CN105628978B - Ultrahigh vacuum sample transfer equipment and transfer method - Google Patents
Ultrahigh vacuum sample transfer equipment and transfer method Download PDFInfo
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- CN105628978B CN105628978B CN201410609148.5A CN201410609148A CN105628978B CN 105628978 B CN105628978 B CN 105628978B CN 201410609148 A CN201410609148 A CN 201410609148A CN 105628978 B CN105628978 B CN 105628978B
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Abstract
A kind of ultrahigh vacuum sample transfer equipment of present invention offer and transfer method, the equipment include：A sample chamber, an adapter cavity and a sample transfer device, the sample cavity maintains ultra-high vacuum environment, one first valve is set between the sample cavity and the adapter cavity, so that the sample cavity is connected to or separates with the adapter cavity, the adapter cavity is connect with a docking facilities, and can be connect with an external target device by the docking facilities, the sample transfer device can transmit sample between the sample cavity and the external target device.The advantage of the invention is that, adapter cavity is as middle chamber, both it may be at ultra-high vacuum state, it again can be identical as outside pressure, so that in sample storage and transfer process, no matter whether transfer equipment is connected with external target device, and sample is in the environment of ultrahigh vacuum always, and can avoid interfering with each other for the noises such as distinct device room machine vibration.
Description
Technical field
The present invention relates to field of material testing, more particularly to one kind are clear to having before carrying out nanoscale accurate measurement
The ultrahigh vacuum sample transfer equipment and transfer method of transmission and the storage of the sample on clean surface.
Background technology
With the development of nanometer science and technology, the scale of the interested material of people and device is smaller and smaller, performance
Atomic Arrangement and electron energy state structure for surface and boundary is more sensitive.Therefore, to the survey of these nano materials and device
It takes temperature sign, the requirement to spatial resolution is also higher and higher.By taking scanning probe microscopy as an example, it is with a metal or semiconductor
Needle point is in sample surfaces point by point scanning, using probe interaction different from sample come searching surface or interface in nanoscale
On the microcells property such as the electricity, power, the light that show.Developed includes scanning tunneling microscope, atomic force microscope and near field light
The a series of new Microbeam Analysis Techniques including microscope etc. are learned, there is very high spatial resolution, it might even be possible to directly in reality
Atomic structure of the space observation to sample surfaces.
The high advantage of this characterization method spatial resolution is given full play to, a necessary condition is exactly sample surfaces in original
Cleaning on sub- grade scale.This requires this kind of experiments to be carried out in ultra-high vacuum environment, to prevent from adsorbing and aoxidizing etc.
Pollution to sample surfaces.By taking STM or AFM as an example, experiment in 5-8 hours is carried out generally for clean surface is ensured, is needed
It maintains to be better than 3E-8The vacuum environment of Pa.And sample will often carry out certain place after atmospheric environment enters vacuum environment
Reason carries out experiment to obtain clean surface.
A kind of traditional processing mode is bombarded sample surfaces with argon ion in ultrahigh vacuum, is touched by physics
The atom for removing several nanometers of sample most surface being contaminated in atmospheric environment is hit, unpolluted surface is exposed,
Then to sample heating anneal so that surfacing.But this processing mode also has significant limitations, the i.e. atom of most surface total
To be removed, this is just difficult to directly research the sample surfaces that fresh Growth comes out or fresh cleavage and focused-ion-beam lithography
Example cross section.
Another settling mode is to etch the vacuum such as the sample growns such as scanning probe microscopy and MBE device, FIB to fill
Set, the devices such as vacuum cleavage are connected with vacuum pipe, the sample of fresh Growth or cleavage does not expose air directly in vacuum
In be directly delivered on scanning probe microscopy and tested by transmission lever, manipulator etc..But this mode is technically
There is prodigious difficulty.
On the one hand, ultra-high vacuum system is extremely complex and cumbersome in operation and maintenance.Especially by these different purposes
Preparation, processing and measuring device when being connected to same set of ultra-high vacuum system, compared to separate mini system, use it
In any one device all will be more cumbersome, failure rate also higher can also influence even wherein some device breaks down
The use of whole system.It is respectively discrete that these all so that the working efficiency of this system all to link together can be far below
Mini system.
On the other hand, also importantly, scanning probe microscopy (including STM and AFM) is very quick to ambient vibration
The equipment of sense, good vibration isolation are a key elements for realizing its nanoscale up to atom level spatial resolution.And
All these devices are all connected in a ultra-high vacuum system as described above, the vibration noise that miscellaneous equipment operating generates
With the resonance of a whole set of vacuum pipe, huge challenge is technically all proposed to the vibration isolation of scanning probe microscopy.
In conclusion should ensure that freshly prepared sample surfaces, not by air environmental pollution, are kept away again before characterization
The problem of exempting from vibration isolation difficulty and the service efficiency reduction that excessively huge ultra-high vacuum system is brought, is to give full play to scanning
The difficulty that the high advantage of probe microscope spatial resolution must pull against.
Invention content
The technical problem to be solved by the invention is to provide a kind of ultrahigh vacuum sample transfer equipment and transfer method,
Sample can be made to be in the environment of ultrahigh vacuum always, and distinct device room machine can be avoided in sample transfer process
The noises such as vibration interfere with each other.
To solve the above-mentioned problems, the present invention provides a kind of ultrahigh vacuum sample transfer equipments, including：A sample chamber,
One adapter cavity and a sample transfer device, the sample cavity maintain ultra-high vacuum environment, the sample cavity and the adapter cavity it
Between one first valve, so that the sample cavity is connected to or separates with the adapter cavity, the adapter cavity and a docking facilities are set
Connection, and can be connect with an external target device by the docking facilities, the sample transfer device can be in the sample cavity
And transmit sample between the external target device.
Further, further include a getter pump, the getter pump is connect with the sample cavity, so that the sample cavity is tieed up
Hold ultra-high vacuum environment.
Further, a mobile device is connect with the ultrahigh vacuum sample transfer equipment, described in carrying, movement and positioning
Ultrahigh vacuum sample transfer equipment.
Further, the sample transfer device is a push-pull rod that the sample cavity is stretched into outside the sample cavity, is pushed away
The push-pull rod is drawn so that the push-pull rod transmits sample between the sample cavity and the external target device.
Further, further include an apparatus for baking, the apparatus for baking dries the ultrahigh vacuum sample transfer equipment
It is roasting, with degasification.
Further, further include a vacuum extractor being connect with the adapter cavity and an air charging system, the vacuum means
It sets for extracting vacuum to the adapter cavity, so that the adapter cavity is vacuum or high vacuum or ultra-high vacuum environment, it is described to fill
Device of air is inflated for the adapter cavity, so that the adapter cavity has gaseous environment.
Further, further include a vacuum checking device being connect with the adapter cavity, the vacuum degree for measuring adapter cavity.
Further, one second valve is provided in the external target device, so that the adapter cavity and the external mesh
Marking device is connected to or partition.
Further, the docking facilities are quick CF flanges.
The present invention also provides a kind of methods of ultrahigh vacuum sample transfer, include the following steps：
(1) one docking facilities are connect with an external target device so that an adapter cavity by the docking facilities with it is described
External target device connects；(2) one vacuum extractors extract vacuum to the adapter cavity, so that the adapter cavity is vacuum ring
Border；(3) the second valve of the external target device is opened, so that the external target device is communicated with the adapter cavity, institute
It is ultra-high vacuum environment to state external target device；(4) the first valve between the adapter cavity and sample cavity is opened, so that described
External target device, adapter cavity and the sample cavity communicate；(5) use a sample transfer device the sample cavity with it is described outer
Sample is shifted between portion's target device；(6) the first valve between the adapter cavity and sample cavity is closed, so that the sample cavity is tieed up
Hold ultra-high vacuum environment.
Further, in step (6), the second valve of the external target device is closed, so that the external object is set
It is standby to separate with the adapter cavity, further comprise following steps after step (6)：Release the ultrahigh vacuum shape of the adapter cavity
State detaches adapter cavity with the external target device.
It is an advantage of the current invention that using always maintain ultra-high vacuum state sample cavity and with the external target device
The adapter cavity of connection, adapter cavity not only may be at ultra-high vacuum state, but also can be identical as ambient pressure as middle chamber,
So that sample storage or transfer process in, no matter ultrahigh vacuum sample transfer equipment whether with external target device phase
Even, the sample is in the environment of ultrahigh vacuum always, and can avoid the mutual of the noises such as distinct device room machine vibration
Interference.
Description of the drawings
Fig. 1 is the structural schematic diagram of ultrahigh vacuum sample transfer equipment of the present invention；
Fig. 2 is the step flow chart of ultrahigh vacuum sample transfer method of the present invention.
Specific implementation mode
Below in conjunction with the accompanying drawings to the specific embodiment party of ultrahigh vacuum sample transfer equipment provided by the invention and transfer method
Formula elaborates.Herein it is to be appreciated that in the present invention, vacuum refers to that pressure reaches the 1EPa orders of magnitude, what high vacuum referred to
It is that pressure reaches 1E-5~1E-6The Pa orders of magnitude, ultrahigh vacuum refer to that pressure reaches 1E-8The Pa orders of magnitude.
Referring to Fig. 1, ultrahigh vacuum sample transfer equipment 100 of the present invention includes a sample chamber 1 and an adapter cavity 2.
The sample cavity 1 maintains ultra-high vacuum environment.The sample cavity 1 maintains ultrahigh vacuum ring by vacuum keeping apparatus
Border, in this embodiment, the sample cavity 1 maintain ultra-high vacuum environment by getter pump 3.Getter pump 3 is one
Kind of chemisorption pump, it can absorb various active gases, such as hydrogen, oxygen, nitrogen, carbon dioxide, carbon monoxide, getter material with
Active gases chemically reacts, and generates the solid chemical compound of extremely low vapour pressure, to permanently extract in vacuum system
Various active gases.Using getter pump 3 maintain sample cavity 1 ultra-high vacuum environment the advantages of be, 3 body of the getter pump
Product is small, and pumping speed is high, can be for a long time in 1E-8It works under the vacuum degree of Pa magnitudes and does not need power supply, consequently facilitating the superelevation is true
The movement and use of empty sample transfer equipment 100.
One first valve 4 is set between the sample cavity 1 and the adapter cavity 2, so that the sample cavity 1 and the transition
Chamber 2 is connected to or partition.In this embodiment, first valve 4 is ultrahigh vacuum plate valve.Close the first valve
4, separate between the sample cavity 1 and the adapter cavity 2, is air if sample cavity 1 is ultra-high vacuum environment, in adapter cavity 2
Or other gaseous environments, sample cavity 1 and adapter cavity 2 are separated using the first valve 4, then the gaseous environment in adapter cavity 2 will not be broken
The ultra-high vacuum environment of bad sample cavity 1 so that sample cavity 1 is able to maintain that ultra-high vacuum environment.Also it is ultrahigh vacuum in adapter cavity 2
When environment, the first valve 4 is opened, sample can be removed or placed into sample cavity 1, be able to maintain that the ultrahigh vacuum of sample cavity 1
Environment.
The adapter cavity 2 is connect with a docking facilities 5, and can pass through the docking facilities 5 and an external target device 200
Connection.In this embodiment, the docking facilities 5 be a quick CF flanges, can accelerate the docking facilities 5 with
The connection speed of external target device 200.
One vacuum extractor 6 is connect with the adapter cavity 2, for extracting vacuum to the adapter cavity 2.When the adapter cavity
2 be gaseous environment, then is vacuumized to adapter cavity 2 using vacuum extractor 6, so that adapter cavity 2 reaches vacuum or high vacuum or super
High vacuum environment.In this embodiment, the vacuum extractor 6 may include turbomolecular pump and dry type volute pump,
In this embodiment, after startup dry type volute pump (mechanical pump) is pumped to the limit (the about 1Pa orders of magnitude), start turbine point
Pressure is evacuated to high vacuum state, i.e., 10 by son pump-6~10-5Pa。
Further, further include an air charging system 7 being connect with the adapter cavity 2, the air charging system 7 is the adapter cavity
2 inflations, so that the adapter cavity 2 has gaseous environment.Or when the adapter cavity 2 vacuumizes or in vacuum or high vacuum surpass
High vacuum environment then closes the air charging system 7, when the vacuum or high vacuum or ultrahigh vacuum vacuum for needing elimination adapter cavity 2
Environment is then opened air charging system 7 and is inflated for adapter cavity 2, so that adapter cavity 2 is balanced with ambient pressure.It can be to the adapter cavity 2
In be filled with nitrogen either inert gas or directly open air charging system 7, admit air into the adapter cavity 2.Further,
Further include a vacuum checking device 8, the vacuum degree for measuring and monitoring the adapter cavity 2.In this embodiment, institute
It is vacuum gauge to state vacuum checking device 8.
The ultrahigh vacuum sample transfer equipment 100 further includes a sample transfer device 9.The sample transfer device 9 can
Sample is transmitted between the sample cavity 1 and the external target device 200.In this embodiment, the sample transmits
Device 9 is a push-pull rod that the sample cavity 1 is stretched into outside the sample cavity 1, pushes and pulls the push-pull rod so that the push-and-pull
Bar transmits sample between the sample cavity 1 and the external target device 200.It is located at the end in sample cavity 1 in the push-pull rod
Portion has (does not indicate) with sample plummer in attached drawing, when needing to transmit sample, make push-pull rod with sample plummer
End enter inside external target device 200, utilize manipulator in external target device 200 to carry out picking and placeing for sample.
Further, a mobile device 10 is connect with the ultrahigh vacuum sample transfer equipment 100, with carrying, movement and is determined
The described position is more than vacuum sample transfer equipment 100.In this embodiment, the mobile device 10 is a trolley, in institute
The bottom for stating trolley is provided with universal wheel, the alignment for horizontal direction when being docked with external target device 200.Further, institute
The supporting rod 11 that sample transfer device 9 can be arranged by one in the mobile device 10 is stated to support simultaneously shift position.Into one
Step, any of the above described device can support fixation by the supporting rod 11 being arranged in mobile device 10.
Further, further include an apparatus for baking (not indicated in attached drawing), the apparatus for baking is to the ultrahigh vacuum sample
Transfer equipment 100 is toasted, with degasification.
Further, one second valve 21 is provided in the external target device 200 so that the adapter cavity 2 with it is described
External target device 200 is connected to or partition.When needing to transmit sample, if the adapter cavity 2 is vacuum or high vacuum or superelevation
Vacuum environment, then can open the second valve 21, and the adapter cavity 2 is connected to the external target device 200, if the mistake
It is vacuum or high vacuum or ultra-high vacuum environment to cross chamber 2 not, then needs to vacuumize the adapter cavity 2 using vacuum extractor 6,
So that the adapter cavity 2 is vacuum or high vacuum or ultra-high vacuum environment.Only it is vacuum or high vacuum or superelevation in adapter cavity 2
Vacuum environment can just open the second valve 21, enter in external target device 200 to can avoid ambient atmos, cause dirt
Dye.
The present invention also provides a kind of methods of ultrahigh vacuum sample transfer, and referring to Fig. 2, described method includes following steps：
Step S20, a docking facilities are connect with an external target device so that an adapter cavity by the docking facilities with
The external target device connection.Device corresponding with the docking facilities is provided in the external target device, so that
The docking facilities are connectable in external target device.
Step S21, a vacuum extractor extracts vacuum to the adapter cavity, so that the adapter cavity is vacuum or high vacuum
Or ultra-high vacuum environment.The adapter cavity is connect by the docking facilities with the external target device, at this point, the transition
Chamber is not communicated with the external target device.The adapter cavity is gaseous environment, and external target device is superelevation Altitude,
It is therefore desirable to which adapter cavity is made to be vacuum or high vacuum or ultra-high vacuum environment.
Step S22, the second valve of the external target device is opened, so that the external target device and the transition
Chamber communicates, and the external target device is ultra-high vacuum environment.When the adapter cavity is vacuum or high vacuum or ultrahigh vacuum ring
When border, second valve can be just opened, so that the adapter cavity is communicated with external target device.If the adapter cavity is true
Empty or high vacuum environment, then since the volume of adapter cavity and internal surface area are much smaller than external target device, open the second valve it
Afterwards, it is true to reach superelevation for the pressure meeting rapid equalisation in adapter cavity to identical level, i.e. adapter cavity with inside external target device
Altitude.
Step S23, the first valve between the adapter cavity and sample cavity is opened, so that the external target device, mistake
It crosses chamber and the sample cavity communicates.At this point, external target device, adapter cavity, sample cavity are ultra-high vacuum environment.
Step S24, using a sample transfer device sample is shifted between the sample cavity and the external target device.It pushes away
Dynamic sample transfer device, is made the sample plummer of sample transfer device end enter inside external target device, is set using target
Standby upper manipulator mutually shifts sample between the specimen holder inside sample transfer device end and target device.
Step S25, the first valve between the adapter cavity and sample cavity is closed, so that the sample cavity maintains superelevation true
Altitude closes the second valve of the external target device, so that the external target device is separated with the adapter cavity.
Step S26, the ultra-high vacuum state for releasing the adapter cavity, by adapter cavity and the external target device point
From so as to carry out sample transfer.
One embodiment of the invention is set forth below.
1, the initialization of ultrahigh vacuum sample transfer equipment.
CF flanges are connect soon by vacuum to connect and seal with an external target device.Close second in external target device
The air charging system of valve and changeover portion chamber filling nitrogen.The first valve between sample cavity and adapter cavity is opened, so that sample
Chamber communicates with one another with adapter cavity.After startup dry type volute pump (mechanical pump) is pumped to the limit (the about 1Pa orders of magnitude), start turbine point
Pressure is evacuated to 10 by son pump-6~10-5Pa.Then ultrahigh vacuum sample transfer equipment of the present invention is toasted with apparatus for baking,
With further degasification.The getter pump for being installed on main chamber is initialized by the power supply near external target device, and
Start getter pump.Baking terminates chamber inner pressure and is down to 1E by force-8Pa, closes the first valve, and sample cavity maintains it by getter pump
The environment of ultrahigh vacuum.At this moment turbomolecular pump and dry type volute pump are closed, is filled into adapter cavity by air charging system high-purity
Then nitrogen is opened to being balanced with atmospheric pressure outside chamber and connects CF flanges soon, the initialization of ultrahigh vacuum sample transfer equipment is completed.
After ultrahigh vacuum sample transfer equipment completes initialization, it is entirely located on an independent trolley, adapter cavity has been exposed through greatly
Gas, molecular pump and dry type volute pump have stalled, and maintain the getter pump of main chamber's ultrahigh vacuum in normal work not
Need power supply power supply, thus can breakaway equipment and power supply and arbitrarily move.
2, the transmission of sample.
After initialization, the sample cavity of ultrahigh vacuum sample transfer equipment is daily to be maintained under UHV condition.It needs
When transmitting sample, the CF flanges that connect soon that moving trolley makes to connect in CF flanges alignment external target device soon make after connection sealing
With the gas of electric power starting dry type volute pump and turbo-molecular pumped adapter cavity near target device, pressure is evacuated to 10-6
~10-5Pa, the second valve being then turned in external target device.Since the volume and internal surface area of adapter cavity are much smaller than outside
Target device, after opening the second valve, identical water inside the pressure meeting rapid equalisation to external target device in adapter cavity
It is flat so that adapter cavity is ultra-high vacuum environment, then opens the first valve between sample cavity and adapter cavity again so that sample
Chamber is connected to external target device.Sample transfer device is pushed, the sample plummer of sample transfer device end is made to enter outside
Inside target device, using specimen holder of the manipulator on target device inside sample transfer device end and target device it
Between mutually shift sample.Sample transfer device of retracting after sample has been shifted, the first valve and the second valve are closed, has closed turbine
Molecular pump and dry type volute pump, and extremely balance each other to changeover portion chamber filling nitrogen with external atmosphere pressure.It finally disconnects and meets CF soon
Flange can remove ultrahigh vacuum sample transfer equipment.At this point, the sample cavity of ultrahigh vacuum sample transfer equipment is still being not required to
It wants to maintain ultra-high vacuum state under the action of the getter pump of power supply power supply, being stored in the sample surfaces of the inside will not be contaminated
And oxidation.
The ultrahigh vacuum sample transfer equipment being loaded on trolley is on shifting another external target device onto, in repetition
Same process is stated, transmission of the sample between distinct device can be completed.Throughout the delivery process, sample is in superelevation always
In vacuum environment, to maintain the cleaning on its surface.Meanwhile different equipment rooms is effectively prevented without any mechanical connection
The noises such as distinct device room machine vibrations interfere with each other.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (7)
1. a kind of ultrahigh vacuum sample transfer equipment, which is characterized in that including：A sample chamber, an adapter cavity and a sample are transmitted
Device, the sample cavity maintain ultra-high vacuum environment, and one first valve is arranged between the sample cavity and the adapter cavity, so that
The sample cavity is connected to or separates with the adapter cavity, and the adapter cavity is connect with a docking facilities, and can pass through the docking
Device is connect with an external target device, and the sample transfer device can pass between the sample cavity and the external target device
Sample is passed, a mobile device is connect with the ultrahigh vacuum sample transfer equipment, with carrying, movement and the positioning ultrahigh vacuum
Sample transfer equipment, the ultrahigh vacuum sample transfer equipment further include a vacuum extractor being connect with the adapter cavity and one
Air charging system, the vacuum extractor is used to extract vacuum to the adapter cavity, so that the adapter cavity is vacuum environment, it is described
Air charging system is inflated for the adapter cavity, so that the adapter cavity has gaseous environment.
2. ultrahigh vacuum sample transfer equipment according to claim 1, which is characterized in that further include a getter pump, institute
It states getter pump to connect with the sample cavity, so that the sample cavity maintains ultra-high vacuum environment.
3. ultrahigh vacuum sample transfer equipment according to claim 1, which is characterized in that the sample transfer device is one
The push-pull rod that the sample cavity is stretched into outside the sample cavity pushes and pulls the push-pull rod so that the push-pull rod is in the sample
Sample is transmitted between chamber and the external target device.
4. ultrahigh vacuum sample transfer equipment according to claim 1, which is characterized in that further include an apparatus for baking, institute
It states apparatus for baking to toast the ultrahigh vacuum sample transfer equipment, with degasification.
5. ultrahigh vacuum sample transfer equipment according to claim 1, which is characterized in that further include one and the adapter cavity
The vacuum checking device of connection, the vacuum degree for measuring adapter cavity.
6. ultrahigh vacuum sample transfer equipment according to claim 1, which is characterized in that set in the external target device
It is equipped with one second valve, so that the adapter cavity is connected to or separates with the external target device.
7. a kind of method of ultrahigh vacuum sample transfer, which is characterized in that include the following steps：
(1) one docking facilities are connect with an external target device, so that an adapter cavity passes through the docking facilities and the outside
Target device connects；
(2) one vacuum extractors extract vacuum to the adapter cavity, so that the adapter cavity is vacuum environment；
(3) the second valve of the external target device is opened, so that the external target device is communicated with the adapter cavity, institute
It is ultra-high vacuum environment to state external target device；
(4) the first valve between the adapter cavity and sample cavity is opened, so that the external target device, adapter cavity and described
Sample cavity communicates；
(5) using a sample transfer device sample is shifted between the sample cavity and the external target device；
(6) the first valve between the adapter cavity and sample cavity is closed, so that the sample cavity maintains ultra-high vacuum environment, is closed
The second valve of the external target device is closed, so that the external target device is separated with the adapter cavity；
Further comprise following steps after step (6)：The ultra-high vacuum state for releasing the adapter cavity, by the transition
Chamber is detached with the external target device.
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| CN111876729B (en) * | 2020-07-02 | 2021-08-13 | 中国科学技术大学 | STM-MBE combined system |
| 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 |
| CN113740108A (en) * | 2021-08-27 | 2021-12-03 | 清华大学 | Particle sampling device, analysis system and sampling method for vacuum environment of equipment |
| CN114277355A (en) * | 2021-12-28 | 2022-04-05 | 深圳优普莱等离子体技术有限公司 | Double-cavity system and equipment for chemical vapor deposition diamond |
| 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 |
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