CN110031445A - A kind of Raman spectrum experimental provision under cryogenic conditions - Google Patents
A kind of Raman spectrum experimental provision under cryogenic conditions Download PDFInfo
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- CN110031445A CN110031445A CN201910347060.3A CN201910347060A CN110031445A CN 110031445 A CN110031445 A CN 110031445A CN 201910347060 A CN201910347060 A CN 201910347060A CN 110031445 A CN110031445 A CN 110031445A
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- 239000013307 optical fiber Substances 0.000 claims abstract description 163
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- 229920006362 Teflon® Polymers 0.000 claims abstract description 80
- 230000003287 optical effect Effects 0.000 claims abstract description 57
- 239000000835 fiber Substances 0.000 claims abstract description 49
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 46
- 239000010935 stainless steel Substances 0.000 claims abstract description 46
- 238000001816 cooling Methods 0.000 claims abstract description 41
- 239000011324 bead Substances 0.000 claims abstract description 30
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 239000003822 epoxy resin Substances 0.000 claims abstract description 21
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 21
- 230000001681 protective effect Effects 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000011241 protective layer Substances 0.000 claims description 13
- 238000005299 abrasion Methods 0.000 claims description 9
- 239000011229 interlayer Substances 0.000 claims description 9
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- BVPWJMCABCPUQY-UHFFFAOYSA-N 4-amino-5-chloro-2-methoxy-N-[1-(phenylmethyl)-4-piperidinyl]benzamide Chemical compound COC1=CC(N)=C(Cl)C=C1C(=O)NC1CCN(CC=2C=CC=CC=2)CC1 BVPWJMCABCPUQY-UHFFFAOYSA-N 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
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- 238000000034 method Methods 0.000 abstract description 11
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- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 4
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
The present invention relates to new materials to research and develop field, a kind of Raman spectrum experimental provision under cryogenic conditions, including cooling chamber, vacuum chamber, sample room, sample, optical fiber I, optical feed trough, air inlet pipe, escape pipe, optics cavity, color separation filter, notch(ing) filter, fiber coupler I, plane mirror, optical fiber collimator, fiber coupler II, optical fiber II, optical detector, optical fiber III, laser, cable and computer, optical feed trough includes fastener I, fastener II, Teflon plug, protective case, stainless steel tube, epoxy resin, supporting bead group and small space, optical fiber is introduced by vacuum chamber using the compact type vacuum feedthrough of special designing, with the direct fiber coupling suitable for the experiment of low temperature Raman spectrum, the assembling process that optical fiber introduces vacuum chamber avoids extruding and distortion to optical fiber, optical fiber is reduced to introduce The risk being broken in the assembling process of vacuum chamber, and the position of optical fiber can be adjusted in situ, and can be improved service life.
Description
Technical field
The present invention relates to new materials to research and develop field, especially a kind of to carry out Raman spectrum experiment under cryogenic
A kind of Raman spectrum experimental provision under cryogenic conditions.
Background technique
Raman spectrum is a kind of scattering spectrum, is to be analyzed the scattering spectrum different from incident light frequency to be divided
Son vibration, rotation aspect information, and it is applied to a kind of analysis method of molecular structure research, certain raman spectroscopy measurement experiments need
It to be carried out under low temperature and vacuum condition, it is therefore desirable to optical fiber is introduced into vacuum system, generally use epoxy in the prior art
Resin is sealed between optical fiber and vacuum cavity, and the hollow conic Teflon plug that passing through will be nested in outside optical fiber is inserted into
One stainless steel tube, and reach air-tightness with the method for fastened by screw, this encapsulating method causes the pressure to optical fiber excessive
To lead to optical attenuation, fibercuts is even resulted in, moreover, serious deformation can occur for Teflon plug after reusing for several times,
Leakproofness is caused to decline, the Raman spectrum experimental provision under a kind of cryogenic conditions is able to solve problem.
Summary of the invention
To solve the above-mentioned problems, the device of the invention is introduced optical fiber using the compact type vacuum feedthrough of special designing
Vacuum chamber, with the direct fiber coupling suitable for the experiment of low temperature Raman spectrum, the assembling process that optical fiber introduces vacuum chamber is avoided
Extruding and distortion to optical fiber, and the position of optical fiber can be adjusted in situ.
The technical scheme adopted by the invention is that:
Raman spectrum experimental provision under a kind of cryogenic conditions includes cooling chamber, vacuum chamber, sample room, sample, light
Fine I, optical feed trough, air inlet pipe, escape pipe, optics cavity, color separation filter, notch(ing) filter, fiber coupler I, plane mirror, light
Fine collimator, fiber coupler II, optical fiber II, optical detector, optical fiber III, laser, cable and computer, xyz are three-dimensional space
Between coordinate system, cooling chamber have low temperature interlayer, by by the helium of low temperature be passed through the low temperature interlayer with can to cooling chamber into
Row cooling, experimental temperature range is from 20K to 120K, and cooling chamber has control arm, and vacuum chamber and sample room are connected to from top to bottom
In cooling chamber, sample is located in sample room, and internal vacuum chamber is equipped with adsorption pump, and the barometric minimum of vacuum chamber is enabled to reach
10-4Pascal, vacuum chamber have bottom through-hole, and edge the upper side and lower side of the bottom through-hole all has the flange edge of a knife, optical fiber I
With optical fiber I protective layer and optical fiber I core wire, the lower end of optical fiber I is located in sample room, upper end is connected to optics cavity, and optics cavity is divided
Colo(u)r filter, notch(ing) filter, fiber coupler I, plane mirror, optical fiber collimator, fiber coupler II, optical fiber II and optical detection
Device is respectively positioned in vacuum chamber, and optical detector, optical fiber II, fiber coupler I, notch(ing) filter and optics cavity successively connect from top to bottom
It connects, color separation filter is located in optics cavity, and laser is located at outside cooling chamber, laser, optical fiber III, fiber coupler II and light
Fine collimator is sequentially connected from top to bottom, and the upper surface of notch(ing) filter is fixed in one end of optical fiber collimator, can pass through optical fiber
Micro- helicitic texture inside collimator changes the position of fiber coupler II, to adjust the position of hot spot of the laser on plane mirror
It sets, plane mirror is located at the side of the optics cavity below optical fiber collimator, can be successively by laser, optical fiber III, fiber coupler
II, optical fiber collimator, plane mirror, color separation filter and optical fiber I form input path, can be successively by sample, optical fiber I, color separation
Optical filter, notch(ing) filter, fiber coupler I, optical fiber II and optical detector form reflected light path；Air inlet pipe and an air outlet pipe it is upper
The top being respectively positioned on outside cooling chamber, lower end is held to be respectively positioned in sample room after vacuum chamber；Optical detector and laser are electric respectively
Cable connects computer, and the optical information collected can be passed through cable transmission to computer by optical detector；Optical feed trough includes
Fastener I, fastener II, Teflon plug, protective case, stainless steel tube, epoxy resin, supporting bead group and small space, fastener I
Be it is hollow and there is external screw thread, there is cone shaped opening, fastener II has internal screw thread and bottom has thoroughly below fastener I
Hole, fastener I and fastener II are located at the upper side and lower side of the bottom through-hole of vacuum chamber and threaded connection, fastener I and
Fastener II is engaged with the flange edge of a knife of bottom through-hole edge the upper side and lower side of vacuum chamber respectively, so that fastener I and fastening
There is air-tightness, optical feed trough, vacuum chamber and cooling chamber all have airtight between any two between part II and vacuum chamber bottom through-hole
Property, the tightness of fastener I and fastener II can be adjusted by cooling chamber control arm；Teflon plug include be integrally machined and
At axis upper hollow rotary table and lower hollow cylindrical body in the y-direction, the hollow part forms Teflon plug along the side y
To through hole, the frustum cone side is adapted mating with the cone shaped opening below fastener I, passes through below Teflon plug
Supporting bead group is crimped on the upper surface of the open-work of the bottom fastener II, and supporting bead group is by two metals that are overlapped and being bonded
Washer composition, the surface of the metal washer is by polishing, so that the frictional resistance very little between two metal washers, works as Teflon
When dragon plug is around center axis rotation, supporting bead group can play a protective role to Teflon plug to reduce the abrasion of Teflon plug；
In the fastener cycle of fastener I and fastener II, fastener II is exerted a force by lower part of the supporting bead group to Teflon plug, is made
Teflon plug is forced upward into the cone shaped opening below fastener I, and between fastener I, fastener II and Teflon plug
A small space is formed, the clast that Teflon plug is generated due to abrasion can be accumulated in the small space；Stainless steel tube from
Top to bottm is nested into fastener I, Teflon plug and fastener II, and by polishing, optical fiber I is nested in the inner surface of stainless steel tube
In stainless steel tube, the part fiber I protective layer of optical fiber I is removed, the optical fiber I core wire that exposed length is 10 millimeters, and uses ring
After oxygen resin will wrap up at the optical fiber I core wire of the exposing, optical fiber I is nested into stainless steel tube, after epoxy resin solidification,
Optical fiber I is capable of fixing with stainless steel tube, and there is optical fiber I the epoxy resin that length is 10 millimeters of non-fiber I protective layer to wrap up section,
The optical fiber I core wire wrapped up in section can be adhesively fixed by epoxy resin with stainless steel pipe inner surface, and make the package section
Beyond the Great Wall in square fastener I, the outside nesting of stainless steel tube is fixed with protective case, protective case position for Teflon in fastener I
At 20 millimeters below the fastener II；The open-work diameter of the bottom fastener II is 4.8 millimeters；The rotary table on the top of Teflon plug
Upper bottom surface radius is 4 millimeters, bottom radius surface is 8.2 millimeters, is highly 6 millimeters, the cylindrical body bottom surface of the lower part of Teflon plug
Radius is 6 millimeters, is highly 5.2 millimeters, and the diameter of the through hole in the y-direction of Teflon plug is 3.8 millimeters；Stainless steel tube
Internal diameter is 0.6 millimeter, outer diameter is 3.6 millimeters, and the tube wall of stainless steel tube is thicker, can be avoided and generates transition extruding to optical fiber I；Branch
The metal washer internal diameter for supportting washer sets is 4 millimeters, outer diameter is 12 millimeters.
The step of being tested using the Raman spectrum experimental provision under a kind of cryogenic conditions are as follows:
Step 1 adjusts the fastener I and fastener II of optical feed trough by the control arm of cooling chamber, so that stainless steel tube
And the lower end of optical fiber I is located at suitable position in sample；
Step 2, by the way that the helium of low temperature to be passed through to the low temperature interlayer of cooling chamber to carry out being cooled to 150K to cooling chamber；
Step 3 opens vacuum chamber (2) internal adsorption pump, so that vacuum chamber (2) interior vacuum reaches 10-4Pascal is cold
But chamber (1) continues to be cooled to 100K；
Reaction gas is passed through in sample room, reaction gas and example reaction by step 4 from air inlet pipe；
Step 5 adjusts the position of optical fiber collimator, so that the laser of laser transmitting successively passes through optical fiber III, optical fiber
Coupler II, optical fiber collimator, plane mirror, color separation filter and optical fiber I, are incident on sample, and the wavelength of the laser is received for 532
Rice, the power of laser are 50 milliwatts；
Step 6, the Raman light generated in sample successively pass through optical fiber I, color separation filter, notch(ing) filter, fiber coupling
Device I and optical fiber II, into optical detector；
Step 7, the data for the Raman light that optical detector collects are transmitted to computer, after computer analysis processing
To the corresponding information of Raman light.
The beneficial effects of the present invention are:
Optical fiber is introduced vacuum chamber using the vacuum feedthrough of special designing by apparatus of the present invention, is reduced optical fiber and is being introduced very
The risk being broken in the assembling process of cavity, and the position of optical fiber can be adjusted in situ, and can be improved service life.
Detailed description of the invention
It is further illustrated below with reference to figure of the invention:
Fig. 1 is schematic diagram of the present invention；
Fig. 2 is optical feed trough partial enlargement diagram.
In figure, 1. cooling chambers, 2. vacuum chambers, 3. sample rooms, 4. samples, 5. optical fiber I, 5-1. optical fiber I protective layers, 5-2. light
Fine I core wire, 6. optical feed troughs, 6-1. fastener I, 6-2. fastener II, 6-3. Teflon plug, 6-4. protective case, 6-5. are stainless
Steel pipe, 6-6. epoxy resin, 6-7. supporting bead group, the small space 6-8., 7. air inlet pipe, 8. escape pipes, 9. optics cavities, 10. points
Colo(u)r filter, 11. notch(ing) filters, 12. fiber coupler I, 13. plane mirrors, 14. optical fiber collimators, 15. fiber couplers
II, 16. optical fiber II, 17. optical detectors, 18. optical fiber III, 19. lasers.
Specific embodiment
If Fig. 1 is schematic diagram of the present invention, including cooling chamber (1), vacuum chamber (2), sample room (3), sample (4), optical fiber I
(5), optical feed trough (6), air inlet pipe (7), escape pipe (8), optics cavity (9), color separation filter (10), notch(ing) filter (11),
Fiber coupler I (12), plane mirror (13), optical fiber collimator (14), fiber coupler II (15), optical fiber II (16), optical detection
Device (17), optical fiber III (18), laser (19), cable and computer, xyz are three-dimensional coordinate system, and cooling chamber (1) has
Low temperature interlayer, by the way that the helium of low temperature is passed through the low temperature interlayer can cool down to cooling chamber (1), experimental temperature model
It encloses from 20K to 120K, cooling chamber (1) has control arm, and vacuum chamber (2) and sample room (3) are connected to cooling chamber (1) from top to bottom
Interior, sample (4) is located in sample room (3), is equipped with adsorption pump inside vacuum chamber (2), enables to the minimum gas of vacuum chamber (2)
Pressure reaches 10-4Pascal, vacuum chamber (2) have bottom through-hole, and edge the upper side and lower side of the bottom through-hole all has flange
The edge of a knife, optical fiber I (5) have optical fiber I protective layer (5-1) and optical fiber I core wire (5-2), and the lower end of optical fiber I (5) is located at sample room (3)
Interior, upper end is connected to optics cavity (9), optics cavity (9), color separation filter (10), notch(ing) filter (11), fiber coupler I
(12), plane mirror (13), optical fiber collimator (14), fiber coupler II (15), optical fiber II (16) and optical detector (17) equal position
In vacuum chamber (2), optical detector (17), optical fiber II (16), fiber coupler I (12), notch(ing) filter (11) and optics cavity
(9) it being sequentially connected from top to bottom, color separation filter (10) is located in optics cavity (9), and laser (19) is located at cooling chamber (1) outside,
Laser (19), optical fiber III (18), fiber coupler II (15) and optical fiber collimator (14) are sequentially connected from top to bottom, optical fiber
The upper surface of notch(ing) filter (11) is fixed in one end of collimator (14), can pass through micro- screw thread of optical fiber collimator (14) inside
Structure changes the positions of (15) fiber coupler II, to adjust the position of hot spot of the laser on plane mirror (13), plane mirror
(13) be located at optical fiber collimator (14) below optics cavity (9) side, can successively by laser (19), optical fiber III (18),
Fiber coupler II (15), optical fiber collimator (14), plane mirror (13), color separation filter (10) and optical fiber I (5) form incident light
Road, can successively by sample (4), optical fiber I (5), color separation filter (10), notch(ing) filter (11), fiber coupler I (12),
Optical fiber II (16) and optical detector (17) form reflected light path；The upper end of air inlet pipe (7) and escape pipe (8) is respectively positioned on cooling chamber
(1) outside top, lower end is respectively positioned in sample room (3) after vacuum chamber (2)；Optical detector (17) and laser (19) are respectively
The optical information collected can be passed through cable transmission to computer by cable connection computer, optical detector (17).
If Fig. 2 is optical feed trough partial enlargement diagram, optical feed trough (6) includes fastener I (6-1), fastener II (6-
2), Teflon plug (6-3), protective case (6-4), stainless steel tube (6-5), epoxy resin (6-6), supporting bead group (6-7) and small
Space (6-8), fastener I (6-1) is hollow and has external screw thread, has cone shaped opening below fastener I (6-1), tightly
Firmware II (6-2) is with internal screw thread and bottom has open-work, and fastener I (6-1) and fastener II (6-2) are located at vacuum chamber
(2) the upper side and lower side of bottom through-hole and threaded connection, fastener I (6-1) and fastener II (6-2) respectively with vacuum chamber
(2) the flange edge of a knife of bottom through-hole edge the upper side and lower side is engaged so that fastener I (6-1) and fastener II (6-2) with very
There is air-tightness, optical feed trough (6), vacuum chamber (2) and cooling chamber (1) all have between any two between empty room (2) bottom through-hole
Air-tightness can adjust the tightness of fastener I (6-1) and fastener II (6-2) by cooling chamber (1) control arm；Teflon
Long Sai (6-3) includes the upper hollow rotary table and lower hollow cylindrical body of axis made of being integrally machined in the y-direction, described hollow
Position forms the through hole of Teflon plug (6-3) in the y-direction, the frustum cone side and the cone of fastener I (6-1) below
Being open, it is mating to be adapted, and is crimped on the bottom fastener II (6-2) by supporting bead group (6-7) below Teflon plug (6-3)
The upper surface of open-work, supporting bead group (6-7) is made of two metal washers that are overlapped and being bonded, the metal washer
Surface is by polishing, so that the frictional resistance very little between two metal washers, when Teflon plug (6-3) is around center axis rotation
When, supporting bead group (6-7) can play a protective role to Teflon plug (6-3) to reduce the abrasion of Teflon plug (6-3)；?
In the fastener cycle of fastener I (6-1) and fastener II (6-2), fastener II (6-2) is by supporting bead group (6-7) to spy
The lower part of fluorine dragon plug (6-3) exerts a force, and is forced upward into Teflon plug (6-3) in the cone shaped opening of fastener I (6-1) below,
And one small space (6-8), Teflon plug are formed between fastener I (6-1), fastener II (6-2) and Teflon plug (6-3)
The clast that (6-3) is generated due to abrasion can be accumulated in the small space (6-8)；Stainless steel tube (6-5) is embedding from top to bottom
It is inserted in fastener I (6-1), Teflon plug (6-3) and fastener II (6-2), the inner surface of stainless steel tube (6-5) is by throwing
Light, optical fiber I (5) are nested in stainless steel tube (6-5), and the part fiber I protective layer (5-1) of optical fiber I (5) is removed, and expose length
The optical fiber I core wire (5-2) that degree is 10 millimeters, and will be wrapped at the optical fiber I core wire (5-2) of the exposing using epoxy resin (6-6)
After wrapping up in, optical fiber I (5) is nested into stainless steel tube (6-5), after epoxy resin (6-6) solidification, optical fiber I (5) and stainless steel tube
(6-5) is capable of fixing, and optical fiber I (5) has epoxy resin (6-6) package that length is 10 millimeters of non-fiber I protective layer (5-1)
The optical fiber I core wire (5-2) wrapped up in section can be adhesively fixed by section, epoxy resin (6-6) with stainless steel tube (6-5) inner surface,
And the package section is located at the fastener I (6-1) above the Teflon plug (6-3) in fastener I (6-1) Nei, stainless steel
The outside nesting of pipe (6-5) is fixed with protective case (6-4), and protective case (6-4) is located at 20 millimeters below fastener II (6-2)
Place；The open-work diameter of the bottom fastener II (6-2) is 4.8 millimeters；The rotary table upper bottom surface radius on the top of Teflon plug (6-3) is
4 millimeters, bottom radius surface is 8.2 millimeters, is highly 6 millimeters, the cylindrical body bottom surface radius of the lower part of Teflon plug (6-3) is 6
Millimeter is highly 5.2 millimeters, and the diameter of the through hole in the y-direction of Teflon plug (6-3) is 3.8 millimeters；Stainless steel tube (6-
5) internal diameter is 0.6 millimeter, outer diameter is 3.6 millimeters, and the tube wall of stainless steel tube (6-5) is thicker, can be avoided and produces to optical fiber I (5)
Raw transition squeezes；The metal washer internal diameter of supporting bead group (6-7) is 4 millimeters, outer diameter is 12 millimeters.
Raman spectrum experimental provision under a kind of cryogenic conditions includes cooling chamber (1), vacuum chamber (2), sample room
(3), sample (4), optical fiber I (5), optical feed trough (6), air inlet pipe (7), escape pipe (8), optics cavity (9), color separation filter
(10), notch(ing) filter (11), fiber coupler I (12), plane mirror (13), optical fiber collimator (14), fiber coupler II
(15), optical fiber II (16), optical detector (17), optical fiber III (18), laser (19), cable and computer, xyz are three-dimensional space
Between coordinate system, cooling chamber (1) has low temperature interlayer, by the way that the helium of low temperature is passed through the low temperature interlayer with can be to cooling chamber
(1) it is cooled down, for experimental temperature range from 20K to 120K, cooling chamber (1) has control arm, vacuum chamber (2) and sample room (3)
It is connected in cooling chamber (1) from top to bottom, sample (4) is located in sample room (3), is equipped with adsorption pump, energy inside vacuum chamber (2)
Enough so that the barometric minimum of vacuum chamber (2) reaches 10-4Pascal, vacuum chamber (2) have bottom through-hole, the side of the bottom through-hole
Edge the upper side and lower side all has the flange edge of a knife, and optical fiber I (5) has optical fiber I protective layer (5-1) and optical fiber I core wire (5-2), optical fiber I
(5) lower end is located in sample room (3), upper end is connected to optics cavity (9), optics cavity (9), color separation filter (10), stepwise filter
Wave device (11), fiber coupler I (12), plane mirror (13), optical fiber collimator (14), fiber coupler II (15), optical fiber II
(16) be respectively positioned on optical detector (17) in vacuum chamber (2), optical detector (17), optical fiber II (16), fiber coupler I (12),
Notch(ing) filter (11) and optics cavity (9) are sequentially connected from top to bottom, and color separation filter (10) is located in optics cavity (9), laser
Device (19) is located at cooling chamber (1) outside, laser (19), optical fiber III (18), fiber coupler II (15) and optical fiber collimator (14)
It is sequentially connected from top to bottom, the upper surface of notch(ing) filter (11) is fixed in one end of optical fiber collimator (14), can pass through optical fiber
The internal micro- helicitic texture of collimator (14) changes the positions of (15) fiber coupler II, to adjust laser in plane mirror (13)
On hot spot position, plane mirror (13) is located at the side of the optics cavity (9) below optical fiber collimator (14), can be successively by swashing
Light device (19), optical fiber III (18), fiber coupler II (15), optical fiber collimator (14), plane mirror (13), color separation filter
(10) and optical fiber I (5) forms input path, can successively be filtered by sample (4), optical fiber I (5), color separation filter (10), stepwise
Device (11), fiber coupler I (12), optical fiber II (16) and optical detector (17) form reflected light path；Air inlet pipe (7) and escape pipe
(8) upper end is respectively positioned on top, the lower end of cooling chamber (1) outside and is respectively positioned in sample room (3) after vacuum chamber (2)；Optical detection
The optical information collected can be passed through electricity by cable connection computer, optical detector (17) respectively for device (17) and laser (19)
Cable is transmitted to computer；Optical feed trough (6) includes fastener I (6-1), fastener II (6-2), Teflon plug (6-3), protective case
(6-4), stainless steel tube (6-5), epoxy resin (6-6), supporting bead group (6-7) and small space (6-8), fastener I (6-1) are
It is hollow and there is external screw thread, there is cone shaped opening, fastener II (6-2) has internal screw thread and bottom below fastener I (6-1)
Portion has open-work, and fastener I (6-1) and fastener II (6-2) are located at the upper side and lower side of the bottom through-hole of vacuum chamber (2)
And be threadedly coupled, fastener I (6-1) and fastener II (6-2) respectively with bottom through-hole edge the upper side and lower side of vacuum chamber (2)
The occlusion of the flange edge of a knife so that with airtight between fastener I (6-1) and fastener II (6-2) and vacuum chamber (2) bottom through-hole
Property, optical feed trough (6), vacuum chamber (2) and cooling chamber (1) all have air-tightness between any two, pass through cooling chamber (1) control arm energy
Enough adjust the tightness of fastener I (6-1) and fastener II (6-2)；Teflon plug (6-3) includes axis made of being integrally machined
The upper hollow rotary table and lower hollow cylindrical body of line in the y-direction, the hollow part form Teflon plug (6-3) along the side y
To through hole, the frustum cone side is adapted mating, Teflon plug (6-3) with the cone shaped opening of fastener I (6-1) below
Below the upper surface of the open-work of the bottom fastener II (6-2), supporting bead group (6-7) be crimped on by supporting bead group (6-7)
It is made of two metal washers that are overlapped and being bonded, the surface of the metal washer is by polishing, so that two metal gaskets
Frictional resistance very little between circle, when Teflon plug (6-3) is around center axis rotation, supporting bead group (6-7) can be to Teflon
Long Sai (6-3) plays a protective role to reduce the abrasion of Teflon plug (6-3)；In fastener I (6-1) and fastener II (6-2)
Fastener cycle in, fastener II (6-2) exerts a force to lower part of Teflon plug (6-3) by supporting bead group (6-7), makes Teflon
Long Sai (6-3) is forced upward into the cone shaped opening of fastener I (6-1) below, and in fastener I (6-1), fastener II (6-
2) one small space (6-8), the clast energy that Teflon plug (6-3) is generated due to abrasion are formed between Teflon plug (6-3)
It is enough accumulated in the small space (6-8)；Stainless steel tube (6-5) is nested into fastener I (6-1), Teflon plug (6- from top to bottom
3) and in fastener II (6-2), for the inner surface of stainless steel tube (6-5) by polishing, optical fiber I (5) is nested in stainless steel tube (6-5)
It is interior, the part fiber I protective layer (5-1) of optical fiber I (5) is removed, exposed length is 10 millimeters of optical fiber I core wire (5-2), and adopts
After being wrapped up at the optical fiber I core wire (5-2) of the exposing with epoxy resin (6-6), optical fiber I (5) is nested into stainless steel tube (6-
5) in, after epoxy resin (6-6) solidification, optical fiber I (5) and stainless steel tube (6-5) are fixed, and it is 10 millis that optical fiber I (5), which has length,
The epoxy resin (6-6) of the non-fiber I protective layer (5-1) of rice wraps up section, and epoxy resin (6-6) can will wrap up the optical fiber in section
I core wire (5-2) is adhesively fixed with stainless steel tube (6-5) inner surface, and the package section is located in fastener I (6-1)
In fastener I (6-1) above Teflon plug (6-3), the outside nesting of stainless steel tube (6-5) is fixed with protective case (6-4), is protected
Sheath (6-4) is located at 20 millimeters below fastener II (6-2)；The open-work diameter of the bottom fastener II (6-2) is 4.8 millis
Rice；The rotary table upper bottom surface radius on the top of Teflon plug (6-3) is 4 millimeters, bottom radius surface is 8.2 millimeters, is highly 6 millis
Meter, the cylindrical body bottom surface radius of the lower part of Teflon plug (6-3) is 6 millimeters, is highly 5.2 millimeters, the edge of Teflon plug (6-3)
The diameter of the through hole in the direction y is 3.8 millimeters；The internal diameter of stainless steel tube (6-5) is 0.6 millimeter, outer diameter is 3.6 millimeters, stainless
The tube wall of steel pipe (6-5) is thicker, can be avoided and generates transition extruding to optical fiber I (5)；The metal washer of supporting bead group (6-7)
Internal diameter is 4 millimeters, outer diameter is 12 millimeters.
The installation method step of optical feed trough (6) and optical fiber I (5) are as follows:
One, the optical fiber I protective layer (5-1) of the middle section on optical fiber I (5) is removed, 10 millimeters of exposed length of optical fiber I
Core wire (5-2), and wrapped up the optical fiber I core wire (5-2) of exposing using epoxy resin (6-6), then optical fiber I (5) is nested into
In stainless steel tube (6-5), after epoxy resin (6-6) solidification, optical fiber I (5) and stainless steel tube (6-5) are fixed；
Two, fastener I (6-1) and fastener II (6-2) are respectively placed in the upper and lower sides of the bottom through-hole of vacuum chamber (2),
Teflon plug (6-3) is placed in the cone shaped opening on the downside of fastener I (6-1), supporting bead group (6-7) is placed in fastener
In II (6-2), fastener I (6-1) is nested in the bottom through-hole of vacuum chamber (2), and is threadably secured in fastener II (6-
2) in；
Three, the lower end of stainless steel tube (6-5) is successively nested into fastener I (6-1), Teflon plug (6-3), supporting bead
Group (6-7) and fastener II (6-2), and the part for exposing optical fiber I core wire (5-2) in optical fiber I (5) is made to be located at fastener I (6-
1) in；
Four, outside that is protective case (6-4) is nested and being fixed on the lower end stainless steel tube (6-5)；
Five, the screw thread between fastener I (6-1) and fastener II (6-2) is screwed, so that fastener I (6-1) and fastener
There is air-tightness between II (6-2) and vacuum chamber (2) bottom through-hole, screwing fastener I (6-1) and fastener II (6- above
2) during the screw thread between, the torque of opposite direction is applied to protective case (6-4) by spanner to protect optical fiber I (5) to keep away
From being broken to excessive torque；
The working method of optical feed trough (6) and the principle that can repeatedly use:
In the fastener cycle of fastener I (6-1) and fastener II (6-2), fastener II (6-2) passes through supporting bead group
(6-7) applies pressure to Teflon plug (6-3) below, and Teflon plug (6-3) is made to be forced upward into the circle on the downside of fastener I (6-1)
In tapered opening, and an areola (6- is formed between fastener I (6-1), fastener II (6-2) and Teflon plug (6-3)
8) clast that, Teflon plug (6-3) is generated due to abrasion can be accumulated in the small space (6-8), thus will not be to spy
The elastic deformation of fluorine dragon plug (6-3) produces bigger effect, tight between fastener I (6-1) and fastener II (6-2) by adjusting
Gu degree can compensate the plastic deformation of Teflon plug (6-3), so that Teflon plug (6-3) has self-regulating function,
It can be repeated as many times and use；Moreover, Teflon plug (6-3) is by tight in the installation process of optical feed trough (6) and optical fiber I (5)
The pressure and fastener II (6-2) of cone shaped opening inner wall on the downside of firmware I (6-1) are applied by supporting bead group (6-7)
Pressure so that Teflon plug (6-3) to stainless steel tube (6-5) outer wall generate pressure, due to being used not in the present invention
Become rusty steel pipe (6-5) tube wall is thicker and outer diameter and internal diameter it is bigger, can be avoided and transition extruding is generated to optical fiber I (5)；It is comprehensive
On, the installation method of optical feed trough (6) and optical fiber I (5) that the present invention uses can overcome teflon material, and the material is soft
Defect makes it have good sealing characteristics and service life.
The principle in situ for adjusting optical fiber I (5) position is, since the structure of the optical feed trough (6) of present apparatus use makes spy
Fluorine dragon plug (6-3) have it is good elasticity and be worn clast influence it is less, therefore, by adjust fastener I (6-1) with
Tightness between fastener II (6-2) reduces Teflon plug (6-3) to the pressure of stainless steel tube (6-5) outer wall, i.e.,
It can rotated by the way that the position of adjusting stainless steel tube (6-5) and optical fiber I (5) in situ is moved or rotated about the axis along axis
During supporting bead group (6-7) can play a protective role to Teflon plug (6-3) to reduce the mill of Teflon plug (6-3)
Damage.
Optical fiber is introduced vacuum chamber using the vacuum feedthrough of special designing by apparatus of the present invention, can be reduced in assembling process
Extruding and distortion to optical fiber, and the position of optical fiber can be adjusted in situ.
Claims (5)
1. the Raman spectrum experimental provision under a kind of cryogenic conditions, including cooling chamber (1), vacuum chamber (2), sample room (3), sample
(4), optical fiber I (5), optical feed trough (6), air inlet pipe (7), escape pipe (8), optics cavity (9), color separation filter (10), stepwise filter
Wave device (11), fiber coupler I (12), plane mirror (13), optical fiber collimator (14), fiber coupler II (15), optical fiber II
(16), optical detector (17), optical fiber III (18), laser (19), cable and computer, xyz is three-dimensional coordinate system, cold
But chamber (1) has low temperature interlayer, cold can carry out to cooling chamber (1) by the way that the helium of low temperature is passed through the low temperature interlayer
But, experimental temperature range is from 20K to 120K, and cooling chamber (1) has control arm, and vacuum chamber (2) and sample room (3) connect from top to bottom
It is connected in cooling chamber (1), sample (4) is located in sample room (3), is equipped with adsorption pump inside vacuum chamber (2), enables to vacuum
The barometric minimum of room (2) reaches 10-4Pascal, vacuum chamber (2) have bottom through-hole, and the edge upside of the bottom through-hole is under
Side all has the flange edge of a knife, and optical fiber I (5) has optical fiber I protective layer (5-1) and optical fiber I core wire (5-2), the lower end of optical fiber I (5)
In sample room (3), upper end be connected to optics cavity (9), optics cavity (9), color separation filter (10), notch(ing) filter (11),
Fiber coupler I (12), plane mirror (13), optical fiber collimator (14), fiber coupler II (15), optical fiber II (16) and optical detection
Device (17) is respectively positioned in vacuum chamber (2), optical detector (17), optical fiber II (16), fiber coupler I (12), notch(ing) filter
(11) it is sequentially connected from top to bottom with optics cavity (9), color separation filter (10) is located in optics cavity (9), and laser (19) is located at
Cooling chamber (1) outside, laser (19), optical fiber III (18), fiber coupler II (15) and optical fiber collimator (14) from top to bottom according to
The upper surface of notch(ing) filter (11) is fixed in secondary connection, one end of optical fiber collimator (14), can pass through optical fiber collimator (14)
Internal micro- helicitic texture changes the positions of (15) fiber coupler II, to adjust hot spot of the laser on plane mirror (13)
Position, plane mirror (13) are located at the side of the optics cavity (9) below optical fiber collimator (14), can successively by laser (19),
Optical fiber III (18), fiber coupler II (15), optical fiber collimator (14), plane mirror (13), color separation filter (10) and optical fiber I
(5) input path is formed, it can be successively by sample (4), optical fiber I (5), color separation filter (10), notch(ing) filter (11), optical fiber
Coupler I (12), optical fiber II (16) and optical detector (17) form reflected light path；The upper end of air inlet pipe (7) and escape pipe (8) is equal
It is respectively positioned in sample room (3) after vacuum chamber (2) positioned at top, the lower end of cooling chamber (1) outside；Optical detector (17) and laser
The optical information collected can be passed through cable transmission to calculating to device (19) by cable connection computer, optical detector (17) respectively
Machine,
It is characterized in that: optical feed trough (6) includes fastener I (6-1), fastener II (6-2), Teflon plug (6-3), protective case
(6-4), stainless steel tube (6-5), epoxy resin (6-6), supporting bead group (6-7) and small space (6-8), fastener I (6-1) are
It is hollow and there is external screw thread, there is cone shaped opening, fastener II (6-2) has internal screw thread and bottom below fastener I (6-1)
Portion has open-work, and fastener I (6-1) and fastener II (6-2) are located at the upper side and lower side of the bottom through-hole of vacuum chamber (2)
And be threadedly coupled, fastener I (6-1) and fastener II (6-2) respectively with bottom through-hole edge the upper side and lower side of vacuum chamber (2)
The occlusion of the flange edge of a knife so that with airtight between fastener I (6-1) and fastener II (6-2) and vacuum chamber (2) bottom through-hole
Property, optical feed trough (6), vacuum chamber (2) and cooling chamber (1) all have air-tightness between any two, pass through cooling chamber (1) control arm energy
Enough adjust the tightness of fastener I (6-1) and fastener II (6-2)；Teflon plug (6-3) includes axis made of being integrally machined
The upper hollow rotary table and lower hollow cylindrical body of line in the y-direction, the hollow part form Teflon plug (6-3) along the side y
To through hole, the frustum cone side is adapted mating, Teflon plug (6-3) with the cone shaped opening of fastener I (6-1) below
Below the upper surface of the open-work of the bottom fastener II (6-2), supporting bead group (6-7) be crimped on by supporting bead group (6-7)
It is made of two metal washers that are overlapped and being bonded, the surface of the metal washer is by polishing, as Teflon plug (6-3)
When around center axis rotation, supporting bead group (6-7) can reduce the abrasion of Teflon plug (6-3)；Fastener I (6-1) and tight
In the fastener cycle of firmware II (6-2), fastener II (6-2) is by supporting bead group (6-7) to the lower part of Teflon plug (6-3)
Force, be forced upward into Teflon plug (6-3) in the cone shaped opening of fastener I (6-1) below, and fastener I (6-1),
One small space (6-8) is formed between fastener II (6-2) and Teflon plug (6-3), Teflon plug (6-3) is produced due to abrasion
Raw clast can be accumulated in the small space (6-8)；Stainless steel tube (6-5) be nested into from top to bottom fastener I (6-1),
In Teflon plug (6-3) and fastener II (6-2), by polishing, optical fiber I (5) is nested in not the inner surface of stainless steel tube (6-5)
It becomes rusty in steel pipe (6-5), optical fiber I (5) has epoxy resin (6-6) package that length is 10 millimeters of non-fiber I protective layer (5-1)
The optical fiber I core wire (5-2) wrapped up in section can be adhesively fixed by section, epoxy resin (6-6) with stainless steel tube (6-5) inner surface,
And the package section is located at the fastener I (6-1) above the Teflon plug (6-3) in fastener I (6-1) Nei, stainless steel
The outside nesting of pipe (6-5) is fixed with protective case (6-4), and protective case (6-4) is located at 20 millimeters below fastener II (6-2)
Place.
2. the Raman spectrum experimental provision under a kind of cryogenic conditions according to claim 1, it is characterized in that: fastener II
The open-work diameter of the bottom (6-2) is 4.8 millimeters.
3. the Raman spectrum experimental provision under a kind of cryogenic conditions according to claim 1, it is characterized in that: Teflon plug
The rotary table upper bottom surface radius on the top of (6-3) is 4 millimeters, bottom radius surface is 8.2 millimeters, is highly 6 millimeters, Teflon plug
The cylindrical body bottom surface radius of the lower part of (6-3) is 6 millimeters, is highly 5.2 millimeters；Running through in the y-direction of Teflon plug (6-3)
The diameter in hole is 3.8 millimeters.
4. the Raman spectrum experimental provision under a kind of cryogenic conditions according to claim 1, it is characterized in that: stainless steel tube
The internal diameter of (6-5) is 0.6 millimeter, outer diameter is 3.6 millimeters.
5. the Raman spectrum experimental provision under a kind of cryogenic conditions according to claim 1, it is characterized in that: supporting bead group
The metal washer internal diameter of (6-7) is 4 millimeters, outer diameter is 12 millimeters.
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