CN110320389A - A kind of original position property test system and sample mounting procedure - Google Patents
A kind of original position property test system and sample mounting procedure Download PDFInfo
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- CN110320389A CN110320389A CN201910712480.7A CN201910712480A CN110320389A CN 110320389 A CN110320389 A CN 110320389A CN 201910712480 A CN201910712480 A CN 201910712480A CN 110320389 A CN110320389 A CN 110320389A
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- 238000012360 testing method Methods 0.000 title claims abstract description 145
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000005057 refrigeration Methods 0.000 claims abstract description 57
- 238000010790 dilution Methods 0.000 claims abstract description 56
- 239000012895 dilution Substances 0.000 claims abstract description 56
- 238000011065 in-situ storage Methods 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims description 20
- 238000009434 installation Methods 0.000 claims description 18
- 239000001307 helium Substances 0.000 claims description 14
- 229910052734 helium Inorganic materials 0.000 claims description 14
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 5
- 230000000704 physical effect Effects 0.000 abstract description 16
- 238000012512 characterization method Methods 0.000 abstract description 15
- 238000005259 measurement Methods 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 8
- 239000000523 sample Substances 0.000 description 148
- 239000000463 material Substances 0.000 description 12
- 230000003287 optical effect Effects 0.000 description 11
- 238000007789 sealing Methods 0.000 description 10
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000003032 molecular docking Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 244000273618 Sphenoclea zeylanica Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 239000013307 optical fiber Substances 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/11—Filling or emptying of cuvettes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/08—Means for establishing or regulating a desired environmental condition within a sample chamber
- G01Q30/10—Thermal environment
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q30/00—Auxiliary means serving to assist or improve the scanning probe techniques or apparatus, e.g. display or data processing devices
- G01Q30/08—Means for establishing or regulating a desired environmental condition within a sample chamber
- G01Q30/16—Vacuum environment
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
Abstract
The present invention relates to physical property measurement technical field in situ, a kind of property test system in situ and sample mounting procedure are disclosed.Original position property test system provided by the invention connects vacuum sample Preparation equipment by vacuum equipment, sample is packed into vacuum test chamber and is sealed in vacuum equipment, vacuum test component is connected to inserted link component again, inserted link component and fast sample room are tightly connected, fast sample room is connected to dilution refrigeration machine by gate valve, control inserted link component movement carries out sample test so that vacuum test component to be pushed into dilution refrigeration machine, it ensure that accuracy when carrying out physical property characterization using above-mentioned property test system in situ, not only meets the needs of physical property characterizes under all extreme conditions relevant with dilution refrigeration machine, solves the project that exposed atmosphere can be undergone by the characterization measurement sample cargo handling process of dilution refrigeration machine, completely remain the high-intensity magnetic field and pole low temperature environment of dilution refrigeration machine script.
Description
Technical field
The present invention relates to physical property measurement technical field in situ more particularly to a kind of property test system in situ and sample installations
Method.
Background technique
Design, preparation and the characterization of quantum material are an important research directions of " quantum regulation and control ".Traditional method is to taste
It tries a variety of different materials and meets demand to find, but this way has period length, the defect of low efficiency.For this purpose, existing
Method be that material is designed and prepared based on the profound understanding to material structure and physical property as desired, with realize precisely manufacture.
But with the reduction of material dimension, the atom accounting on material surface is increasing, and exposure atmosphere will be to the intrinsic of material
Matter brings tremendous influence.
Vacuum interconnection is acknowledged as solving the effective technology of this problem in science, and many laboratories in the prior art
This technology has been utilized, thin-film material growth and the interconnection of phenetic analysis means have been got up, to material in the environment of vacuum
Intrinsic properties progress extensively and profoundly is studied, and the result much to attract people's attention is also achieved.But characterization under extreme conditions, especially
It is that the extremely low temperature high-intensity magnetic field physical property characterization based on dilution refrigeration machine technology is difficult to accomplish quasi- in situ, existing to rely on dilution refrigeration machine
Characterization measurement sample switching process exposure atmosphere, the oxygen gas and water etc. in atmosphere brings serious shadow to the intrinsic properties of sample
It rings, therefore is badly in need of a kind of property test system in situ and sample mounting procedure, during realizing that sample enters dilution refrigeration machine
Not ingress of air completely not only can satisfy the demand that physical property characterizes under all extreme conditions relevant with dilution refrigeration machine, and
And it avoids and exposes atmosphere by the characterization measurement sample cargo handling process of dilution refrigeration machine.
Summary of the invention
The purpose of the present invention is to provide a kind of property test system in situ and sample mounting procedures, can be realized sample
It is not in that sample is exposed to the problems in air during being placed in dilution refrigeration machine.
To achieve this purpose, the present invention adopts the following technical scheme:
A kind of original position property test system, including dilution refrigeration machine, further includes:
Vacuum test component comprising for placing the vacuum test chamber of sample, and to the survey that the sample is tested
Try unit；
Fast sample room, inserted link component, one end of the inserted link component protrude into the fast sample room and with it is described fast
Fast Sample Room is removably tightly connected, and the inserted link component can move axially so that the vacuum test component enters or takes off
From the dilution refrigeration machine；
Vacuum equipment is capable of providing vacuum environment or inert gas environment, described for connecting vacuum sample Preparation equipment
It is placed in vacuum test subassembly selection in the vacuum equipment or takes out out of described vacuum equipment to be removably attachable to
The inserted link component protrudes into the indoor one end of the fast sample；
Gate valve, one end are connected to the dilution refrigeration machine, and the other end is sealedly attached to the fast sample room, described
Gate valve can selectively control the dilution refrigeration machine and be connected to or disconnect with the fast sample room；
Vacuum unit, for being vacuumized to the fast sample room.
As a kind of optimal technical scheme of above-mentioned property test system in situ, the vacuum test chamber is equipped with disengaging gas
Mouthful, the air inlet/outlet is equipped with valve.
As a kind of optimal technical scheme of above-mentioned property test system in situ, the inserted link component includes operating stick, institute
The one end for stating operating stick is connected to the valve, the other end be pierced by from one end of the fast sample room and with the fast sample
Room is tightly connected, and the operating stick is configured as controlling the valve event so that the vacuum test chamber and the fast sample
Room connection disconnects.
It further include unit of supplying gas as a kind of optimal technical scheme of above-mentioned property test system in situ, the list of supplying gas
Member is for helium to be sent into the fast sample room.
As a kind of optimal technical scheme of above-mentioned property test system in situ, the fast sample room includes can be axial
Flexible bellows；The inserted link component includes:
First flange, one end of the bellows are removably tightly connected with the first flange, and the other end is connected to
The gate valve；
Multiple connecting rods, one end of each connecting rod and the first flange are tightly connected, and the other end is connected with
Connect disk.
As a kind of optimal technical scheme of above-mentioned property test system in situ, one end of the test cell, which is connected with, draws
Connector out, the extraction connector stretch out the vacuum test chamber and are detachably electrically connected with the terminal pad.
As a kind of optimal technical scheme of above-mentioned property test system in situ, the vacuum test chamber include sample cavity and
The installation top cover being connect with its removable seal.
The present invention also provides the sample mounting procedures of above-mentioned property test system in situ, comprising the following steps:
S1, that sample is packed into the vacuum test in the vacuum equipment is intracavitary, seal the vacuum test chamber and from
The vacuum test component is taken out in the vacuum equipment；
S2, the vacuum test component is connected to the inserted link component, and the inserted link component is connected into vacuum test
One end of component is protruded into the fast sample room, and the fast sample room is removably tightly connected with the inserted link component；
S3, the fast sample room is evacuated to predetermined vacuum degree；
S4, the dilution refrigeration machine is connected to the fast sample room by the gate valve, control the inserted link group
The vacuum test component is sent into the dilution refrigeration machine by part axial movement.
A kind of optimal technical scheme of sample mounting procedure as above-mentioned property test system in situ, the vacuum test
Chamber is equipped with air inlet/outlet, and the air inlet/outlet is equipped with valve；
In step sl, by sample be packed into the vacuum test it is intracavitary after, open the valve for inert gas and be sent into institute
State that vacuum test is intracavitary to turn off the valve；
In step s3, after the fast sample room being evacuated to predetermined vacuum degree, open the valve make it is described true
The intracavitary inert gas of hollow testing is discharged into the fast sample room, is again evacuated to the fast sample room described default true
Reciprocal of duty cycle.
A kind of optimal technical scheme of sample mounting procedure as above-mentioned property test system in situ, it is described quickly into
Before the indoor vacuum degree of sample reaches the predetermined vacuum degree again, the vacuum test chamber is vacuumized, multiple helium
It rinses, then the vacuum test chamber is evacuated to the predetermined vacuum degree.
Beneficial effects of the present invention: the present invention connects vacuum sample Preparation equipment by vacuum equipment, to accept vacuum sample
The sample of Preparation equipment preparation provides vacuum environment or inert gas environment by vacuum equipment, by sample in vacuum equipment
It is packed into vacuum test chamber and seals, then vacuum test component is connected to inserted link component, inserted link component is sealedly attached to
Fast sample room is to close fast sample room, after vacuumizing to fast sample room, is made quickly by gate valve
Sample Room is connected to dilution refrigeration machine, and the movement of control inserted link component is vacuum test component to be pushed into dilution refrigeration machine to sample
Physical property characterization is carried out, sample is realized and enters during dilution refrigeration machine not ingress of air completely, ensure that using above-mentioned original
Position property test system carries out accuracy when physical property characterization, solves and measures by the characterization of dilution refrigeration machine in vacuum environment
The problem of lower process for carrying out sample switching can undergo the sample cargo handling process of exposed atmosphere.
It is provided by the invention original position property test system, sample is placed in vacuum test it is intracavitary after, can be in vacuum
Sample is placed in equipment, to wiring between sample and test cell etc., it is easy to operate.
Vacuum test component provided by the invention can be applied to all test cells and vacuum for relying on dilution refrigeration machine
The docking of sample preparation device, it is versatile.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, institute in being described below to the embodiment of the present invention
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also implement according to the present invention
The content of example and these attached drawings obtain other attached drawings.
Fig. 1 is the main view for the property test system in situ that the embodiment of the present invention provides；
Fig. 2 is the connection schematic diagram of inserted link component and vacuum test component provided in an embodiment of the present invention；
Fig. 3 is the structural schematic diagram of vacuum test component provided in an embodiment of the present invention；
Fig. 4 is the flow chart of the sample mounting procedure of property test system in situ provided in an embodiment of the present invention.
In figure:
1, dilution refrigeration machine；
2, fast sample room；
3, inserted link component；31, first flange；311, incidence hole；312, port is pumped；313, the first fairlead；32, it supports
Disk；321, perforating；322, the second fairlead；33, connecting rod；34, operating stick；35, terminal pad；
4, gate valve；
5, vacuum test component；51, top cover is installed；52, sample cavity；53, connector is drawn；54, optical lens；55, valve；
6, straight spur unit.
Specific embodiment
To keep the technical problems solved, the adopted technical scheme and the technical effect achieved by the invention clearer, below
In conjunction with attached drawing and pass through specific embodiment to further illustrate the technical scheme of the present invention.It is understood that this place is retouched
The specific embodiment stated is used only for explaining the present invention rather than limiting the invention.It also should be noted that in order to just
Only the parts related to the present invention are shown in description, attached drawing and it is not all.
Fig. 1 is the main view of property test system in situ provided in this embodiment, and Fig. 2 is inserted link group provided in this embodiment
The connection schematic diagram of part and vacuum test component, Fig. 3 are the structural schematic diagrams of vacuum test component provided in this embodiment.Such as figure
1 to shown in Fig. 3, and original position property test system provided in this embodiment is for making sample carry out physical property table under particular detection environment
Sign comprising dilution refrigeration machine 1, dilution refrigeration machine 1 make sample carry out physical property characterization in the environment of extremely low mild high-intensity magnetic field.On
Stating property test system in situ further includes vacuum test component 5 and vacuum equipment (not shown), wherein vacuum equipment can
Vacuum environment or inert gas environment are provided.Preferably, vacuum equipment uses glove box, to provide inert gas environment.Vacuum
Test component 5 includes sample cavity 52 and installation top cover 51, and it is true that sample cavity 52 and installation top cover 51 are removably tightly connected formation
Hollow testing chamber, sample cavity 52 is interior to be equipped with specimen holder, and sample is placed in specimen holder (not shown), will by installation top cover 51
Sample is sealed in sample cavity 52.In the present embodiment, sample cavity 52 and installation top cover 51 can using be threadedly coupled or clamping or
Other dismountable connection types.
Glove box provides inert gas environment in order to sample installation, and vacuum sample Preparation equipment such as vacuum film deposition is set
It prepares standby sample to transfer in glove box, vacuum test component 5 is placed in glove box, then dismantle installation top cover 51 and sample
Product chamber 52, sample is placed on specimen holder, and then installation top cover 51 and sample cavity 52 link together again.
In order to further protect to sample, installation top cover 51 is equipped with air inlet/outlet, and air inlet/outlet is equipped with valve
55, after installation top cover 51 and sample cavity 52 link together in glove box, open valve 55, the inert gas in glove box
Will be intracavitary automatically into vacuum test by air inlet/outlet, with to the intracavitary sample of vacuum test provide inert gas environment into
Row protection.Inert gas can be helium, argon gas etc., and due to being helium environment in dilution refrigeration machine 1, inert gas is preferred
Using helium.
Vacuum test component 5 further includes test cell, and test cell generally includes scanning probe, optical lens 54 and measurement
Chip, wherein scanning probe is set to the inner wall of installation top cover 51 and by drawing the extraction installation top cover of connector 53 with chip is measured
Outside 51, scanning probe and measure chip model according to the detection demand of sample determine, draw connector 53 and scanning probe and
Measuring chip can be connected by conducting wire or microwave line, use conducting wire or microwave line can according to actual needs really as specific
It is fixed, it is no longer superfluous herein to chat.It, can be in glove box to the test such as sample and measurement chip after sample is placed on specimen holder
Wiring between unit, such as pressure welding (Wire Bonding), have the advantages that easy to operate.Installation is opened up on installation top cover 51
Optical lens 54 is set in mounting hole and is tightly connected with mounting hole by hole, and the type of optical lens 54 can be according to optics object
Property measurement demand selection, such as can choose the higher optical lens 54 of optical projection rate, realize hypersensitive optical measurement.As for
Scanning probe, measurement chip and optical lens 54 are how to carry out test for the state of the art, no longer superfluous herein
It chats.
Above-mentioned original position property test system further includes fast sample room 2, inserted link component 3 and gate valve 4, wherein fast sample
Room 2 includes the bellows for capableing of axial stretching.One end of inserted link component 3 is protruded into fast sample room 2 and can with fast sample room 2
Releasably it is tightly connected.Specifically, inserted link component 3 includes first flange 31, terminal pad 35 and multiple connecting rods 33, bellows
One end is connected with second flange, and second flange is circular ring structure, is folded with sealing ring between first flange 31 and second flange, leads to
It crosses and is bolted first flange 31 and second flange, realize and be removably tightly connected between bellows and inserted link component 3.Each
One end of connecting rod 33 is connect with the inner wall of first flange 31, and the other end is connected to terminal pad 35, passes through the connection of connecting rod 33 the
One flange 31 and terminal pad 35.
Further, it is equipped in order to improve the stability of entire inserted link component 3, between first flange 31 and terminal pad 35 more
A support plate 32 axially laid, each connecting rod 33 sequentially pass through each support plate 32 and are arranged.Multiple support plates 32 are all provided with
In in bellows, the diameter of support plate 32 is less than the minimum diameter of bellows and is less than the outer diameter of first flange 31.In bellows
When being compressed, inserted link component 3 will be moved axially along dilution refrigeration machine 1, and by the restriction of above-mentioned size, it can guarantee support plate
32 will not collide with ripple inside pipe wall.The quantity of support plate 32 can be 4,5 or more, it is not limited here.
In the present embodiment, terminal pad 35 is detachably electrically connected with connector 53 is drawn, it is preferable that using pin and box sub clamping
Mode realizes electrical connection, for example, one end of terminal pad 35 is equipped with pin end, corresponding extraction connector 53 is to be clamped with pin end
Female connector realizes the detachable electrical connection of terminal pad 35 and vacuum test component 5 by pin end and female connector docking.Certainly
Female connector can be set in terminal pad 35, connector 53 will be drawn and select pin end.
The effect of signal transmitting is assumed responsibility for due to drawing connector 53, the pin end in terminal pad 35 is connected with signal biography thus
Defeated line (not shown).There are many modes that fast sample room 2 is drawn as signal transmssion line, there are two main ways mode
Mixing is laid, the first is that the first fairlead 313 is equipped in first flange 31, and the second fairlead is arranged in each support plate 32
322, signal transmssion line sequentially passes through each second fairlead 322 and is pierced by again from the first fairlead 313.In order to avoid outside air
Into in fast sample room 2, it is tightly connected at the link position of signal lead-out wire and the first fairlead 313.Second is to connect
Bar 33 uses hollow stem, and signal lead-out wire leads to the other end through one end of connecting rod 33, after the extraction of the side wall of connecting rod 33 again
It is drawn from the first fairlead 313.Preferably, in the present embodiment, axis direction of multiple second fairleads 322 along inserted link component 3
Spiral is laid or dislocation is laid, wherein the non-face of the second fairlead 322 in dislocation laying i.e. two neighboring support plate 32
Setting, multiple support plates 32 and the thereon distribution of the second fairlead 322 can play heat-blocking action, it is preferable that above-mentioned support
Disk 322 is made of heat-barrier material.
Further, first flange 31 is equipped with incidence hole 311, is equipped with face incidence hole 311 in each support plate 32
Perforating 321；One end of optical fiber and incidence hole 311 are tightly connected, and the other end sequentially passes through incidence hole 311, multiple perforatings
321 and it is connected to optical lens 54, realizes the propagation of optical signalling.
Further, vacuum test component 5 further includes operating stick 34, and one end of operating stick 34 is connected to valve 55, another
End is pierced by from one end of fast sample room 2 and is tightly connected with fast sample room 2, and it is dynamic that operating stick 34 is configured as control valve 55
Make so that vacuum test chamber is connected to or disconnects with fast sample room 2.In the present embodiment, above-mentioned valve 55, which preferably uses, passes through rotation
Operating stick 34 realizes the air valve that valve 55 opens or closes, or cooperates the controls such as prime mover such as motor to grasp by magnetic coupling
Make the rotation of bar 34, is placed in and how to cooperate prime mover to control the rotation of operating stick 34 for the prior art, herein not by magnetic coupling
It goes to live in the household of one's in-laws on getting married and chats again.
The other embodiment of the present invention can also using other modes control operating stick 34 rotate so that vacuum test chamber and
The connection of fast sample room 2 disconnects.Such as, the operating block for opening or closing air valve is set on air valve, and operating block is equipped with six sides
Shape hole, one end of operating stick 34 are pierced by first flange 31 and connect with 31 rotary seal of first flange, and the other end protrudes into bellows
Interior and sequentially pass through each support plate 32, one end of operating stick 34 is equipped with the hexagonal prisms for being inserted into hexagonal hole, then rotates
Operating stick 34 can make operating block that operating stick 34 be followed to rotate, and then open or close air valve.Certainly operating block can also be adopted
With hexagonal prisms, correspondingly, one end setting of aforesaid operations bar 34 is inserted into the hexagonal hole of hexagonal prisms.
One end of above-mentioned gate valve 4 is connected to dilution refrigeration machine 1, and the other end is connected to bellows.Preferably, gate valve 4
For gate valve, one end that bellows does not set second flange is equipped with third flange, and one end of gate valve is connected to dilution refrigeration machine 1,
The other end is bolted by multiple in third flange, to realize the connection between bellows and gate valve.In order to avoid occurring
Leakage problem is equipped with sealing ring between gate valve and the contact surface of third flange.State by adjusting gate valve can make dilute
It releases refrigeration machine 1 and is connected to or disconnects with fast sample room 2.
Above-mentioned inserted link component 3 can move axially so that the into and out dilution refrigeration machine 1 of vacuum test component 5.Tool
Body, above-mentioned original position property test system further includes straight spur unit 6, and straight spur unit 6 is connected to second flange, straight
When line driving unit 6 acts, bellows will stretch, to drive inserted link component 3 to move axially.Preferably, above-mentioned linear drives
Unit 6 can be using it is not limited to motor screw structure.When in the state that gate valve being in and opens, straight spur unit
6 movements will be such that bellows compresses, and then inserted link component 3 be driven to move axially to the direction close to dilution refrigeration machine 1, by vacuum
Test component 5 is pushed into dilution refrigeration machine 1.
Make sample not ingress of air, the present embodiment to guarantee for sample to be sent into during the entire process of dilution refrigeration machine 1
The property test system in situ of offer further includes vacuum unit, for vacuumizing to fast sample room 2.The mistake vacuumized
Vacuum test component 5 is mainly being connected to inserted link component 3 by journey, and one end that inserted link component 3 connects vacuum test component 5 is stretched
Enter in fast sample room 2, and by after inserted link component 3 and the sealed connection of fast sample room 2, exists in fast sample room 2 at this time empty
Gas, and in order to which vacuum test component 5 to be pushed into dilution refrigeration machine 1, need to open gate valve, in order to avoid fast sample room 2
Interior air impacts the environment in dilution refrigeration machine 1, therefore needs to pass through vacuum unit before opening gate valve
Fast sample room 2 is vacuumized, to avoid the environment in dilution refrigeration machine 1 by air impact, while can be avoided sample
Ingress of air.Preferably, above-mentioned vacuum unit is vacuum pump.
In order to keep fast sample room 2 consistent with the atmosphere in dilution refrigeration machine 1, it is desirable that opening air valve keeps vacuum test intracavitary
Inert gas be discharged into fast sample room 2 by air inlet/outlet, first flange 31 be equipped with pump port 312, vacuumize list
Member vacuumizes fast sample room 2 by pumping port 312, recycles unit of supplying gas by helium by pumping port 312
Be sent into fast sample room 2 in, the helium in fast sample room 2 enters vacuum test chamber by air inlet/outlet, with to quickly into
Specimen chamber 2 and vacuum test chamber carry out helium purge, are repeated a number of times helium purge later, then take out to fast sample room 2
Vacuum makes the vacuum degree in vacuum test chamber and fast sample room 2 all reach 1 × 10-7Mbar opens gate valve at this time, passes through
Straight spur unit 6 drives inserted link component 3 to move axially, and vacuum test component 5 is sent into dilution refrigeration machine 1 and is surveyed
Examination.Such as: the low-temperature space that vacuum test component 5 can be sent into dilution refrigeration machine 1 carries out physical property characterization to sample.The present embodiment
In above-mentioned unit of supplying gas using the structure that is conveyed in the prior art to inert gas, it is no longer superfluous in detail herein to chat.
Sample is packed into vacuum test chamber and is sealed in glove box by the present embodiment, then vacuum test component 5 is connected
It is connected to inserted link component 3, inserted link component 3 and fast sample room 2 are tightly connected to close to fast sample room 2, to quick
After Sample Room 2 is vacuumized, it is connected to fast sample room 2 with dilution refrigeration machine 1 by gate valve 4, straight spur unit 6
Movement compresses bellows, then inserted link component 3 is driven to move axially to the direction close to dilution refrigeration machine 1, by vacuum
Test component 5 is pushed into dilution refrigeration machine 1 and carries out physical property characterization to sample, realizes the process that sample enters dilution refrigeration machine 1
In ingress of air completely, ensure that accuracy when carrying out physical property characterization using above-mentioned property test system in situ, not only may not be used
To meet the needs of physical property characterizes under all extreme conditions relevant with dilution refrigeration machine, and avoid by dilution refrigeration machine
Characterization measurement sample cargo handling process exposure atmosphere, completely remain the high-intensity magnetic field and pole low temperature environment of 1 script of dilution refrigeration machine.
The sealing ring and first flange 31 that are used between the present embodiment centerboard valve 4 and the contact surface of third flange and
Sealing ring between two flanges is made of anaerobic copper band, other sealings of original position property test system provided in this embodiment
If first fairlead 313 uses the sealing of feedthrough metal and ceramics in inserted link component 3, drawn in vacuum test component 5
Sealing between connector 53, optical lens 54 and valve 55 and installation top cover 51 is installed close between top cover 51 and sample cavity 52
Sealing structure made of indium (In) material, sealing performance with higher can be used in envelope etc..
The present embodiment additionally provides the sample mounting procedure of above-mentioned property test system in situ, Fig. 4 be the present embodiment provides
Property test system in situ sample mounting procedure flow chart, below with reference to Fig. 4 to above-mentioned property test system in situ
Sample mounting procedure describes in detail.
S1, sample is packed into vacuum test is intracavitary, and sealing vacuum test chamber simultaneously takes out out of glove box true in glove box
Hollow testing component 5.
The low-dimensional quantum material of the type of sample such as vacuum film deposition equipment preparation, can also be other equipment system certainly
The sample of standby sample, preparation is entered in glove box by way of switching, to avoid sample ingress of air.
S2, one end that the vacuum test component 5 for being placed with sample is connected to inserted link component 3, later connect inserted link component 3
The one end for connecing vacuum test component 5 is protruded into fast sample room 2, and the other end of inserted link component 3 and fast sample room 2 are sealed
Connection.
S3, fast sample room 2 is evacuated to predetermined vacuum degree, opens valve 55, again vacuumizes fast sample room 2
To predetermined vacuum degree.
S4, it is connected to dilution refrigeration machine 1 with fast sample room 2 by gate valve 4, the movement of straight spur unit 6 makes ripple
Pipe is compressed, and then drives the axial movement of inserted link component 3 vacuum test component 5 to be sent into dilution refrigeration machine 1.
In glove box by sample be packed into vacuum test it is intracavitary after, vacuum test is intracavitary to will be filled with inert gas.Quick
After vacuum degree in Sample Room 2 reaches predetermined vacuum degree, since vacuum test is intracavitary there are inert gas, need to open gas thus
Inert gas is discharged into fast sample room 2 by valve, then is extracted out the inert gas in fast sample room 2 by vacuum unit.
In order to guarantee that the intracavitary atmosphere of vacuum test is consistent with the atmosphere of dilution refrigeration machine 1, by helium to vacuum test
Chamber and fast sample room 2 carry out multiple helium purge, and vacuumize after multiple helium purge to fast sample room 2, make
Vacuum degree in vacuum test chamber and fast sample room 2 reaches predetermined vacuum degree.In the present embodiment, predetermined vacuum degree is preferably 1
×10-7mbar。
Original position property test system provided in this embodiment can also carry out the measurement of electricity transport property to sample, compared to
The difference of the measurement of scanning probe and optics physical property measurement in the present embodiment is the difference of test cell, as to how to sample
It carries out electricity transport property and is measured as the prior art, it is no longer superfluous herein to chat.
Property test system in situ and vacuum sample Preparation equipment may be implemented in the environment for not exposing atmosphere in the present embodiment
Under docking, i.e., product prepared by vacuum sample Preparation equipment is sent into glove box by way of switching, then use this reality
Product is sent into dilution refrigeration machine by the sample mounting procedure for applying the property test system in situ of example offer.
Obviously, the above embodiment of the present invention is just for the sake of clearly illustrating examples made by the present invention, and being not is pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation,
It is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.In addition, term " first ", " second ", only
For descriptive purposes, it is not understood to indicate or imply relative importance.Wherein, term " first position " and " second position "
For two different positions.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
Claims (10)
1. a kind of original position property test system, including dilution refrigeration machine (1), which is characterized in that further include:
Vacuum test component (5) comprising for placing the vacuum test chamber of sample, and to the test that the sample is tested
Unit；
Fast sample room (2), inserted link component (3), one end of the inserted link component (3) are protruded into the fast sample room (2) simultaneously
It is removably tightly connected with the fast sample room (2), the inserted link component (3) can move axially so that the vacuum is surveyed
Try component (5) into and out described dilution refrigeration machine (1)；
Vacuum equipment is capable of providing vacuum environment or inert gas environment, for connecting vacuum sample Preparation equipment, the vacuum
Test component (5) is optionally disposed in the vacuum equipment or takes out out of described vacuum equipment to be removably attachable to
State one end that inserted link component (3) protrudes into the fast sample room (2)；
Gate valve (4), one end are connected to the dilution refrigeration machine (1), and the other end is sealedly attached to the fast sample room
(2), the gate valve (4) can selectively control the dilution refrigeration machine (1) and the fast sample room (2) even on-off
It opens；
Vacuum unit, for being vacuumized to the fast sample room (2).
2. original position property test system according to claim 1, which is characterized in that the vacuum test chamber is equipped with disengaging
Port, the air inlet/outlet are equipped with valve (55).
3. original position property test system according to claim 2, which is characterized in that the inserted link component (3) includes operation
One end of bar (34), the operating stick (34) is connected to the valve (55), and the other end is from one end of the fast sample room (2)
It is pierced by and is tightly connected with the fast sample room (2), the operating stick (34) is configured as controlling the valve (55) movement
So that the vacuum test chamber is connected to or disconnects with the fast sample room (2).
4. original position property test system according to claim 3, which is characterized in that it further include unit of supplying gas, it is described to supply gas
Unit is used to for helium being sent into the fast sample room (2).
5. original position property test system according to claim 3, which is characterized in that the fast sample room (2) includes energy
The bellows of enough axial stretchings；The inserted link component (3) further include:
First flange (31), one end of the bellows are removably tightly connected with the first flange (31), and the other end connects
It is connected to the gate valve (4)；
Multiple connecting rods (33), one end and the first flange (31) of each connecting rod (33) are tightly connected, the other end
It is connected with terminal pad (35).
6. original position property test system according to claim 5, which is characterized in that one end of the test cell is connected with
It draws connector (53), the extraction connector (53) stretches out the vacuum test chamber and is detachably electrically connected with the terminal pad (35)
It connects.
7. original position property test system according to claim 1, which is characterized in that the vacuum test chamber includes sample cavity
(52) the installation top cover (51) of He Yuqi removable seal connection.
8. a kind of sample mounting procedure of property test system in situ as described in any one of claim 1 to 7, which is characterized in that
The following steps are included:
S1, that sample is packed into the vacuum test in the vacuum equipment is intracavitary, seals the vacuum test chamber and from described
The vacuum test component (5) is taken out in vacuum equipment；
S2, the vacuum test component (5) is connected to the inserted link component (3), and the inserted link component (3) is connected into vacuum
One end of test component (5) is protruded into the fast sample room (2), by the fast sample room (2) and the inserted link component (3)
Removably it is tightly connected；
S3, the fast sample room (2) is evacuated to predetermined vacuum degree；
S4, the dilution refrigeration machine (1) is connected to the fast sample room (2) by the gate valve (4), control described insert
The vacuum test component (5) is sent into the dilution refrigeration machine (1) by bar assembly (3) axial movement.
9. the sample mounting procedure of original position property test system according to claim 8, which is characterized in that the vacuum is surveyed
It tries chamber and is equipped with air inlet/outlet, the air inlet/outlet is equipped with valve (55)；
In step sl, by sample be packed into the vacuum test it is intracavitary after, open the valve (55) for inert gas and be sent into institute
State that vacuum test is intracavitary to turn off the valve (55)；
In step s3, after the fast sample room (2) being evacuated to predetermined vacuum degree, open the valve (55) make it is described
The intracavitary inert gas of vacuum test is discharged into the fast sample room (2), and the fast sample room (2) is evacuated to institute again
State predetermined vacuum degree.
10. the sample mounting procedure of original position property test system according to claim 9, which is characterized in that described fast
Before vacuum degree in fast Sample Room (2) reaches the predetermined vacuum degree again, the vacuum test chamber is vacuumized, is more
Secondary helium purge, then the fast sample room (2) is evacuated to the predetermined vacuum degree.
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| CN201910712480.7A CN110320389A (en) | 2019-08-02 | 2019-08-02 | A kind of original position property test system and sample mounting procedure |
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|---|---|---|---|
| CN201910712480.7A CN110320389A (en) | 2019-08-02 | 2019-08-02 | A kind of original position property test system and sample mounting procedure |
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