CN108663276A - A kind of sample Environmental coupling loading device for neutron scattering - Google Patents
A kind of sample Environmental coupling loading device for neutron scattering Download PDFInfo
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- CN108663276A CN108663276A CN201810290189.0A CN201810290189A CN108663276A CN 108663276 A CN108663276 A CN 108663276A CN 201810290189 A CN201810290189 A CN 201810290189A CN 108663276 A CN108663276 A CN 108663276A
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- 230000007613 environmental effect Effects 0.000 title claims abstract description 34
- 230000008878 coupling Effects 0.000 title claims abstract description 33
- 238000010168 coupling process Methods 0.000 title claims abstract description 33
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 33
- 238000001956 neutron scattering Methods 0.000 title claims abstract description 26
- 238000005057 refrigeration Methods 0.000 claims abstract description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 239000010949 copper Substances 0.000 claims abstract description 20
- 238000007789 sealing Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 20
- 230000005540 biological transmission Effects 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 10
- 229910000838 Al alloy Inorganic materials 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 4
- 230000002706 hydrostatic effect Effects 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910001120 nichrome Inorganic materials 0.000 claims description 3
- 230000008859 change Effects 0.000 abstract description 3
- 230000009977 dual effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 description 8
- 238000013461 design Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000011160 research Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- QLZJFWXEALRXPL-UHFFFAOYSA-N C(CCC)N(CCCC)CCCC.[F] Chemical compound C(CCC)N(CCCC)CCCC.[F] QLZJFWXEALRXPL-UHFFFAOYSA-N 0.000 description 1
- 240000008067 Cucumis sativus Species 0.000 description 1
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 241000720974 Protium Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- RVZRBWKZFJCCIB-UHFFFAOYSA-N perfluorotributylamine Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)N(C(F)(F)C(F)(F)C(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F RVZRBWKZFJCCIB-UHFFFAOYSA-N 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000005428 wave function Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
- G01N3/18—Performing tests at high or low temperatures
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- Physics & Mathematics (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
This application discloses a kind of sample Environmental coupling loading devices for neutron scattering.The device of the application, including G M refrigeration machines, high pressure sample room, sample cell and piston；High pressure sample room includes outer barrel and inner cylinder, outer barrel both ends open, and internal thread is set on opening inner wall；Inner cylinder both ends open is interference fitted with outer barrel；Sample cell one end open, open end are downwardly into interior tube inner chamber, are fitted close therewith；Plug is inserted into its cavity by sample tube opening, is fitted close in piston structure；Piston is inserted into inner cylinder by top, is slidably matched therewith, and piston is contacted with sample bottom of the tube；Outer barrel top end opening is closed by upper locking nut, and upper locking nut sets centre bore on central axes, for placing pressure rod；Heat conduction copper post one end connects G M cryocooler cold heads, and the other end is connect with upper locking nut.The device of the application is, it can be achieved that high pressure and the dual load of low temperature, study the structure of matter and change of properties under various dimensions factors to neutron scattering and be of great significance.
Description
Technical field
Sample environment loading equipemtn field in being applied this application involves neutron scattering being used for neutron more particularly to one kind
The sample Environmental coupling loading device of scattering.
Background technology
Under cryogenic, the amplitude reductions such as thermal vibration, rotation of atom in the structure of matter, and phase can occur for Cucumber
Become or show excellent performance, the statistical result of Britain's spallation neutron target show 60% or more neutron scattering experiment be
It is completed under low temperature environment.Therefore, low temperature environment has very important significance for the research field of material science.
Under the conditions of high pressure is extreme, with the increase of substance pressure, the volume of substance tapers into, atom or intermolecular distance
It is gradually shortened, promotes the variation of overlapping degree and free energy between electron wave function, eventually lead to the structure and property of substance
Matter changes, and influence of the high pressure to substance is greatly enriched our material world.
Neutron scattering technology is the hand of the static structure and micro kinetics property using neutron scattering methods research substance
Section.Since neutron does not have charge, there is extremely strong penetrability, the cavity for maintaining sample environment can be passed through, so sample environment
Application of the equipment in neutron spectrometer has advantageous advantage.The measurement of the existing neutron spectrometer in the whole world, about 85% with
On experiment be to be completed on special sample environmental unit.
Special, extreme sample environment is combined with Neutron scattering technology, for expanding material science research space, solution
Certainly great scientific and technical problem and synthesis new material, discovery new phenomenon etc. play extremely important and crucial effect.
But the neutron close to the ultralow temperature and GPa rank super-pressure of absolute zero can not be loaded simultaneously still at present
Scatter sample environment loading device.
Invention content
The purpose of the application is to provide a kind of improved new sample Environmental coupling for neutron scattering of structure and loads dress
It sets.
The application uses following technical scheme：
This application discloses a kind of sample Environmental coupling loading devices for neutron scattering, including G-M refrigeration machines 1, height
Press sample room 2, sample cell 3 and piston 4；High pressure sample room 2 includes outer barrel 21 and inner cylinder 22,21 both ends open of outer barrel, and is opening
Internal thread is opened up on inner wall at mouthful；22 both ends open of inner cylinder, inner cylinder 22 are inserted into outer barrel 21, and the two is in the cylinder being interference fitted
Structure；3 one end open of sample cell, and open end is downwardly into the inner cavity of inner cylinder 22, is fitted close therewith, and sample cell 3 is opened
A plug 31 is inserted at mouthful, plug 31 is inserted into the inner cavity of sample cell 3, is in therewith the tight fit of piston structure, and uses one
A sealing ring seal；In use, being equipped with transmission medium in sample cell 3, hydrostatic pressing is provided for sample；Plug 31 is by lower locking nut
211 fix, and lower locking nut 211 has the external screw thread with the screw-internal thread fit being arranged on the open end inner wall of the outer barrel 21,
Lower ending opening for closing outer barrel 21, while plug is fixed；Piston 4 is inserted into the inner cavity of inner cylinder 22 by top, therewith
It is slidably matched, piston 4 is contacted with the bottom of sample cell 3；The top end opening of outer barrel 21 is closed by upper locking nut 212, by locking
Piston 4 is enclosed in outer barrel 21 by tight nut 212；Upper locking nut 212 has and is arranged on the open end inner wall of outer barrel 21
The external screw thread of screw-internal thread fit, also, centre bore is offered on the central axes of upper locking nut 212, centre bore adds for placing
Compression bar 5 is contacted across centre bore with piston 4 by pressure rod 5；In use, by the conduction of pressure rod 5 and piston 4 to sample cell 3
Apply pressure, so that sample cell 3 is moved down, plug 31 is made to be further inserted into sample cell 3, realizes the extruding to transmission medium,
By transmission medium by pressure transmission to the sample in sample cell 3；The cold head of G-M refrigeration machines 1 connects with one end of heat conduction copper post 6
It connects, the other end of heat conduction copper post 6 is fixedly connected with upper locking nut 212, and G-M refrigeration machines 1 and high pressure sample room 2 are assembled into one
Body；The cold of G-M refrigeration machines 1 is passed into sample cell 3 by heat conduction copper post 6, upper locking nut 212 and piston 4；21 He of outer barrel
Inner cylinder 22 is all prepared using the metal or alloy of nonmagnetic material.
It should be noted that the sample Environmental coupling loading device of the application, when needing high pressure low temperature environment, Ke Yixian
Using special structure design, first pressure rod is inserted into the centre bore of upper locking nut, using general pressue device, in advance
High pressure is applied to sample, at the same time, upper locking nut is screwed, keeps high pressure conditions, then further take out pressure rod, it will be entire high
Pressure sample room is fixedly mounted in heat conduction copper post, is freezed using G-M refrigeration machines, is realized the Environmental coupling of cryogenic high pressure.This
The sample Environmental coupling loading device of application can realize the cryogenic high pressure load of minimum 4.2K temperature, highest 2GPa pressure.Its
In, low temperature part is recycled using helium compressor and cryocooler cold head composition G-M freezes, and by cold head by cold conduct to
In high pressure sample room on sample, which cools down using direct-cooling type, this mode is with easy to operate, cool down soon excellent
Point.The high pressure sample room of outer barrel and inner cylinder composition is symmetrical structure, and sample is in geometry center；Consider to be used under low temperature,
High-pressure chamber core ensures the stability of sample pressure using metal sealing, high pressure sample ceiling portion, that is, open top end
Thread mill drilling on side wall, is easily installed at cold head.
It is appreciated that the sample Environmental coupling loading device of the application is for neutron scattering experiment, therefore, neutron beam
It is as thin as possible that incident and scattering institute by material at channel is necessary for nonmagnetic, chamber wall, to improve neutron scattering experiment efficiency
And the quality of data.Specifically, the non-magnetic material of neutron scattering can refer to conventional neutron scattering experiment material, such as nickel chromium triangle
Aluminium alloy, beallon etc., are not specifically limited herein.
Preferably, the cold head of G-M refrigeration machines 1, heat conduction copper post 6, and entire high pressure sample room 2 are uniformly encapsulated in the
In one shell 7, and high pressure sample room 2 is located at the middle and lower part position of first shell 7, and the middle and lower part position of corresponding first shell 7 is set
It is equipped with the first screen beam window 71, the first screen beam window 71 is prepared using nonmagnetic material.
Preferably, the first screen beam window 71 is detachably secured in first shell 7.
It should be noted that first shell and its first screen beam window are mainly used for maintaining low temperature environment, prevent and reduce
Heat radiation；Wherein, the design of the first screen beam window be in order to make neutron beam can be good at across, facilitate research neutron to sample
Function and effect.
Preferably, first shell 7 is whole is fixed in a vacuum (-tight) housing 8, and vacuum (-tight) housing 8 can be used vacuum system and be taken out
Vacuum provides vacuum environment for entire high pressure sample room 2；Also, likewise, high pressure sample room 2 is located at the middle and lower part of vacuum (-tight) housing 8
The middle and lower part position of position, corresponding vacuum (-tight) housing 8 is provided with vacuum beam window 81, and vacuum beam window 81 is prepared using nonmagnetic material.
Preferably, vacuum beam window 81 is detachably secured on vacuum (-tight) housing 8.
It should be noted that the effect of vacuum (-tight) housing and vacuum beam window is to make entire first shell, high pressure sample room and wherein
Sample cell be in vacuum environment, prevent the warm-up movement of air molecule from passing cold, cause loss of refrigeration capacity；Likewise,
The design of vacuum beam window also for make neutron beam can be good at across.Generally speaking, the purpose of first shell and vacuum (-tight) housing
Loss of refrigeration capacity is exactly reduced, sample is made to maintain under stable low temperature environment.Also, in a kind of realization method of the application,
In the case where maintaining vacuum environment to be damaged without deformation, detection efficient, the first screen beam window are improved to reduce neutron loss
It is all worked into vacuum beam window as thin as possible.
Preferably, the first screen beam window 71 and vacuum beam window 81 all use aluminum alloy material to prepare.
Preferably, the inner surface of the outer surface of inner cylinder 22 and outer barrel 21, the two is respectively according to taper 1:50 carry out finishing
Work realizes the self-locking function of inner cylinder 22 and outer barrel 21 under the conditions of pressure-bearing for stationary fit to be accurately positioned.
It should be noted that the taper of inner barrel and outer barrel is too small, the concentricity of inner barrel and outer barrel can be influenced；And taper mistake
Greatly, then it can lead to the reduction of the high pressure sample room pressure resistance limit；Therefore, 1 is used in a kind of preferred embodiment of the application:50 taper；
It is appreciated that according to different use requirements and above-mentioned principle, can suitably being adjusted to taper, not doing specific limit herein
It is fixed.
Preferably, inner cylinder 22 and outer barrel 21 are interference fitted, wherein the processing interference volume of inner cylinder 22 is 0.05mm.
It should be noted that the processing interference volume of inner cylinder, which refers to the outer diameter of inner cylinder, is slightly larger than the internal diameter of outer barrel, interference volume is
Determined by the pressure-resistant limit of high pressure sample room, interference volume it is too big or it is too small can all cause the pressure-resistant limit to reduce, especially interference
Amount greatly, can also increase the assembling difficulty of inner barrel and outer barrel very much；Therefore, 0.05mm is used in a kind of preferred embodiment of the application
Interference volume.
Preferably, inner cylinder 22 is prepared using nichrome aluminum alloy, and outer barrel 21 is prepared using high intensity beallon.
Preferably, the bottom end of sample cell 3 uses cone face process, and close using sealing ring corresponding with cone face process progress
Envelope.
It should be noted that for sample cell, both ends are one end open, the structure that the other end is not open；Sample
Pipe bottom end be exactly the one end not being open, the one end not being open uses cone face process, is to form one in the outer surface of sample cell
The contour structure of taper, to facilitate sealing ring to be sealed it.
Preferably, it is closed using the sealing ring of annealing copper material between plug and the lower ending opening of outer barrel, to realize
The sealing of high pressure transmission medium.
Preferably, it on the outer wall of high pressure sample room 2, at the position that sample cell 3 accommodates sample, is installed with and adds
Hot device and thermometer, the feedback for sample temperature and control.
It should be noted that the purpose of installation heater and thermometer is can more accurately to control the temperature of sample application
Degree, it will be understood that in the process of refrigeration, in order to maintain under certain low temperature, it is necessarily required to lasting refrigeration, and if refrigeration
Amount is more than required amount, then can be restored the temperature of sample cell to required temperature by heater, reaches and maintains low temperature temperature
Spend stable purpose.
The advantageous effect of the application is：
High pressure and low temperature may be implemented by special structure design in the sample Environmental coupling loading device of the application
Dual load, and use it in neutron scattering research, to studying the structure and property of substance under a variety of dimension factors
Qualitative change is of great significance.
Description of the drawings
Fig. 1 is the structural schematic diagram of sample Environmental coupling loading device in the embodiment of the present application；
Fig. 2 is the schematic cross-sectional view at visual angle shown in Fig. 1, and A figures are the enlarged diagram of the parts A in figure；
Fig. 3 is the structural schematic diagram of sample Environmental coupling loading device another side in the embodiment of the present application；
Fig. 4 is the schematic cross-sectional view at visual angle shown in Fig. 3；
Fig. 5 is the structural schematic diagram of the embodiment of the present application sample Environmental coupling loading device mesohigh sample room；
Fig. 6 is the schematic cross-sectional view of the high pressure sample room at visual angle shown in Fig. 5；
Fig. 7 is the dimensional structure diagram of sample Environmental coupling loading device in the embodiment of the present application.
Specific implementation mode
Low temperature, high pressure are combined with neutron scattering, to study under a variety of dimension factors the structure of substance and
Change of properties is of great significance；This contributes in high-temperature superconductor mechanism, spin Quantum control, new energy materials exploitation, albumen
The research fields such as matter interaction, magnetic phase transition and magnetic structure obtain important breakthrough achievement.However, in spallation neutron target, still
The device of the dual load of low temperature, high pressure can not be realized effectively.Although being loaded there is also low temperature or high pressure in other fields
Device still all cannot be satisfied the extreme sample environment of neutron scattering demand, it is difficult to realize while load close to absolute zero
The sample environment of ultralow temperature and GPa rank super-pressure.For this purpose, the application especially has developed a kind of sample Environmental coupling of new construction
Loading device can apply high pressure to sample in advance, then be realized again by G-M refrigeration machines using its special structure design
The high pressure of low temperature, the low temperature load and 1atm-2GPa that can be realized simultaneously 300-4.2K loads.
It should be noted that in the application the directions word such as upper and lower, left and right, upper locking nut, lower locking nut, top or
With the structure feature of directional correlation, be all with the orientation towards user when sample Environmental coupling loading device normal use,
The description of the present application attached drawing can be referred to；It is appreciated that these direction words and the structure feature with directional correlation, direction refer to
To being intended merely to facilitate explanation and understanding.
The application is described in further detail below by specific embodiment.Following embodiment is only to the application into traveling
One step illustrates, should not be construed as the limitation to the application.
Embodiment
This example is used for the sample Environmental coupling loading device of neutron scattering, as shown in Figures 1 to 7, including G-M refrigeration machines 1,
High pressure sample room 2, sample cell 3 and piston 4.Wherein, high pressure sample room 2 include outer barrel 21 and inner cylinder 22,21 both ends open of outer barrel,
And open up internal thread on the inner wall of opening；22 both ends open of inner cylinder, inner cylinder 22 are inserted into outer barrel 21, and the two is in interference fit
Cylindrical structure.In this example, the combination assembly of inner cylinder 22 and outer barrel 21 is the core of high pressure sample room, 22 appearance of inner cylinder
Face and 21 inner surface of outer barrel are respectively according to taper 1:50 are finished, for stationary fit to be accurately positioned and inner/outer tube can held
There is self-locking function under the conditions of pressure.Further, to provide the pressure-resistant limit of high pressure sample room, inner cylinder 22 and outer barrel 21 need to carry out
Interference fit, specifically, the processing interference volume of inner cylinder is 0.05mm.In addition, Material Strength is the key that ensure the pressure-resistant limit, because
This, in this example, inner cylinder 22 is prepared using nichrome aluminum alloy, and outer barrel 21 is prepared using high intensity beallon, yield strength difference
About 2.0GPa and 1.2GPa.Also, the internal thread of 21 upper and lower side of outer barrel design, the i.e. threaded hole at both ends, aperture is equal, and
The diameter of threaded hole is more than the diameter of inner cylinder 22.
As shown in Figure 5 and Figure 6,3 one end open of sample cell, and open end is downwardly into the inner cavity of inner cylinder 22, therewith tightly
The opening of close fit, sample cell 3 is inserted into a plug 31, and plug 31 is inserted into the inner cavity of sample cell 3, is in piston structure therewith
It is fitted close, and hydrostatic pressing is provided in use, being equipped with transmission medium in sample cell 3 for sample using a sealing ring seal；
Plug 31 is fixed by lower locking nut 211, and lower locking nut 211 has and the internal thread that is arranged on the open end inner wall of outer barrel 21
The external screw thread of cooperation, the lower ending opening for closing outer barrel 21, while plug is fixed；Piston 4 is inserted into inner cylinder by top
22 inner cavity, is slidably matched therewith, and piston 4 is contacted with the bottom of sample cell 3；The top end opening of outer barrel 21 is by upper locking nut
Piston 4, is enclosed in outer barrel 21 by 212 closings by upper locking nut 212；Upper locking nut 212 has the opening with outer barrel 21
The external screw thread for the screw-internal thread fit being arranged on the inner wall of end, also, centre bore is offered on the central axes of upper locking nut 212, in
Heart hole is contacted across centre bore with piston 4 for placing pressure rod 5 by pressure rod 5.The sample tube wall of this example is as thin as possible, outside
Diameter is fitted close with inner cylinder internal diameter, and sample bore is as big as possible, in order to accommodate more samples.
In order to further increase the pressure leakproofness and stability of sample area, sample cell bottom end and two sealing rings are bored
Face processes, and sample cell bottom end can be embedded in corresponding sealing ring after processing, sample cell open at one end and sealing ring cone face process
End in contact.The sealing ring of this example is processed using annealing copper material, and annealing copper material is soft, is easily deformed under high pressure, to real
The sealing of existing high pressure transmission medium.The transmission medium of this example is encapsulated in sample cell and sample is used in mixed way, and transmission medium is complete
Fluorine tri-n-butylamine organic solvent is prevented from generating stronger incoherent scattering to neutron scattering without protium, be made to neutron scattering spectra
At compared with highback bottom.The perfluorotributylamine that this example uses does not cure in 2.5GPa or less, and good hydrostatic pressing can be provided for sample.
In use, the conduction by pressure rod 5 and piston 4 applies pressure to sample cell 3, so that sample cell 3 is moved down, make
Plug 31 is further inserted into sample cell 3, the extruding to transmission medium is realized, by transmission medium by pressure transmission to sample cell
Sample in 3.
The cold head of the G-M refrigeration machines 1 of this example is connect with one end of heat conduction copper post 6, the other end of heat conduction copper post 6 and upper locking
Nut 212 is fixedly connected, and G-M refrigeration machines 1 and high pressure sample room 2 are assembled into one；Pass through heat conduction copper post 6, upper locking nut
212 and piston 4 cold of G-M refrigeration machines 1 is passed into sample cell 3；Outer barrel 21 and inner cylinder 22 all use the gold of nonmagnetic material
Belong to or is prepared by alloy.
In the present embodiment, low temperature portion is divided into sample and provides low temperature environment.It is cold that high pressure sample room is placed on G-M refrigerants bottom
, it can be achieved that cold is quickly transferred at sample on head, cooling purpose is realized.The realization of this example refrigerating function is compressed using helium
Machine freezes with cryocooler cold head composition G-M cycles, and is conducted cold into high pressure sample room on sample by cold head, this
Example cools down using direct-cooling type, has the advantages that easy to operate, cooling is fast.Certainly, according to experiment condition demand, rate of temperature fall
High-power G-M refrigeration machines should be used as quickly as possible.
In further improvement project, cold head, heat conduction copper post 6 and the entire high pressure sample of the G-M refrigeration machines 1 of this example
Room 2 is uniformly encapsulated in first shell 7, and first shell 7 is whole to be fixed in a vacuum (-tight) housing 8, and vacuum (-tight) housing 8 can be used
Vacuum system is vacuumized, and vacuum environment is provided for entire high pressure sample room 2.Wherein, high pressure sample room 2 is located at first shell
The middle and lower part position of 7 middle and lower part position, corresponding first shell 7 is provided with the first screen beam window 71, corresponding with the first screen beam window 71
Vacuum beam window 81 is provided on the vacuum (-tight) housing 8 of position.First screen beam window 71 and vacuum beam window 81 are all prepared using nonmagnetic material,
To facilitate neutron beam to pass through, this example specifically uses aluminium alloy to prepare.
First shell is used for maintaining low temperature environment, prevents heat radiation；Vacuum (-tight) housing is used for keeping vacuum environment, prevents air point
The warm-up movement of son passes cold, causes loss of refrigeration capacity.First screen beam window and vacuum beam window are that neutron incidence and scattering are logical
Detection efficient is improved, two beam windows are processed as thin as possible in the case where ensureing security situation at this to reduce neutron loss in road.Specifically,
First screen beam window is not subject to pressure, and being processed according to working ability keeps it as thin as possible, according to current working ability and makes
Thickness with service life the first screen beam window is 0.8-1.0mm, and this example is specially 1.0mm；Vacuum beam window bears an atmospheric pressure, needs
It is processed according to pressure-resistant thickness results are calculated, the vacuum beam window thickness of this example is 1.0-1.2mm, and specific this example is
1.2mm。
Sample Environmental coupling loading device of this example for neutron scattering can be assembled in the following way：
(1) high pressure sample room is assembled
Using press, first inner cylinder 22 is pressed into outer barrel 21, is until inner cylinder both ends of the surface are concordant with outer barrel screw hole both ends of the surface
Only.Then lower cushion block is put into the groove of lower locking nut 211, lower locking nut 211 is screwed into 21 bottom thread hole of outer barrel
In, until tightening.Then by seal ring set in 31 path one end of plug, sealing ring circular conical surface is in path end face side, so
3 open end of sample cell is inserted into plug path afterwards, which is put into inner cylinder center hole, then at the center circle of inner cylinder
Sealing ring is put into hole, sealing ring circular conical surface and the top conical face that sample cell is not open are tangent.Then piston 4 is put into inner cylinder
Center hole in, upper cushion block is put into 212 groove of upper clamp nut, upper clamp nut is screwed into the internal thread on outer barrel top
Kong Zhong, until tightening.
When needing pressurization, pressure rod 5 is put into the centre bore of upper locking nut, high pressure sample room is moved in press,
Gradually apply pressure, tighten upper locking nut after applying pressure every time, until being loaded onto goal pressure, and by upper locking nut
Until tightening.
(2) low-temperature components assemble
Flange 9 is placed in eminence, then vacuum (-tight) housing 8 is put into, has seal groove at the two interface, is put into O-ring
Carry out vacuum sealing.Connection component is placed in 8 upper surface of vacuum (-tight) housing, equally carries out vacuum sealing using O-ring, it will using screw
Three tightens up.Heat conduction copper post 6 is fixed on the cold head of 1 bottom end of G-M refrigeration machines, then by 1 company of being fixed on of G-M refrigeration machines
On connected components, equally vacuum sealing is carried out using O-ring.
(3) sample Environmental coupling loading device assembles
Finally high pressure sample ceiling end is screwed on the bolt below heat conduction copper post, is consolidated at sample in high pressure sample room
Determine thermometer and heater and be wired on ten needle aviation interfaces, by the first screen beam window 71 and vacuum beam window 81 respectively into
Row is connected and fixed, and vacuum beam window 81 is attached with vacuum (-tight) housing 8 using Quick Release clip, and carries out vacuum sealing, more convenient for sample
It changes.
Vacuum, leak rate detection are carried out to the sample Environmental coupling loading device of this example, specifically, by KF25 flanges respectively with
Vacuum pump is connected with leak detector, opens vacuum pump, and vacuum degree carries out leak rate detection after meeting the requirements.It is wanted as vacuum degree is not met
It asks, please checks sealing surface bolt one by one, repeat to fasten.After vacuum degree and leak rate all meet the requirements, cooling process can be carried out.This
The vacuum degree of example is less than 10-3Pa, leak rate are less than 1 × 10-9Pa.m3/ s, meets design requirement.
When needing pressurization, pressure rod is put into the centre bore of upper locking nut, high pressure sample room is moved in press, by
Gradually apply pressure, tightens upper locking nut after applying pressure every time, until being loaded onto goal pressure.After the completion of pressurization, take out
Pressure rod carries out the assembly of sample Environmental coupling loading device according to preceding method.By temperature controller access ten needle Aviation Connectors on
After carry out cooling process.After temperature is down to target temperature, you can carry out neutron scattering experiment.
This example is used for the sample Environmental coupling loading device of neutron scattering, and high pressure sample room is connected directly between G-M refrigeration machines
On, while high pressure, cryogenic sample environment being provided, the high pressure of the low temperature load and 1atm-2GPa of 300-4.2K may be implemented in this example
Load so that be carried out at the same time the research that various dimensions factor influences substance and may be implemented, disclosure satisfy that neutron scattering uses.
The foregoing is a further detailed description of the present application in conjunction with specific implementation manners, and it cannot be said that this Shen
Specific implementation please is confined to these explanations.For those of ordinary skill in the art to which this application belongs, it is not taking off
Under the premise of conceiving from the application, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to the protection of the application
Range.
Claims (10)
1. a kind of sample Environmental coupling loading device for neutron scattering, it is characterised in that：Including G-M refrigeration machines (1), high pressure
Sample room (2), sample cell (3) and piston (4)；
The high pressure sample room (2) includes outer barrel (21) and inner cylinder (22), outer barrel (21) both ends open, and in opening
Internal thread is opened up on inner wall；Inner cylinder (22) both ends open, inner cylinder (22) are inserted into outer barrel (21), and the two is in interference fit
Cylindrical structure；
Sample cell (3) one end open, and open end is downwardly into the inner cavity of inner cylinder (22), is fitted close therewith, sample
The opening for managing (3) is inserted into a plug (31), and plug (31) is inserted into the inner cavity of sample cell (3), is in the tight of piston structure therewith
Close fit, and using a sealing ring seal；In use, being equipped with transmission medium in the sample cell (3), hydrostatic is provided for sample
Pressure；
The plug (31) is fixed by lower locking nut (211), and lower locking nut (211) has the opening with the outer barrel (21)
The external screw thread for the screw-internal thread fit being arranged on the inner wall of end, the lower ending opening for closing outer barrel (21), and the fixed plug
(31)；
The piston (4) is inserted into the inner cavity of the inner cylinder (22) by top, is slidably matched therewith, piston (4) and sample cell (3)
Bottom contacts；
The top end opening of the outer barrel (21) is closed by upper locking nut (212), and by upper locking nut (212) by the piston
(4) it is enclosed in outer barrel (21)；
The upper locking nut (212) has the outer spiral shell with the screw-internal thread fit being arranged on the open end inner wall of the outer barrel (21)
Line, the upper end opening for closing outer barrel (21), also, offer centre bore, center on the central axes of upper locking nut (212)
Hole is contacted across centre bore with piston (4) for placing pressure rod (5) by pressure rod (5)；In use, by pressure rod (5) and
The conduction of piston (4) applies pressure to sample cell (3), so that sample cell (3) is moved down, while plug (31) being made to be further inserted into
In sample cell (3), the extruding to transmission medium is realized, by transmission medium by pressure transmission to the sample in sample cell (3)；
The cold head of the G-M refrigeration machines (1) is connect with one end of heat conduction copper post (6), the other end of heat conduction copper post (6) with it is described on
Locking nut (212) is fixedly connected, and G-M refrigeration machines (1) and high pressure sample room (2) are assembled into one；Pass through heat conduction copper post
(6), the cold of G-M refrigeration machines (1) is passed to sample cell (3) by upper locking nut (212) and piston (4)；
The outer barrel (21) and inner cylinder (22) are all prepared using the metal or alloy of nonmagnetic material.
2. sample Environmental coupling loading device according to claim 1, it is characterised in that：The G-M refrigeration machines (1) it is cold
Head, heat conduction copper post (6), and entire high pressure sample room (2), are uniformly encapsulated in first shell (7), and high pressure sample room
(2) it is located at the middle and lower part position of first shell (7), the middle and lower part position of corresponding first shell (7) is provided with the first screen beam window (71),
The first screen beam window (71) is prepared using nonmagnetic material；Preferably, the first screen beam window (71) is detachably secured to described
In first shell (7).
3. sample Environmental coupling loading device according to claim 2, it is characterised in that：The first shell (7) is whole
It is fixed in a vacuum (-tight) housing (8), vacuum (-tight) housing (8) can be used vacuum system and be vacuumized, and be entire high pressure sample room (2)
Vacuum environment is provided；Also, likewise, high pressure sample room (2) are located at the middle and lower part position of vacuum (-tight) housing (8), corresponding vacuum (-tight) housing (8)
Middle and lower part position be provided with vacuum beam window (81), the vacuum beam window (81) is prepared using nonmagnetic material；Preferably, vacuum beam
Window (81) is detachably secured on the vacuum (-tight) housing (8).
4. sample Environmental coupling loading device according to claim 3, it is characterised in that：The first screen beam window (71) and
Vacuum beam window (81) all uses aluminum alloy material to prepare.
5. according to claim 1-4 any one of them sample Environmental coupling loading devices, it is characterised in that：The inner cylinder (22)
Outer surface and the outer barrel (21) inner surface, the two is respectively according to taper 1:50 are finished, for stationary fit with
It is accurately positioned, to realize the self-locking function of inner cylinder (22) and outer barrel (21) under the conditions of pressure-bearing.
6. according to claim 1-4 any one of them sample Environmental coupling loading devices, it is characterised in that：The inner cylinder (22)
It is interference fitted with outer barrel (21), wherein the processing interference volume of the inner cylinder (22) is 0.05mm.
7. according to claim 1-4 any one of them sample Environmental coupling loading devices, it is characterised in that：The inner cylinder (22)
It is prepared using nichrome aluminum alloy, the outer barrel (21) is prepared using high intensity beallon.
8. according to claim 1-4 any one of them sample Environmental coupling loading devices, it is characterised in that：The sample cell
(3) bottom end uses cone face process, and is sealed using sealing ring corresponding with cone face process.
9. according to claim 1-4 any one of them sample Environmental coupling loading devices, it is characterised in that：The plug (31)
It is closed using the sealing ring of annealing copper material between the lower ending opening of the outer barrel (21), to realize high pressure transmission medium
Sealing.
10. according to claim 1-4 any one of them sample Environmental coupling loading devices, it is characterised in that：The high pressure-like
On the outer wall of product room (2), at the position that sample cell (3) accommodates sample, having heaters and thermometer is fixedly mounted, is used for
The feedback of sample temperature and control.
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| CN201810290189.0A CN108663276B (en) | 2018-04-03 | 2018-04-03 | Sample environment coupling loading device for neutron scattering |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109596647A (en) * | 2018-12-01 | 2019-04-09 | 金华职业技术学院 | A method of for neutron scattering experiment |
| CN109758976A (en) * | 2018-12-24 | 2019-05-17 | 中国科学院广州能源研究所 | A kind of neutron diffraction hydrate high pressure generating means |
| CN109991255A (en) * | 2019-05-22 | 2019-07-09 | 中国科学技术大学 | A kind of high pressure chest piston cylinder and its manufacturing method for X-ray scattering |
| CN110823768A (en) * | 2019-11-21 | 2020-02-21 | 中国核动力研究设计院 | Device and method for researching interface compatibility of solid material |
| CN110865318A (en) * | 2019-10-23 | 2020-03-06 | 散裂中子源科学中心 | Method for detecting safe magnetic environment of magnet and application thereof |
| CN113960084A (en) * | 2021-09-14 | 2022-01-21 | 散裂中子源科学中心 | In-situ high-temperature and high-pressure experimental device for small-angle scattering |
| CN116380664A (en) * | 2023-04-14 | 2023-07-04 | 北京航空航天大学 | Bridgman piston pressurizing device for measuring comprehensive physical properties of sample |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01129193A (en) * | 1987-11-16 | 1989-05-22 | Toshiba Corp | Control rod assembly |
| JPH0481691A (en) * | 1990-07-25 | 1992-03-16 | Hitachi Ltd | Fuel assembly for fast reactor |
| CN205263003U (en) * | 2015-12-08 | 2016-05-25 | 东莞中子科学中心 | A sample box mobile device for neutron scattering experiment |
| CN205263002U (en) * | 2015-12-08 | 2016-05-25 | 东莞中子科学中心 | A sample box for neutron scattering experiment |
| CN106514495A (en) * | 2016-12-30 | 2017-03-22 | 青岛理工大学 | Expansion machine driven refrigeration low-temperature cooling nano particle jet flow minimal quantity lubrication supply system |
| CN206339501U (en) * | 2016-12-22 | 2017-07-18 | 东莞中子科学中心 | Neutron scattering gases at high pressure sample box |
| CN107290363A (en) * | 2017-07-25 | 2017-10-24 | 中国科学院物理研究所 | High-pressure low-temperature in-situ neutron scattering device |
-
2018
- 2018-04-03 CN CN201810290189.0A patent/CN108663276B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01129193A (en) * | 1987-11-16 | 1989-05-22 | Toshiba Corp | Control rod assembly |
| JPH0481691A (en) * | 1990-07-25 | 1992-03-16 | Hitachi Ltd | Fuel assembly for fast reactor |
| CN205263003U (en) * | 2015-12-08 | 2016-05-25 | 东莞中子科学中心 | A sample box mobile device for neutron scattering experiment |
| CN205263002U (en) * | 2015-12-08 | 2016-05-25 | 东莞中子科学中心 | A sample box for neutron scattering experiment |
| CN206339501U (en) * | 2016-12-22 | 2017-07-18 | 东莞中子科学中心 | Neutron scattering gases at high pressure sample box |
| CN106514495A (en) * | 2016-12-30 | 2017-03-22 | 青岛理工大学 | Expansion machine driven refrigeration low-temperature cooling nano particle jet flow minimal quantity lubrication supply system |
| CN107290363A (en) * | 2017-07-25 | 2017-10-24 | 中国科学院物理研究所 | High-pressure low-temperature in-situ neutron scattering device |
Non-Patent Citations (2)
| Title |
|---|
| 王铜: "中国散裂中子源控制网测量方案及数据处理", 《地理空间信息》 * |
| 胡海韬: "中国散裂中子源小型非直冷式低温恒温器技术", 《低温工程》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109596647A (en) * | 2018-12-01 | 2019-04-09 | 金华职业技术学院 | A method of for neutron scattering experiment |
| CN109596647B (en) * | 2018-12-01 | 2023-08-29 | 金华职业技术学院 | Method for neutron scattering experiment |
| CN109758976A (en) * | 2018-12-24 | 2019-05-17 | 中国科学院广州能源研究所 | A kind of neutron diffraction hydrate high pressure generating means |
| CN109758976B (en) * | 2018-12-24 | 2021-07-27 | 中国科学院广州能源研究所 | High-pressure generation device for neutron diffraction hydrate |
| CN109991255A (en) * | 2019-05-22 | 2019-07-09 | 中国科学技术大学 | A kind of high pressure chest piston cylinder and its manufacturing method for X-ray scattering |
| CN109991255B (en) * | 2019-05-22 | 2024-01-05 | 中国科学技术大学 | High-pressure cavity piston cylinder for X-ray scattering and manufacturing method thereof |
| CN110865318A (en) * | 2019-10-23 | 2020-03-06 | 散裂中子源科学中心 | Method for detecting safe magnetic environment of magnet and application thereof |
| CN110823768A (en) * | 2019-11-21 | 2020-02-21 | 中国核动力研究设计院 | Device and method for researching interface compatibility of solid material |
| CN110823768B (en) * | 2019-11-21 | 2023-02-28 | 中国核动力研究设计院 | Device and method for researching interface compatibility of solid material |
| CN113960084A (en) * | 2021-09-14 | 2022-01-21 | 散裂中子源科学中心 | In-situ high-temperature and high-pressure experimental device for small-angle scattering |
| CN113960084B (en) * | 2021-09-14 | 2023-09-19 | 散裂中子源科学中心 | In-situ high-temperature high-pressure experimental device for small-angle scattering |
| CN116380664A (en) * | 2023-04-14 | 2023-07-04 | 北京航空航天大学 | Bridgman piston pressurizing device for measuring comprehensive physical properties of sample |
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