CN112505335A - Ultrahigh vacuum sample transfer equipment and method - Google Patents
Ultrahigh vacuum sample transfer equipment and method Download PDFInfo
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- CN112505335A CN112505335A CN201910871823.4A CN201910871823A CN112505335A CN 112505335 A CN112505335 A CN 112505335A CN 201910871823 A CN201910871823 A CN 201910871823A CN 112505335 A CN112505335 A CN 112505335A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
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Abstract
The invention discloses ultrahigh vacuum sample transfer equipment and a transfer method, and belongs to the technical field of material testing. The transfer device comprises a transfer main body and an auxiliary device, wherein the transfer main body comprises a sample chamber for placing a sample and a vacuum device, and a first valve and a second valve are respectively arranged at two ends of the sample chamber; the auxiliary device comprises a corrugated pipe, a sample transfer device and a cooling device, one end of the corrugated pipe is communicated with the sample transfer device, the other end of the corrugated pipe is communicated or disconnected with the sample introduction chamber through a first valve, the sample transfer device can grab a sample in the sample introduction chamber and send the sample to the target chamber, the cooling device can be communicated or disconnected with the sample introduction chamber through a second valve simultaneously, the cooling device is communicated with the target chamber and communicated with the mobile pump set through a third valve, and the cooling device is provided with a liquid injection port and a vent port. The main body and the cooling device can be transported separately, the liquid nitrogen can be circulated in the cooling device and can be reduced to the temperature of the liquid nitrogen, the water vapor is adsorbed on the inner wall, and the sample is not polluted in the transfer process.
Description
Technical Field
The invention relates to the technical field of material testing, in particular to ultrahigh vacuum sample transfer equipment and a method for transferring a sample by using the same.
Background
An ultrahigh vacuum equipment system is an indispensable important hardware basis in performing ultrahigh vacuum experiments, and is generally formed by combining a vacuum pump, a vacuum gauge, a vacuum cavity and other elements according to certain requirements by means of a vacuum pipeline. The method ensures that a specific ultrahigh vacuum environment (the typical vacuum degree is better than 10E-10mbar) is obtained and maintained in a certain space, ensures that a certain process or physical process is implemented in a vacuum system, and has wide application in various research fields of semiconductors, machining, physics, chemistry, materials, bioscience and the like.
After the sample is prepared in the ultra-high vacuum system, it is usually tested and analyzed in an environment without destroying the ultra-high vacuum in order to ensure the stable properties of the sample. At present, the sample preparation and testing equipment can be integrated into an ultra-high vacuum system, and the system generally comprises a manipulator which can be used for transferring a sample at a certain specific position in a chamber, so that the sample preparation and the sample testing are completed in the same ultra-high vacuum environment. However, the testing equipment required in one set of equipment is limited, and to analyze the properties of the sample more comprehensively, the sample has to be taken out from a certain vacuum system and transferred to other ultrahigh vacuum systems for testing and analysis, and the process inevitably contacts air and dust to cause the pollution of the sample.
At present, several methods can protect a sample, for example, inert gas is introduced into a vacuum cavity to be used as protective gas, and then the sample is taken out and is rapidly placed into a clean sample box or a vacuum box; or plating a protective film on the sample and taking out the sample. However, most of them are complicated to operate, and each method cannot avoid the operation of "open cavity sampling" in which the sample is exposed to a non-vacuum gas atmosphere. Once the vacuum environment around the sample is broken, the gas is adsorbed to the surface of the sample, and the sample is polluted to some extent.
In view of the above problems, related ultra-high vacuum sample transfer devices have appeared in the industry, but besides the problem of high manufacturing cost of the device, there still exist many problems in the using process, such as: the vacuum degree of the whole equipment is difficult to ensure. Long-distance transportation is inconvenient, and the ultrahigh vacuum degree cannot be maintained for a long time. The middle interface needs to be baked in the process of transferring the sample from the transfer cavity to the vacuum cavity, heat can be transferred to transfer equipment in the baking process, the vacuum degree can be reduced by more than two orders of magnitude, the sample can not be ensured to be always in an ultrahigh vacuum environment, and the requirement of ultrahigh vacuum (1E-10mbar) can not be met.
Therefore, there is a need for an ultra-high vacuum sample transferring apparatus and transferring method, which can solve the problem of the vacuum degree of the transferring apparatus becoming poor during the baking process.
Disclosure of Invention
The invention aims to provide an ultrahigh vacuum sample transfer device and a transfer method, which are used for ensuring that a sample is always in an ultrahigh vacuum environment in the processes of storage, transportation and transfer and the sample is not polluted.
In order to realize the purpose, the following technical scheme is provided:
the invention provides an ultrahigh vacuum sample transfer device, comprising:
the transfer main body comprises a sample chamber for placing a sample and a vacuum device for vacuumizing the sample chamber, wherein a first valve and a second valve are respectively arranged at two ends of the sample chamber;
auxiliary device, including bellows, biography appearance device and cooling device, the one end of bellows with pass the appearance device intercommunication, the other end with the sampling room passes through first valve intercommunication or disconnection, pass the appearance device can snatch in the sample room sample and deliver to the target cavity, cooling device can simultaneously with the sampling room passes through second valve intercommunication or disconnection, with the target cavity intercommunication passes through the third valve intercommunication with the mobile pump package, cooling device is provided with notes liquid mouth and drain.
Further, the appearance room of advancing includes the main cavity room and stretches into advance kind platform in the main cavity room, advance kind platform and be used for depositing the sample, advance kind platform can reciprocate in the main cavity room.
Furthermore, the corrugated pipe is externally provided with three adjusting screws along the axial direction of the corrugated pipe, and the three adjusting screws can selectively adjust the axial direction of the corrugated pipe.
Furthermore, the auxiliary device also comprises a tee joint, and the tee joint is respectively connected with the corrugated pipe, one end of the sampling chamber and the vacuum equipment.
Furthermore, the cooling device is a cold trap, and the cold trap is provided with two ports, namely a liquid nitrogen injection port and a vent port.
Further, the first valve, the second valve and the third valve are hand valves.
Further, the vacuum device comprises an adsorption pump and an ion pump, the adsorption pump is communicated with the sample chamber, and the ion pump is communicated with the adsorption pump.
Furthermore, the sample transfer device comprises a magnetic rod extending into the sample chamber from the outside of the sample chamber, and the magnetic rod can clamp the sample in the sample chamber and control the movement and rotation of the sample.
The invention also provides a method for transferring a sample by using the ultrahigh vacuum sample transfer device, which comprises the following steps:
s1, opening the first valve, closing the second valve, and vacuumizing the sample chamber, the corrugated pipe and the sample transfer device by using a vacuum device;
s2, connecting the cooling device to the second valve of the sample chamber;
s3, vacuumizing the cooling device by using the movable pump group, introducing liquid nitrogen into a liquid injection port of the cooling device, and opening a vent port of the cooling device to allow the liquid nitrogen to circulate in the cooling device;
s4, after the cooling device is cooled to the temperature of liquid nitrogen, closing a third valve, communicating the cooling device with the target chamber, and vacuumizing the target chamber and the cooling device to 10E-10 mbar;
s5, opening the second valve, adjusting the corrugated pipe, enabling the sample transfer device to enter the sample introduction chamber for sampling, adjusting the corrugated pipe again, and pushing the sample to the target chamber by the sample transfer device;
and S6, after the process is finished, cutting off the communication between the cooling device and the target chamber, closing the second valve, and detaching the cooling device after the liquid nitrogen is evaporated.
Further, the ultra-high vacuum sample transfer method further comprises the following steps:
and after the cooling device is cooled to the liquid nitrogen temperature, wrapping the cooling device by using a heat insulating material.
Compared with the prior art, the ultra-high vacuum sample transfer equipment provided by the invention has the advantages that the transfer main body and the sample transfer device are always connected, the sample can be kept in the ultra-high vacuum environment of 1E-10mbar in the sample injection chamber, and the time for re-vacuumizing in each use is saved. The main body is detachably connected with the cooling device, the main body can be transported separately during transportation, the space is saved, the cooling device can be exposed in the atmosphere, the requirements on storage and transportation conditions are low, and the storage and transportation are facilitated. When the sample feeding device is used for connection, the free end of the sample feeding chamber is communicated with the cooling device through the second valve, the cooling device and the mobile pump set are communicated for vacuumizing, liquid nitrogen is communicated in the cooling device, the temperature in the cooling device is reduced to the temperature of the liquid nitrogen, water vapor in the cooling device is adsorbed on the inner wall, and the sample is not polluted in the transfer process.
When the ultrahigh vacuum sample transfer method is used, the cooling device is connected to the second valve of the transfer main body, then the cooling device is vacuumized, and meanwhile, liquid nitrogen flows through the inside of the cooling device, so that the temperature inside the cooling device is reduced to the temperature of the liquid nitrogen, water vapor inside the cooling device is adsorbed on the inner wall, and the sample is prevented from being polluted in the transfer process.
Drawings
FIG. 1 is a schematic diagram of an ultra-high vacuum sample transfer apparatus in an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a transfer body according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a bellows according to an embodiment of the present invention;
fig. 4 is a schematic structural diagram of a cold trap in an embodiment of the present invention.
Reference numerals: 1-a main chamber; 2-an adsorption pump; 3-an ion pump; 4-a first valve; 5-a second valve; 6-a sample introduction table; 7-magnetic pole; 8-a bellows; 801-adjusting screw; 9-a tee joint; 10-a cooling device; 1001-liquid injection port; 1002-a vent; 11-third valve.
Detailed Description
In order to make the technical problems solved, technical solutions adopted and technical effects achieved by the present invention clearer, the technical solutions of the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the present embodiment provides an ultrahigh vacuum sample transfer apparatus, which includes a transfer main body and an auxiliary device, wherein the transfer main body includes a sample chamber for placing a sample and a vacuum device for evacuating the sample chamber, and a first valve 4 and a second valve 5 are respectively installed at two ends of the sample chamber; the auxiliary device comprises a corrugated pipe 8, a sample transfer device and a cooling device 10, one end of the corrugated pipe 8 is communicated with the sample transfer device, the other end of the corrugated pipe is communicated or disconnected with a sample introduction chamber through a first valve 4, the sample transfer device can grab samples in the sample introduction chamber and send the samples to a target chamber, the cooling device 10 can be communicated or disconnected with the sample introduction chamber through a second valve 5, the cooling device is communicated with the target chamber and a mobile pump set through a third valve 11, and the cooling device 10 is provided with a liquid injection port 1001 and a vent port 1002.
The transfer main part and the sample transmission device of the ultrahigh vacuum sample transfer equipment are always connected, and the sample can keep an ultrahigh vacuum environment of 1E-10mbar in the sample injection chamber, so that the time for vacuumizing again in each use is saved. The main transfer body is detachably connected with the cooling device 10, the main transfer body can be transported separately during transportation, the space is saved, the cooling device 10 can be exposed in the atmosphere, the requirements on storage and transportation conditions are low, and the storage and transportation are facilitated. When the sample collection device is used for connection, the free end of the sample inlet chamber is communicated with the cooling device 10 through the second valve 5, the cooling device 10 and the mobile pump set are communicated and vacuumized, liquid nitrogen is communicated in the cooling device 10, the temperature in the cooling device 10 is reduced to the temperature of the liquid nitrogen, water vapor in the cooling device 10 is adsorbed on the inner wall, and therefore the sample is not polluted in the transfer process.
Specifically, as shown in fig. 2, the sample introduction chamber comprises a main chamber 1 and a sample introduction table 6 extending into the main chamber 1, the sample introduction table 6 is used for storing samples and storing 5 flag-type sample holders, and the sample introduction table 6 can move up and down in the main chamber 1, specifically, the sample introduction table 6 can move up and down by rotating an operation rod. As shown in fig. 1, the sample transfer device includes a magnetic rod 7 extending into the main chamber 1 from the outside of the main chamber 1, the magnetic rod 7 can clamp the sample in the main chamber 1 and control the sample to move and rotate, so as to realize the grabbing and parking of the sample on the sample introduction table 6 and transfer the sample to the target chamber.
Further, as shown in fig. 3, three adjusting screws 801 are respectively arranged outside the bellows 8 along the axial direction thereof, and the three adjusting screws 801 can selectively adjust the axial direction of the corresponding bellows 8, so as to achieve fine adjustment of the axial direction of the magnetic rod 7. Specifically, firstly, the adjusting screw 801 on the corrugated pipe 8 is adjusted, so that the sampling head at the end of the magnetic rod 7 can smoothly grab the sample in the main chamber 1; the adjustment screw 801 on the bellows 8 is adjusted again so that the magnetic rod 7 can smoothly transfer the grasped sample to the target chamber.
In this embodiment, the main chamber 1 adopts a spherical chamber structure, and two sides are respectively provided with an observation window, so that the sample can be conveniently transferred and observed.
Furthermore, the auxiliary device also comprises a tee joint 9, wherein the tee joint 9 is respectively connected with the corrugated pipe 8, one end of the sampling chamber and the vacuum equipment. The tee joint 9 can realize vacuum pumping of the magnetic rod 7 mainly when the magnetic rod 7 is partially atmospheric.
Preferably, the cooling device 10 in this embodiment is a cold trap, which connects the main chamber 1 and the target chamber, and one of the interfaces can be connected with the mobile pump group. As shown in fig. 4, the cold trap is further provided with two ports, namely a liquid nitrogen injection port 1001 and a vent port 1002, and the cold trap is cooled by injecting liquid nitrogen into the liquid injection port 1001. The third valve 11 blocks the opening of the main chamber 1 and the moving pump group after the start of cooling. In the present embodiment, the first valve 4, the second valve 5, and the third valve 11 are preferably hand valves. Wherein, by dismounting the side part of the second valve 5, the hyper-transfer body, the bellows 8 and the magnetic rod 7 are separated from the cooling device 10, and the carrying and the transportation are convenient. First valve 4 is the on-state under the normal condition, and magnetic rod 7 and main cavity 1 remain the super vacuum state all the time, but if expose atmosphere with magnetic rod 7, need close first valve 4 this moment, use vacuum apparatus to carry out the evacuation to main cavity 1, also need the evacuation to magnetic rod 7 to need toast magnetic rod 7 simultaneously when main cavity 1 does not have the sample, guarantee that the sample does not have the pollution.
Optionally, the vacuum device comprises an adsorption pump 2 and an ion pump 3, the adsorption pump 2 is communicated with the main chamber 1, and the ion pump 3 is communicated with the adsorption pump 2. The sorption pump 2 maintains a vacuum, typically around 1E-10mbar, in the main chamber 1, mainly by chemical reaction of rare metals in combination with air. The ion pump 3 can be vacuumized after being electrified, and the vacuum degree of the main chamber 1 can be displayed at the same time.
The invention also provides a method for transferring a sample by using the ultrahigh vacuum sample transfer equipment, which comprises the following steps:
s1, opening the first valve 4, closing the second valve 5, and vacuumizing the main chamber 1, the corrugated pipe 8 and the magnetic rod 7 by using the adsorption pump 2 and the ion pump 3;
s2, connecting the cold trap to the second valve 5 of the main chamber 1;
s3, connecting a mobile pump set to a third valve 11, vacuumizing the cold trap by using the mobile pump set, wherein the vacuumizing can be normally carried out to 10E-7mbar and can reach 10E-8mbar, introducing liquid nitrogen into a liquid injection port 1001 of the cold trap, and opening a vent port 1002 of the cold trap to enable the liquid nitrogen to circulate in the cold trap;
and S4, after the cold trap is cooled to the temperature of liquid nitrogen, wrapping the cold trap by using a heat insulating material to prevent an operator from being frostbitten. Then closing the third valve 11, communicating the cold trap with the target chamber, and vacuumizing the target chamber and the cold trap to 10E-10mbar by using the ion pump 3 and the titanium pump in the target chamber;
s5, opening the second valve 5, adjusting the corrugated pipe 8, enabling the magnetic rod 7 to enter the main chamber 1 for sampling, adjusting the corrugated pipe 8 again, and pushing the sample to the target chamber by the magnetic rod 7;
s6, after the process is completed, taking out the sample, placing the sample on a sample injection platform 6, cutting off the communication between the cold trap and the target chamber, closing the second valve 5, keeping the main chamber 1 and the magnetic rod 7 in ultrahigh vacuum, breaking the atmosphere of the cold trap after the liquid nitrogen is evaporated, and then detaching the cold trap.
When the sample baking device is used, if the magnetic rod 7 is exposed to the atmosphere, the first valve 4 must be closed first, the adsorption pump 2 and the ion pump 3 are used for vacuumizing the main chamber 1, and the magnetic rod 7 and the tee joint 9 are baked when no sample exists in the main chamber 1, so that no pollution is caused to the sample, the baking temperature is 100-. Naturally cooling to room temperature after baking, and then performing other operations.
In the ultra-high vacuum sample transfer method provided by this embodiment, the transfer main body and the sample transfer device are always connected, and the ultra-high vacuum state is maintained, and the transfer main body and the sample transfer device are detachable from the cooling device 10 and can be separately transported. When the vacuum liquid cooling device is used, the cooling device 10 is connected to the second valve 5 of the transfer main body firstly, then the cooling device 10 is vacuumized, and meanwhile liquid nitrogen flows through the inside of the cooling device 10, so that the temperature inside the cooling device 10 is reduced to the temperature of the liquid nitrogen, water vapor inside the cooling device 10 is adsorbed on the inner wall, and a sample is not polluted in the transfer process.
It is to be noted that the foregoing is only illustrative of the preferred embodiments of the present invention and the technical principles employed. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.
Claims (10)
1. An ultra-high vacuum sample transfer apparatus, comprising:
the transfer main body comprises a sample chamber for placing a sample and a vacuum device for vacuumizing the sample chamber, wherein a first valve (4) and a second valve (5) are respectively arranged at two ends of the sample chamber;
auxiliary device, including bellows (8), biography appearance device and cooling device (10), the one end of bellows (8) with pass appearance device intercommunication, the other end with the introduction room passes through first valve (4) intercommunication or disconnection, pass appearance device can snatch in the sample introduction room sample and deliver to the target cavity, cooling device (10) can simultaneously with the introduction room passes through second valve (5) intercommunication or disconnection, with the target cavity intercommunication passes through third valve (11) intercommunication with the removal pump package, cooling device (10) are provided with annotates liquid mouth (1001) and vent hole (1002).
2. The ultra-high vacuum sample transfer device according to claim 1, wherein the sample chamber comprises a main chamber (1) and a sample stage (6) extending into the main chamber (1), the sample stage (6) being used for storing samples, the sample stage (6) being movable up and down within the main chamber (1).
3. The ultra-high vacuum sample transfer apparatus according to claim 1, wherein the bellows (8) is provided with three adjusting screws (801) on the outside along the axial direction thereof, and the three adjusting screws (801) can selectively adjust the axial direction of the bellows (8).
4. Ultra-high vacuum sample transfer device according to claim 1, wherein the auxiliary means further comprises a tee (9), said tee (9) connecting the bellows (8), one end of the sample chamber and the vacuum device, respectively.
5. The ultra-high vacuum sample transfer device according to claim 4, wherein the cooling means (10) is a cold trap having two ports, respectively a liquid nitrogen injection port (1001) and a vent port (1002).
6. The ultra-high vacuum sample transfer device according to claim 5, wherein the first valve (4), the second valve (5) and the third valve (11) are hand valves.
7. The ultra-high vacuum sample transfer device according to claim 1, wherein the vacuum means comprises an adsorption pump (2) and an ion pump (3), the adsorption pump (2) being in communication with the sample entry chamber, the ion pump (3) being in communication with the adsorption pump (2).
8. The ultra-high vacuum sample transfer device according to claim 1, wherein the sample transfer means comprises a magnetic rod (7) extending into the sample chamber from outside the sample chamber, the magnetic rod (7) being capable of gripping the sample in the sample chamber and controlling the movement and rotation of the sample.
9. A method of sample transfer using the ultra-high vacuum sample transfer device of any of claims 1-8, the method comprising the steps of:
s1, opening the first valve (4), closing the second valve (5), and vacuumizing the sample chamber, the bellows (8) and the sample transfer device by using a vacuum device;
s2, connecting the cooling device (10) to the second valve (5) of the sample chamber;
s3, vacuumizing the cooling device (10) by using a movable pump group, introducing liquid nitrogen into a liquid injection port (1001) of the cooling device (10), and opening a vent port (1002) of the cooling device (10) to allow the liquid nitrogen to flow in the cooling device (10);
s4, after the device (10) to be cooled is cooled to the temperature of liquid nitrogen, closing the third valve (11), communicating the cooling device (10) with the target chamber, and vacuumizing the target chamber and the cooling device (10) to 10E-10 mbar;
s5, opening the second valve (5), adjusting the corrugated pipe (8), enabling the sample transfer device to enter the sample introduction chamber for sampling, adjusting the corrugated pipe (8) again, and pushing the sample to the target chamber by the sample transfer device;
s6, after the process is completed, taking out the sample, placing the sample in a sample introduction chamber, cutting off the communication between the cooling device (10) and the target chamber, closing the second valve (5), and detaching the cooling device (10) after the liquid nitrogen is evaporated.
10. The transfer method according to claim 9, characterized in that it further comprises the steps of:
and after the cooling device (10) is cooled to the temperature of the liquid nitrogen, wrapping the cooling device (10) by using a heat insulating material.
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Cited By (5)
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| CN113340813A (en) * | 2021-05-12 | 2021-09-03 | 西安交通大学 | Portable ultrahigh vacuum low-temperature observation cavity with micro-area characterization function and operation method |
| CN113655241A (en) * | 2021-08-19 | 2021-11-16 | 中国科学院苏州纳米技术与纳米仿生研究所 | Butt joint sample transfer device and optical system |
| CN114113285A (en) * | 2021-12-08 | 2022-03-01 | 中国工程物理研究院材料研究所 | Mechanism and method for measuring air release rate of metal material |
| CN114878841A (en) * | 2022-04-26 | 2022-08-09 | 中国工程物理研究院材料研究所 | Interconnecting switching vacuum device and ultrahigh vacuum equipment |
| CN116223771A (en) * | 2023-02-27 | 2023-06-06 | 中国科学院合肥物质科学研究院 | Vacuum low-temperature lunar soil simulation delivery system and experimental equipment |
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