises the following steps: cleaning each part of the long-acting vacuum transfer sample table, ensuring that each part of the long-acting vacuum transfer sample is clean and has no obvious dust on the surface, placing a sample to be tested on the sample placing support 11, adhering the sample to be tested on the sample placing support 11 by using a double-sided adhesive tape or a conductive adhesive tape, and ensuring that the battery unit 2 and the sample table unit 3 are fixedly arranged on the base 4;
step two: placing the long-acting vacuum transfer sample table in a glove box, wherein inert gas filled in the glove box is an atmosphere;
step three: starting the micro vacuum pump 6 to perform vacuum pumping for 15 minutes, and ensuring that a cavity between the vacuum cover 9 of the sample table unit 3 and the sample placing support 11 is in a stable vacuum state;
step four: covering the protective cover 1, and transferring the sample table unit 3 out of the glove box;
step five: the vacuum of a sample introduction chamber of the X-ray photoelectron spectrometer is discharged, and a sample introduction chamber door is opened;
step six: the power of the long-acting vacuum transfer sample stage system is turned off, the transfer sample stage is quickly placed on the magnetic force transmission rod of the sample chamber,
step seven: and vacuumizing the sample chamber.
Claims (6)
- The long-acting vacuum transfer sample stage for the X-ray photoelectron spectrometer is characterized in that: the device comprises a protective cover (1), a battery unit (2), a sample stage unit (3) and a base (4), wherein the battery unit (2) and the sample stage unit (3) are fixedly arranged on the upper end face of the base (4), the protective cover (1) is buckled on the base (4), and the battery unit (2) is connected with the sample stage unit (3) and supplies power to the sample stage unit (3).
- 2. The long-acting vacuum transfer sample stage for the X-ray photoelectron spectrometer of claim 1, which is characterized in that: the sample stage unit (3) comprises a self-suction lifting frame (5), a micro vacuum pump (6), an air release valve (7), a vacuum cover locking nut (8), a vacuum cover (9), a sealing rubber ring (10), a sample placing support (11), a vacuum cover locking bolt (12) and a transfer sample stage (13), the sample placing support (11) is fixedly arranged on the transfer sample stage (13), the vacuum cover (9) and the sealing rubber ring (10) are arranged on the sample placing support (11), the vacuum cover (9) is pressed on the sealing rubber ring (10), the vacuum cover locking nut (8) is sleeved on the vacuum cover (9) and is in threaded connection with the sample placing support (11), the micro vacuum pump (6) and the air release valve (7) are both arranged on the top end of the vacuum cover (9), the micro vacuum pump (6) and the air release valve (7) are both communicated with the vacuum cover (9), the bottom end of the self-suction lifting frame (5) is fixedly arranged on the upper end face of the vacuum cover locking nut (8), the battery unit (2) is connected with the micro vacuum pump (6) and supplies power to the micro vacuum pump (6).
- 3. The long-acting vacuum transfer sample stage for the X-ray photoelectron spectrometer of claim 2, wherein: an annular iron sheet is installed on the edge of the bottom end of the vacuum cover (9), a top pressure plate of a vacuum cover locking nut (8) is pressed on the annular iron sheet of the vacuum cover (9), and the vacuum cover locking nut (8) is in threaded connection with a sample placing support (11).
- 4. The long-acting vacuum transfer sample stage for the X-ray photoelectron spectrometer of claim 1, which is characterized in that: the battery unit (2) and the sample stage unit (3) are fixedly arranged on the base (4) through bolt connection.
- 5. The long-acting vacuum transfer sample stage for the X-ray photoelectron spectrometer of claim 1, which is characterized in that: the protective cover (1) is a cover body made of transparent materials, and the protective cover (1) is installed on the base (4) in a sealing and buckling mode.
- 6. A transfer method for long-acting vacuum transfer sample stage of X-ray photoelectron spectrometer as claimed in claim 1, 2, 3, 4 or 5, characterized by that: the method is realized according to the following steps:the method comprises the following steps: cleaning each part of the long-acting vacuum transfer sample table and ensuring the cleanness of each part of the long-acting vacuum transfer sample, placing a sample to be tested on a sample placing support (11), adhering the sample to be tested on the sample placing support (11) by using a double-sided adhesive tape or a conductive adhesive tape, and ensuring that the battery unit (2) and the sample table unit (3) are fixedly arranged on the base (4);step two: placing the long-acting vacuum transfer sample table in a glove box, wherein inert gas filled in the glove box is an atmosphere;step three: starting a micro vacuum pump (6) to perform vacuum pumping for 15 minutes, and ensuring that a cavity between a vacuum cover (9) of the sample table unit (3) and the sample placing support (11) is in a stable vacuum state;step four: covering the protective cover (1), and transferring the sample table unit (3) out of the glove box;step five: the vacuum of a sample introduction chamber of the X-ray photoelectron spectrometer is discharged, and a sample introduction chamber door is opened;step six: the power of the long-acting vacuum transfer sample stage system is turned off, the transfer sample stage is quickly placed on the magnetic force transmission rod of the sample chamber,step seven: and vacuumizing the sample chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110730216.3A CN113447513A (en) | 2021-06-29 | 2021-06-29 | Long-acting vacuum transfer sample stage for X-ray photoelectron spectrometer and transfer method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110730216.3A CN113447513A (en) | 2021-06-29 | 2021-06-29 | Long-acting vacuum transfer sample stage for X-ray photoelectron spectrometer and transfer method |
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| Publication Number | Publication Date |
|---|---|
| CN113447513A true CN113447513A (en) | 2021-09-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110730216.3A Pending CN113447513A (en) | 2021-06-29 | 2021-06-29 | Long-acting vacuum transfer sample stage for X-ray photoelectron spectrometer and transfer method |
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| CN (1) | CN113447513A (en) |
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|---|---|---|---|---|
| CN1514221A (en) * | 2002-12-31 | 2004-07-21 | 中国石油化工股份有限公司 | Rock sealing hydrocarbon extraction instrument |
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-
2021
- 2021-06-29 CN CN202110730216.3A patent/CN113447513A/en active Pending
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| CN206725477U (en) * | 2017-01-18 | 2017-12-08 | 中国科学院化学研究所 | A kind of sample transfer device of half in situ X-ray diffraction XPS Analysis instrument |
| WO2018209408A1 (en) * | 2017-05-19 | 2018-11-22 | University Of Tasmania | Device and method for interfacing two separation techniques |
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| US20210055534A1 (en) * | 2018-01-05 | 2021-02-25 | Hennyz B.V. | Vacuum transfer assembly |
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Application publication date: 20210928 |
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