CN113655078A - Sample vacuum preparation cavity - Google Patents
Sample vacuum preparation cavity Download PDFInfo
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- CN113655078A CN113655078A CN202110834673.7A CN202110834673A CN113655078A CN 113655078 A CN113655078 A CN 113655078A CN 202110834673 A CN202110834673 A CN 202110834673A CN 113655078 A CN113655078 A CN 113655078A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000012545 processing Methods 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims description 17
- 238000001704 evaporation Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 11
- 238000012544 monitoring process Methods 0.000 claims description 10
- 108010083687 Ion Pumps Proteins 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract description 7
- 239000010408 film Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000004 low energy electron diffraction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a sample vacuum preparation cavity which is integrally arranged on a supporting rack for bearing, and comprises a spherical cavity for processing a sample, wherein the lower end part of the spherical cavity is fixedly arranged on the upper end surface of the supporting rack, a plurality of connecting flange ports for connecting external equipment are formed in the spherical cavity, a high-low temperature sample table for bearing and cleaning the sample is arranged in the spherical cavity, the spherical cavity is respectively and fixedly connected with a high-low temperature sample frame for adjusting the position of the sample and a vacuum component for maintaining the vacuum in the cavity through the connecting flange ports, and the high-low temperature sample frame is connected with the high-low temperature sample table and can drive the high-low temperature sample frame to move in the spherical cavity. The invention meets the two use requirements of sample surface cleaning pretreatment and simple film growth on the premise of not additionally adding a pretreatment cavity and other equipment.
Description
Technical Field
The invention relates to sample preparation equipment, in particular to a vacuum sample preparation cavity, and belongs to the field of vacuum scientific research equipment.
Background
In various ultrahigh vacuum surface science experiments, because an experimental sample is often characterized by different detection modes (such as STM, XPS and the like), the sample needs to be pretreated after being subjected to ultrahigh vacuum sample transmission and before being characterized so as to achieve the purpose of cleaning. If this pretreatment step is omitted directly, the characterization parameters of the sample in the ultrahigh vacuum environment are directly affected because the sample is exposed to the atmosphere, and the sample is also outgassed in the ultrahigh vacuum environment, so that the vacuum degree is deteriorated. Therefore, in each experiment at the present stage, a sample pretreatment step before the start of the experiment is necessary, and the existence of the step greatly prolongs the experiment time.
In order to solve the above problems, shorten the working time and improve the working efficiency, researchers in the industry have tried to make a sample capable of both pretreatment and simple thin film growth in an ultra-high vacuum. It is now conventional to add separate pre-treatment chambers and growth chambers to the apparatus to meet the requirements, but this not only makes the system as a whole more bulky and complex, but also greatly increases the manufacturing cost of the apparatus.
In summary, how to provide a brand-new and reasonably designed sample vacuum preparation device based on the existing research can meet the two requirements of sample pretreatment and film growth without adding other components, and further overcome many defects in the prior art, which is a problem to be solved by the technical staff in the field.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides a vacuum sample preparation chamber, which comprises the following components.
The utility model provides a sample vacuum preparation chamber, wholly sets up on a support rack that is used for bearing the weight of the effect, includes a spherical cavity that is used for carrying out sample processing, spherical cavity's lower tip fixed set up in the up end of support rack, set up a plurality of flange mouths that are used for connecting external equipment on the spherical cavity, the inside high low temperature sample platform that is used for bearing and clean sample that is provided with of spherical cavity, spherical cavity passes through flange mouth difference fixedly connected with is used for adjusting the high low temperature sample frame of sample position and is used for maintaining the vacuum component of vacuum in the cavity, high low temperature sample frame with high low temperature sample platform is connected and can drive it and be in spherical cavity removes.
Preferably, a sample feeding cavity connecting port is further formed in the spherical cavity, and the spherical cavity is connected with external sample feeding equipment through the sample feeding cavity connecting port; and in the sample transfer process, the magnetic rod is used for grabbing the high-low temperature sample table through the sample injection cavity connecting port.
Preferably, a plurality of observation windows are further formed in the spherical cavity and used for observing the process that the magnetic rod grabs the high-low temperature sample stage through the sample feeding cavity connecting port in real time in the sample feeding process.
Preferably, the bottom of the spherical cavity is further connected with at least one reserved evaporation source flange port, the reserved evaporation source flange port is a CF35 flange port, and the spherical cavity is connected with an external evaporation source through the reserved evaporation source flange port; and under the action of the external evaporation source, the sample in the spherical cavity can be subjected to simple film growth.
Preferably, the vacuum assembly comprises a dry pump and a common molecular pump for performing vacuum pumping operation on the spherical cavity, and a sputtering ion pump for maintaining ultrahigh vacuum in the spherical cavity; the universal molecular pump is connected with the spherical cavity through an adapter tube and a gate valve, one end of the adapter tube is connected with the connecting flange port, the other end of the adapter tube is connected with the gate valve, the gate valve is a CF100 gate valve, the gate valve is connected with the universal molecular pump and can control the switching of the universal molecular pump, and the sputtering ion pump is fixedly connected to the middle section of the adapter tube.
Preferably, the vacuum assembly further comprises an ion gauge for reading the vacuum degree in the spherical cavity and a residual gas analyzer for monitoring residual gas in the spherical cavity, and the ion gauge and the residual gas analyzer are both connected with the spherical cavity through the connecting flange port.
Preferably, one of the connecting flange ports on the spherical cavity is a CF100 flange port, which can be connected with a low-energy electron diffractometer for monitoring the growth condition of the film on the sample in real time.
Preferably, a plurality of the connecting flange ports on the spherical cavity are CF35 flange ports which can be used as reserved flange ports for connecting external reaction equipment.
The advantages of the invention are mainly reflected in that:
the sample vacuum preparation cavity disclosed by the invention meets two use requirements of sample surface cleaning pretreatment and simple film growth on the premise of not additionally adding a pretreatment cavity and other equipment. In the scheme of the invention, the LEED can be used for monitoring the film growth process in real time, so that the use effect of the preparation cavity is further ensured.
By adopting the scheme of the invention, the vacuum environment of the test sample can be ensured to meet the experimental requirements, the experiment and time cost for transferring the sample among different chambers can be reduced to the maximum extent, and the sample can be processed more efficiently and more intuitively.
In addition, the invention also provides technical inspiration for the design, manufacture and use of other vacuum preparation equipment in the same field, and has high reference, use and popularization values.
The following detailed description of the embodiments of the present invention is provided in connection with the accompanying drawings for the purpose of facilitating understanding and understanding of the technical solutions of the present invention.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
fig. 2 is a schematic diagram of the center cross-sectional structure of the present invention.
Wherein: 1. A support stand; 2. a spherical cavity; 3. a high and low temperature sample stage; 4. a high and low temperature sample holder; 5. a sample feeding cavity connecting port; 6. an observation window; 7. reserving an evaporation source flange port; 8. a common molecular pump; 9. a sputter ion pump; 10. a gate valve; 11. an ion gauge; 12. a residual gas analyzer.
Detailed Description
As shown in fig. 1 to 2, the present invention discloses a sample preparation chamber with a simple structure and convenient for sample pretreatment, which is used for realizing surface cleaning pretreatment of a sample under an ultra-vacuum condition, and simultaneously, using an LEED (low energy electron diffraction instrument) to monitor the growth of a simple thin film in real time, and saving the time cost for sample treatment. The specific scheme is as follows.
The utility model provides a sample vacuum preparation chamber, wholly sets up on a support rack 1 that is used for playing the bearing effect, includes a spherical cavity 2 that is used for carrying out sample treatment, spherical cavity 2's lower tip fixed set up in support rack 1's up end, spherical cavity 2 is last to have seted up a plurality of flange mouths that are used for connecting external equipment, spherical cavity 2 inside is provided with a high low temperature sample platform 3 that is used for bearing and clean sample, spherical cavity 2 passes through flange mouth fixedly connected with respectively is used for adjusting high low temperature sample frame 4 of sample position and is used for maintaining the vacuous vacuum component in the cavity, high low temperature sample frame 4 with high low temperature sample platform 3 is connected and can drive it and be in remove in the spherical cavity 2.
The spherical cavity 2 is also provided with a sample feeding cavity connecting port 5, and the spherical cavity 2 is connected with external sample feeding equipment through the sample feeding cavity connecting port 5; in the transmission process of the sample, the magnetic rod is used for grabbing the high-low temperature sample table 3 through the sample feeding cavity connecting port 5.
In order to further facilitate the operation, a plurality of observation windows 6 are further arranged on the spherical cavity 2 and used for observing the process that the magnetic rod grabs the high-low temperature sample stage 3 through the sample injection cavity connecting port 5 in real time in the sample injection process.
The bottom of the spherical cavity 2 is also connected with at least one reserved evaporation source flange port 7, the reserved evaporation source flange port 7 is a CF35 flange port, and the spherical cavity 2 is connected with an external evaporation source through the reserved evaporation source flange port 7; under the action of the external evaporation source, the sample in the spherical cavity 2 can be subjected to simple film growth.
The vacuum assembly comprises a dry pump (not shown in the figure) and a common molecular pump 8 for performing vacuum pumping operation on the spherical cavity 2, and a sputtering ion pump 9 for maintaining ultrahigh vacuum in the cavity of the spherical cavity 2; the universal molecular pump 8 is connected with the spherical cavity 2 through an adapter tube and a gate valve 10, one end of the adapter tube is connected with the connecting flange port, the other end of the adapter tube is connected with the gate valve 10, the gate valve 10 is a CF100 gate valve which is connected with the universal molecular pump 8 and can control the opening and the closing of the universal molecular pump 10, and the sputtering ion pump 9 is fixedly connected to the middle section of the adapter tube.
The vacuum assembly further comprises an ion gauge 11 for reading the vacuum degree in the spherical cavity 2 and a Residual Gas Analyzer (RGA) 12 for monitoring residual gas in the spherical cavity 2, wherein the ion gauge 11 and the residual gas analyzer 12 are connected with the spherical cavity 2 through the connecting flange port.
One of the connection flange ports on the spherical cavity 2 is a CF100 flange port, which can be connected with a Low Energy Electron Diffractometer (LEED) for real-time monitoring of the growth condition of the film on the sample. In addition, the other one or more connecting flange ports on the spherical cavity 2 are CF35 flange ports which can be used as reserved flange ports for connecting external reaction equipment.
In the working process of the invention, the dry pump is required to be started firstly, the common molecular pump 8 is started after the dry pump is completely operated, and the sputtering ion pump 9 is started when the vacuum degree is 5.0-7.0 mbar. The entire system was then baked at a temperature of 150 degrees celsius for a time period exceeding 48 hours. After baking is finished, the sample is annealed and cleaned by using the high-low temperature sample stage 3, and then cooled by using liquid nitrogen. The residual gas analysis was performed in the chamber using the residual gas analyzer 12 to confirm the cleanliness of the interior of the chamber. Then, the evaporation source can be used for simple film growth of the sample, and a low-energy electron diffractometer is used for real-time monitoring. After the scheme of the invention is adopted, the parameter indexes of the whole preparation cavity can reach the vacuum degree of less than 5x10-10mbar and the leakage rate of less than 1x10-10 mbar.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, the high-low temperature sample table is utilized, and through the use of the four-axis high-low temperature sample table, the annealing treatment and the cleaning of the sample are realized, and the position of the sample can be adjusted at any time according to actual requirements;
(2) the ball cavity is specially designed, so that a sample can be cleaned, simple film growth can be realized, the integral integration level of the preparation cavity is greatly improved, and the integral size of the preparation cavity and the equipment manufacturing cost are reduced;
(3) in the scheme of the invention, the LEED can be used for monitoring in the growth process of the film so as to observe the condition of the film in real time and ensure the quality of the film.
In summary, the vacuum sample preparation chamber disclosed by the invention meets the two use requirements of sample surface cleaning pretreatment and simple thin film growth on the premise of not additionally adding a pretreatment chamber and other equipment. In the scheme of the invention, the LEED can be used for monitoring the film growth process in real time, so that the use effect of the preparation cavity is further ensured.
By adopting the scheme of the invention, the vacuum environment of the test sample can be ensured to meet the experimental requirements, the experiment and time cost for transferring the sample among different chambers can be reduced to the maximum extent, and the sample can be processed more efficiently and more intuitively.
In addition, the invention also provides technical inspiration for the design, manufacture and use of other vacuum preparation equipment in the same field, and has high reference, use and popularization values.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A sample vacuum preparation chamber is integrally arranged on a supporting rack (1) for bearing, and is characterized in that: including a spherical cavity (2) that is used for carrying out sample processing, the lower tip of spherical cavity (2) is fixed set up in the up end of support rack (1), set up a plurality of flange mouths that are used for connecting external equipment on spherical cavity (2), spherical cavity (2) inside is provided with one and is used for bearing and clean high low temperature sample platform (3) of sample, spherical cavity (2) pass through flange mouth difference fixedly connected with is used for adjusting high low temperature sample frame (4) of sample position and is used for maintaining the vacuum component of cavity internal vacuum, high low temperature sample frame (4) with high low temperature sample platform (3) are connected and can drive it and be in remove in spherical cavity (2).
2. The sample vacuum preparation chamber of claim 1, wherein: the spherical cavity (2) is also provided with a sample feeding cavity connecting port (5), and the spherical cavity (2) is connected with external sample feeding equipment through the sample feeding cavity connecting port (5); in the transmission process of the sample, the magnetic rod is used for grabbing the high-low temperature sample table (3) through the sample injection cavity connecting port (5).
3. The sample vacuum preparation chamber of claim 2, wherein: a plurality of observation windows (6) are further formed in the spherical cavity (2) and used for observing the process that the magnetic force rod is grabbed by the sample injection cavity connecting port (5) in real time in the sample injection process of the high-temperature and low-temperature sample table (3).
4. The sample vacuum preparation chamber of claim 1, wherein: the bottom of the spherical cavity (2) is also connected with at least one reserved evaporation source flange port (7), the reserved evaporation source flange port (7) is a CF35 flange port, and the spherical cavity (2) is connected with an external evaporation source through the reserved evaporation source flange port (7); under the action of the external evaporation source, the sample in the spherical cavity (2) can be subjected to simple film growth.
5. The sample vacuum preparation chamber of claim 1, wherein: the vacuum assembly comprises a dry pump and a common molecular pump (8) which are used for performing vacuum pumping operation on the spherical cavity (2), and a sputtering ion pump (9) which is used for maintaining ultrahigh vacuum in the cavity of the spherical cavity (2); the universal molecular pump (8) is connected with the spherical cavity (2) through an adapter tube and a gate valve (10), one end of the adapter tube is connected with the connecting flange port, the other end of the adapter tube is connected with the gate valve (10), the gate valve (10) is a CF100 gate valve which is connected with the universal molecular pump (8) and can control the opening and closing of the universal molecular pump, and the sputtering ion pump (9) is fixedly connected to the middle section of the adapter tube.
6. The sample vacuum preparation chamber of claim 5, wherein: the vacuum assembly further comprises an ion gauge (11) used for reading the vacuum degree in the spherical cavity (2) and a residual gas analyzer (12) used for monitoring residual gas in the spherical cavity (2), and the ion gauge (11) and the residual gas analyzer (12) are connected with the spherical cavity (2) through the connecting flange port.
7. The sample vacuum preparation chamber of claim 1, wherein: one of the connecting flange ports on the spherical cavity (2) is a CF100 flange port which can be connected with a low-energy electron diffractometer for monitoring the growth condition of a film on a sample in real time.
8. The sample vacuum preparation chamber of claim 1, wherein: the plurality of connecting flange ports on the spherical cavity (2) are CF35 flange ports which can be used as reserved flange ports and are used for connecting external reaction equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110834673.7A CN113655078A (en) | 2021-07-23 | 2021-07-23 | Sample vacuum preparation cavity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110834673.7A CN113655078A (en) | 2021-07-23 | 2021-07-23 | Sample vacuum preparation cavity |
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| Publication Number | Publication Date |
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| CN113655078A true CN113655078A (en) | 2021-11-16 |
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| CN202110834673.7A Pending CN113655078A (en) | 2021-07-23 | 2021-07-23 | Sample vacuum preparation cavity |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507845A (en) * | 2022-01-24 | 2022-05-17 | 仪晟科学仪器(嘉兴)有限公司 | Ultrahigh vacuum metal evaporation equipment and evaporation method thereof |
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| JP2000260325A (en) * | 1999-03-10 | 2000-09-22 | Canon Inc | Manufacture of image display device |
| CN2837831Y (en) * | 2005-11-11 | 2006-11-15 | 中国科学院物理研究所 | Ultra-high vacuum in-situ growth, characterization and test system |
| CN101846635A (en) * | 2010-05-07 | 2010-09-29 | 中国科学院半导体研究所 | Ultra-high vacuum multifunctional integrated test system |
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2021
- 2021-07-23 CN CN202110834673.7A patent/CN113655078A/en active Pending
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| JP2000260325A (en) * | 1999-03-10 | 2000-09-22 | Canon Inc | Manufacture of image display device |
| CN2837831Y (en) * | 2005-11-11 | 2006-11-15 | 中国科学院物理研究所 | Ultra-high vacuum in-situ growth, characterization and test system |
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| CN102928080A (en) * | 2012-10-30 | 2013-02-13 | 东南大学 | Method and device for testing hyperfine structure energy level of hydrogen atom |
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| Title |
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| 金懋昌编著: ""3.6.3 溅射离子泵的运用"，《真空技术》", vol. 1, 东南大学出版社, pages: 87 - 88 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114507845A (en) * | 2022-01-24 | 2022-05-17 | 仪晟科学仪器(嘉兴)有限公司 | Ultrahigh vacuum metal evaporation equipment and evaporation method thereof |
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