CN109883919B - Vacuum environment sample replacing device - Google Patents
Vacuum environment sample replacing device Download PDFInfo
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- CN109883919B CN109883919B CN201910147919.6A CN201910147919A CN109883919B CN 109883919 B CN109883919 B CN 109883919B CN 201910147919 A CN201910147919 A CN 201910147919A CN 109883919 B CN109883919 B CN 109883919B
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Abstract
The invention belongs to the field of vacuum analysis equipment and discloses a vacuum environment sample replacing device which comprises a sample replacing table, a valve seat and a sealing unit, wherein the sample replacing table is used for placing and replacing samples; a first reaction chamber in the valve seat is provided with a through hole for communicating with the first cavity and realizing the opening and closing of the first channel through the movement of the first valve core, a sample chamber is used for placing and replacing a sample table, a second reaction chamber is provided with a through hole for communicating with the second cavity and realizing the opening and closing of the second channel through the movement of the second valve core; the sealing unit is used for being matched with the valve seat to isolate the outside air. According to the invention, the sample can be replaced through the first valve core and the second valve core under the condition that the vacuum environment of the first chamber and the vacuum environment of the second chamber are not influenced, and the sample can be in a working environment by opening the first channel and the second channel after the sample is replaced, so that the time for recovering the working environment is saved.
Description
Technical Field
The invention belongs to the field of vacuum analysis equipment, and particularly relates to a sample replacing device in a vacuum environment.
Background
When the gas permeability of the film is tested by a mass spectrometry method or a pressure difference method, the film needs to be clamped and fixed, then the upper side and the lower side of the film are pumped to be in extremely high vacuum, and gas with constant pressure and permeability to be tested is introduced to the other side under the condition that one side is kept in extremely high vacuum; gas is adsorbed and dissolved on the surface of the film under the action of pressure difference and concentration difference, diffuses in the film and is desorbed when diffusing to the other side; the mass spectrometer or vacuum gauge on the side of the extreme high vacuum can capture the content change of the gas, and the permeability of the film to the gas is calculated according to the content change.
When the existing detection equipment is used for replacing a film sample, the upper side and the lower side of the film need to be forced to be raised to atmospheric pressure, then the equipment can be opened to replace the sample, at the moment, the equipment can be exposed in the atmospheric environment, and the inner wall can adsorb a large amount of air molecules and is not easy to be pumped away by a vacuum pump set. If water molecules are adsorbed on the inner wall of the equipment, the environment can not reach high vacuum due to long-time vacuum pumping, and auxiliary baking and other measures are needed, so that the problems of long testing time, low sample changing efficiency and high cost are caused.
Disclosure of Invention
In view of the above drawbacks or needs for improvement in the prior art, the present invention provides a vacuum environment sample replacement device, wherein devices such as a sample replacement device and a valve seat are correspondingly designed in combination with the characteristic that two sides of a sample are in a vacuum environment, and the structures and specific arrangement modes of key components thereof, such as a first reaction chamber and a second reaction chamber, are studied and designed, so that the problem of low sample replacement efficiency in a vacuum environment can be effectively solved, and the vacuum environment sample replacement device is particularly suitable for application occasions of sample replacement in a vacuum environment.
In order to achieve the above object, the present invention provides a vacuum environment sample replacing device, which is characterized in that the device comprises a sample replacing table, a valve seat and a sealing unit, wherein:
the sample changing table is used for placing and changing samples, and the sample changing table and the valve seat are matched with each other to isolate external air;
the valve seat comprises a first reaction chamber, a sample chamber and a second reaction chamber which are sequentially arranged from top to bottom along the vertical direction, wherein the first reaction chamber is provided with a through hole along the vertical direction for being communicated with the first chamber, the first reaction chamber is provided with a first channel along the horizontal direction, a first valve core with one stepped end penetrates through the first channel, and the first channel is opened and closed by moving along the horizontal direction; the sample chamber is used for placing the sample changing table and fixing the sample between the first reaction chamber and the second reaction chamber; the second reaction chamber is provided with a through hole along the vertical direction for communicating with the second chamber, a second channel is arranged along the horizontal direction in the second reaction chamber, a second valve core with one end in a step shape penetrates through the second channel, and the second channel is opened and closed through the movement of the second valve core along the horizontal direction;
the sealing unit is used for being matched with the valve seat to isolate the outside air.
Preferably, the sample changing table comprises a baffle, a handle and a sample table, wherein the baffle is provided with a through hole for fixing the baffle and the valve seat by using a fastener, the handle is fixed on one side of the baffle, the sample table is fixed on the other side of the baffle, a stepped hole is arranged in the middle of the sample table, the reticular support is arranged above the stepped hole for supporting the sample, and the pressing plate is fixed above the sample.
Further preferably, the sealing unit includes a first partition plate, a first bellows, a second partition plate, and a second bellows, wherein the first partition plate is connected to the first reaction chamber to isolate the first bellows from the atmospheric environment, one end of the first bellows is connected to the first valve body, and the other end thereof is connected to the first partition plate, the second partition plate is connected to the second reaction chamber to isolate the second bellows from the atmospheric environment, one end of the second bellows is connected to the second valve body, and the other end thereof is connected to the second partition plate.
Preferably, one side of the sample stage, which is connected with the baffle, is stepped, the baffle and the valve seat are sealed by a first sealing ring, and two sides of the sample stage and the valve seat are respectively sealed by a second sealing ring and a third sealing ring.
Preferably, the valve seat is provided with a first vacuum channel, and the first vacuum channel is connected with a mechanical pump to vacuumize or deflate the space between the first sealing ring and the second sealing ring.
Preferably, a second vacuum channel is arranged on the valve seat, and the second vacuum channel is connected with a mechanical pump to vacuumize or deflate the inside of the third sealing ring.
As a further preferred, two sides of the sample are respectively provided with a sealing ring for isolating the vacuum environment of the first reaction chamber and the second reaction chamber on two sides of the sample.
Preferably, the first valve core, the second valve core and the valve seat are sealed by sealing rings, so as to ensure the vacuum environment of the first chamber and the second chamber.
Further preferably, the first reaction chamber and the first partition plate are sealed by a sealing ring, and the second reaction chamber and the second partition plate are sealed by a sealing ring.
Preferably, the pressing plate is provided with a through hole for fixing with the sample stage by using a fastener.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. according to the invention, in the process of replacing the sample when the gas permeability of the sample is tested by a mass spectrometry method or a differential pressure method, the opening and closing of the first channel and the second channel can be realized by the horizontal movement of the first valve core and the second valve core, so that the sample can be replaced under the condition that the vacuum environment of the first chamber and the vacuum environment of the second chamber are not influenced, and the sample can be in a working environment by opening the first channel and the second channel after the sample is replaced, thereby saving the time for obtaining the working environment again;
2. meanwhile, the sealing rings are arranged on the two sides of the sample, so that the sample changing device can be used in working environments with different pressures of the first chamber and the second chamber, and the sample can be changed under the condition that the pressures of the first chamber and the second chamber are not influenced;
3. particularly, after the device provided by the invention is used for replacing a sample, better sealing performance can be obtained by vacuumizing between the first sealing ring and the second sealing ring, the influence of outside air on a system is avoided, and in addition, the sample is convenient to replace while the sealing performance is ensured through the first vacuumizing channel and the second vacuumizing channel;
4. in addition, the sample changing table can effectively clamp the sample, and the defects of deformation, edge air leakage and the like of the sample caused by pressure difference are avoided through the support of the net-shaped support, so that the gas molecules in the first chamber and the second chamber can only be exchanged through the sample.
Drawings
FIG. 1 is a schematic diagram of a sample exchange device under vacuum provided by a preferred embodiment of the present invention;
FIG. 2 is a schematic diagram of a sample changing station according to a preferred embodiment of the present invention;
FIG. 3 is a schematic view of the normal operation of the vacuum environment sample replacement device provided by the present invention;
FIG. 4 is a schematic view of a vacuum environment change sample device provided by the present invention in preparation for a change;
FIG. 5 is a schematic view of the present invention providing a vacuum environment for replacing a sample loading and replacing stage;
fig. 6 is a schematic view of an application environment of the vacuum environment replacement sample device provided by the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1, the present invention provides a vacuum environment changing sample device, which comprises a changing table 1, a valve seat 2 and a sealing unit, wherein:
the sample changing table 1 is used for placing and changing a sample 6, the sample changing table 1 and the valve seat 2 are matched with each other to isolate external air, and a proper sample changing table 1 can be selected according to the shape of the sample;
according to a preferred embodiment of the present invention, as shown in fig. 2, the sample changing table 1 comprises a baffle 13, a handle 3 and a sample table, wherein the baffle 13 is provided with a through hole for fixing the baffle 13 with the valve seat 2 by using a fastener such as a screw, the handle 3 is fixed on one side of the baffle 13 for facilitating the replacement of a sample, the sample table is fixed on the other side of the baffle 13, a stepped hole is arranged in the middle of the sample table, a net-shaped bracket is arranged above the stepped hole for supporting the sample 6, the deformation of the sample 6 can be effectively weakened even if the sample 6 has a pressure difference up and down, and a pressure plate 7 is fixed above the sample 6 for fixing and sealing the sample 6;
more specifically, the surface of the sample changing table 1 is polished, so that the sample changing table is convenient to take and place, the surface area of gas adsorption can be reduced, the pressure plate 7 is made of stainless steel and acts together with the sealing ring to compress and seal the sample 6, the reticular support 5 is made of stainless steel, and a porous structure is adopted to enable gas molecules to permeate the sample 6, so that the effective permeation area of the sample 6 is ensured;
the valve seat 2 comprises a first reaction chamber, a sample chamber and a second reaction chamber which are sequentially arranged from top to bottom along the vertical direction, wherein the first reaction chamber is provided with a through hole along the vertical direction for being communicated with the first chamber 17, the first reaction chamber is provided with a first channel along the horizontal direction, a first valve core 12 with one stepped end penetrates through the first channel, and the first channel is opened and closed by moving along the horizontal direction; the sample chamber is used for placing and replacing the sample platform 1 and fixing the sample 6 between the first reaction chamber and the second reaction chamber; a through hole is formed in the second reaction chamber along the vertical direction and is used for being communicated with the second chamber 18, a second channel is arranged in the second reaction chamber along the horizontal direction, a second valve core 12' with one end being in a step shape penetrates through the second channel, and the second channel is opened and closed through the movement of the second valve core along the horizontal direction;
the sealing unit is used for mutually matching with the valve seat 2 to isolate the outside air;
according to another preferred embodiment of the present invention, the sealing unit comprises a first partition 9, a first bellows 11, a second partition 9 ' and a second bellows 11 ', wherein the first partition 9 is connected to the first reaction chamber to isolate the first partition from the atmosphere, one end of the first bellows 11 is connected to the first valve core 12, the other end of the first bellows is connected to the first partition 9, the second partition is connected to the second reaction chamber to isolate the second partition from the atmosphere, one end of the second bellows 11 ' is connected to the second valve core 12 ', and the other end of the second bellows is connected to the second partition 9 ', therefore, the first bellows 11 and the second bellows 11 ' have the advantages of large expansion amount and good sealing effect, and thus not only can the first valve core 12 and the second valve core 12 ' be isolated from the outside air be ensured, but also they can expand and contract with the horizontal movement thereof.
Further, one side of the sample platform connected with the baffle 13 is preferably in a step shape, the baffle 13 and the valve seat 2 are sealed through a first sealing ring 14, two sides of the sample platform and the valve seat 2 are respectively sealed through a second sealing ring 15 and a third sealing ring 16, a first vacuumizing channel 4 is arranged on the valve seat 2, the first vacuumizing channel 4 is connected with a mechanical pump, vacuumizing or air bleeding is conducted between the first sealing ring 14 and the second sealing ring 15, good sealing performance is guaranteed, influence of outside air on the system is avoided, a second vacuumizing channel 10 is further arranged on the valve seat 2, the second vacuumizing channel 10 is connected with the mechanical pump, vacuumizing or air bleeding is conducted inside the third sealing ring 16, and the first sealing ring 14, the second sealing ring 15 and the third sealing ring 16 are preferably made of fluororubber.
Further, two sides of the sample 6 are respectively provided with a sealing ring for isolating the vacuum environment of the first reaction chamber and the second reaction chamber on two sides of the sample 6, and the sealing ring is preferably a fluorine rubber sealing ring.
Further, the first valve core 12, the second valve core 12' and the valve seat are sealed by sealing rings, preferably fluorine rubber sealing rings, to ensure the vacuum environment of the first chamber 17 and the second chamber 18.
Further, the first reaction chamber and the first partition plate 9 are sealed by a sealing ring, the second reaction chamber and the second partition plate 9 'are sealed by a sealing ring, so that the first valve core 12 and the second valve core 12' are convenient to replace, and the sealing ring is preferably a metal sealing ring.
Further, a through hole is provided on the pressing plate 7 for fixing with a sample stage using a fastener such as a screw.
As shown in fig. 3 to 5, the specific working steps of the sample changing device in vacuum environment provided by the present invention include:
(a) the first valve core 12 and the second valve core 12' are moved inwards along the horizontal direction to close the first through hole and the second through hole, and then air is discharged through the first vacuum-pumping channel 4 and the second vacuum-pumping channel 10 to enable the air pressure of the sample changing table 1 to be consistent with the outside;
(b) loosening the screws on the baffle 13, and moving the handle 3 to take out the sample changing table 1;
(c) screws on the pressing plate 7 are symmetrically unscrewed, the tested sample 6 is taken down after the pressing plate 7 is taken down, a new sample 6 is put on the sample, and then the pressing plate 7 is covered and the screws are symmetrically screwed down;
(d) the sample changing table 1 is placed in and screwed down on a screw on a baffle 13 by moving the handle 3, and a vacuum pump is used for vacuumizing through the first vacuumizing channel 4 and the second vacuumizing channel 10;
(e) finally, the first valve core 12 and the second valve core 12' are moved outwards along the horizontal direction, so that the first through hole and the second through hole are opened, and the test is carried out.
FIG. 6 is a schematic diagram of a vacuum environment sample replacing device applied to mass spectrometry for testing gas permeability of a thin film sample, a valve seat 2 is connected with a first chamber 17 and a second chamber 18 through CF35 flanges respectively at the upper and lower parts, the connection part is sealed by a metal sealing ring, and the first chamber 17 and the second chamber 18 are pumped to 10-7Torr～10-8Torr, the vacuum degree of the system is improved by auxiliary baking measures in the vacuumizing process, then detection gas (such as water vapor) is introduced into the first chamber 17, the pressure of the first chamber is accurately controlled to be 0-100.000 Torr by using a fine adjustment valve 19, the second chamber 18 keeps high vacuum unchanged, and the change of the content of the gas (such as water vapor) is monitored in real time by using a mass spectrometer (QMS)20 of the second chamber 18;
when the sample 6 needs to be replaced, the first valve core 12 and the second valve core 12' are moved to isolate the first chamber 17 and the second chamber 18, at this time, the first chamber 17 still maintains 0-100.000 Torr, and the second chamber 18 still maintains 10 Torr-7Torr～10-8Stopping vacuumizing operation on the first vacuumizing channel 4 and the second vacuumizing channel 10, changing to an operation of exhausting air into the vacuumizing operation, when the pressure of a gap between the sample changing table 1 and the valve seat 2 is consistent with the external atmosphere, unscrewing screws on the sample changing table 1, taking down the sample changing table 1 by the movable handle 3 on a dust-free operation table, taking down a pressing plate 7 after unscrewing the screws on the pressing plate 7, then taking down a sample 6, after checking that the state of a sealing ring is intact, horizontally placing a new sample 6 on the reticular support 5, pressing the sample 6 by the pressing plate 7, symmetrically screwing the screws, putting the sample changing table 1 into the valve seat 2 by the movable handle 3, and screwing the screws on the sample changing table 1;
the first vacuum-pumping channel 4 and the second vacuum-pumping channel 10 are vacuumized, and the first valve core 12 and the second valve core 12' are moved to open the first chamber 17 and the second chamber 18, at which time the sample 6 isThe upper side is in a gas of 0-100.000 Torr, and the lower side of the sample 6 is at 10 Torr-7Torr～10-8And when the pressure of Torr is higher and two layers of sealing protection are arranged between the sample 6 and the outside air, and one layer is a vacuum sealing layer, the gas molecules in the first chamber 17 and the second chamber 18 can only exchange through the sample 6, and the requirement of the equipment for testing the gas permeability of the thin film sample by mass spectrometry is met.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A vacuum environment change sample device, characterized in that the device comprises a sample changing station (1), a valve seat (2) and a sealing unit, wherein:
the sample changing table (1) is used for placing and changing samples (6), and the sample changing table (1) and the valve seat (2) are matched with each other to isolate external air;
the valve seat (2) comprises a first reaction chamber, a sample chamber and a second reaction chamber which are sequentially arranged from top to bottom along the vertical direction, wherein the first reaction chamber is provided with a through hole along the vertical direction for being communicated with a first cavity (17), the first reaction chamber is provided with a first channel along the horizontal direction, a first valve core (12) with one stepped end penetrates through the first channel, and the first channel is opened and closed by moving along the horizontal direction; the sample chamber is used for placing the sample changing table (1) and fixing the sample (6) between the first reaction chamber and the second reaction chamber; the second reaction chamber is provided with a through hole along the vertical direction for being communicated with a second chamber (18), a second channel is arranged along the horizontal direction, a second valve core (12') with one stepped end penetrates through the second channel, and the second channel is opened and closed through the movement of the second valve core along the horizontal direction;
the sealing unit is used for being matched with the valve seat (2) to isolate the outside air.
2. The vacuum environment sample replacing device according to claim 1, wherein the sample replacing table (1) comprises a baffle plate (13), a handle (3) and a sample table, wherein the baffle plate (13) is provided with a through hole for fixing the baffle plate (13) and a valve seat (2) by using a fastening piece, the handle (3) is fixed on one side of the baffle plate (13), the sample table is fixed on the other side of the baffle plate (13), a stepped hole is arranged in the middle of the sample table, a mesh bracket is arranged above the stepped hole for supporting the sample (6), and a pressing plate (7) is fixed above the sample (6).
3. The vacuum environment change sample device according to claim 1, wherein the sealing unit comprises a first diaphragm (9), a first bellows (11), a second diaphragm (9 ') and a second bellows (11 '), wherein the first diaphragm (9) is isolated from the atmosphere by being connected to the first reaction chamber, the first bellows (11) is connected to the first valve element (12) at one end and to the first diaphragm (9) at the other end, the second diaphragm is isolated from the atmosphere by being connected to the second reaction chamber, and the second bellows (11 ') is connected to the second valve element (12 ') at one end and to the second diaphragm (9 ') at the other end.
4. The vacuum environment sample replacing device according to claim 2, wherein the side of the sample stage connected with the baffle (13) is stepped, the baffle (13) and the valve seat (2) are sealed by a first sealing ring (14), and the two sides of the sample stage and the valve seat (2) are respectively sealed by a second sealing ring (15) and a third sealing ring (16).
5. Vacuum environment change-over sample device according to claim 4, characterized in that a first evacuation channel (4) is provided on the valve seat (2), which first evacuation channel (4) is connected to a mechanical pump for evacuating or venting the space between the first sealing ring (14) and the second sealing ring (15).
6. Vacuum environment change sample device according to claim 4, characterized in that a second evacuation channel (10) is provided on the valve seat (2), which second evacuation channel (10) is connected to a mechanical pump for evacuating or evacuating the interior of the third sealing ring (16).
7. The vacuum environment sample replacing device according to claim 1, wherein the two sides of the sample (6) are respectively provided with a sealing ring for isolating the vacuum environment of the first reaction chamber and the second reaction chamber on the two sides of the sample (6).
8. The vacuum environment sample replacing device according to any one of claims 1 to 7, characterized in that the first valve core (12), the second valve core (12') and the valve seat are sealed by sealing rings to ensure the vacuum environment of the first chamber (17) and the second chamber (18).
9. The vacuum environment change sample device according to claim 3, wherein the first reaction chamber is sealed from the first partition (9) by a sealing ring, and the second reaction chamber is sealed from the second partition (9') by a sealing ring.
10. Vacuum environment change-over-sample device according to claim 2, characterized in that the pressure plate (7) is provided with through-holes for fastening to a sample stage using fasteners.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910147919.6A CN109883919B (en) | 2019-02-28 | 2019-02-28 | Vacuum environment sample replacing device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910147919.6A CN109883919B (en) | 2019-02-28 | 2019-02-28 | Vacuum environment sample replacing device |
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| CN109883919A CN109883919A (en) | 2019-06-14 |
| CN109883919B true CN109883919B (en) | 2020-09-18 |
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| CN116626242B (en) * | 2023-06-06 | 2024-01-30 | 河北盛马电子科技有限公司 | Elevator type low-temperature vacuum sample replacing device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN200952588Y (en) * | 2006-07-17 | 2007-09-26 | 中国科学院近代物理研究所 | Mechanical safety valve for secondary vacuum system |
| JP2014149215A (en) * | 2013-01-31 | 2014-08-21 | National Institute Of Advanced Industrial & Technology | Gas permeability evaluation device |
| CN203892709U (en) * | 2014-03-25 | 2014-10-22 | 上海天马微电子有限公司 | Vacuum valve and vacuum pumping equipment |
| CN204389455U (en) * | 2014-12-08 | 2015-06-10 | 南京阿克赛斯科技有限公司 | Fully automatic vacuum infiltration degasser |
| CN106092827B (en) * | 2016-06-03 | 2019-04-23 | 沈阳大学 | A kind of the gas transfer diffusion coefficient measuring device and method of thin-film material |
| CN106525683B (en) * | 2016-10-27 | 2019-03-08 | 华中科技大学 | A kind of film permeation rate measuring device and measurement method |
| GB201702785D0 (en) * | 2017-02-21 | 2017-04-05 | Univ Liverpool | Gas sorption screening |
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