CN107991735B - Metal capillary cyclic olefin polymer dielectric film Terahertz hollow-core fiber and preparation - Google Patents
Metal capillary cyclic olefin polymer dielectric film Terahertz hollow-core fiber and preparation Download PDFInfo
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- CN107991735B CN107991735B CN201610953543.4A CN201610953543A CN107991735B CN 107991735 B CN107991735 B CN 107991735B CN 201610953543 A CN201610953543 A CN 201610953543A CN 107991735 B CN107991735 B CN 107991735B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/032—Optical fibres with cladding with or without a coating with non solid core or cladding
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- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
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Abstract
The invention discloses a kind of metal capillary/cyclic olefin polymer dielectric film Terahertz hollow-core fibers and preparation method thereof, and preparation method, which includes the following steps: for cyclic olefin polymer to be dissolved in toluene solvant, prepares solution；Solution is injected in metal capillary, control toluene solution makes toluene solution liquid level uniform descent from bottom end outflow, and cyclic olefin polymer thickness liquid film is formed on metal capillary inner wall；Metal capillary is immersed in anisotropic solvent after toluene solution discharge, the toluene solvant molecule in cyclic olefin polymer thickness liquid film diffuses in anisotropic solvent, and cyclic olefin polymer dielectric film is formed on metal capillary inner wall；It is passed through nitrogen into metal capillary or air is slowly dried, obtains metal capillary/cyclic olefin polymer dielectric film Terahertz hollow-core fiber.The position of the low loss window of the optical fiber can be adjusted by changing the thickness of cyclic olefin polymer dielectric film, to realize the transmission of different frequency THz wave.
Description
Technical field
The present invention relates to photoelectron material and devices field more particularly to a kind of metal capillary/cyclic olefin polymers
(COC) dielectric film Terahertz hollow-core fiber and preparation method.
Background technique
Terahertz (Terahertz, THz) wave refers to electricity of the frequency in 0.1~10THz (30~3000 μm of wavelength) range
Magnetic wave, also known as far ir ray.THz wave is great in addition to having in basic fields such as physics, chemistry, astronomy, life sciences
Scientific research value except, indoors short-distance wireless communication, satellite communication, medical imaging, environmental monitoring, radio astronomy and
The Applied research fields such as military radar also have broad prospect of application.It is big at present due to lacking effective THz waveguide transmission technology
Most Terahertz systems can only all handle THz wave in free space.These system occupied spaces are big, power consumption is high, by ring
Border influence is big, stability is poor, big using calibration difficulty, seriously limits its application and promotes.Study effective THz waveguide
Transmission means has become and builds multi-functional, high reliability, low energy consumption, novel " flexibility easy to operate, easy to maintain and portable
The key of change " THz devices.
There has been proposed the various optical fiber structures of transmission THz wave, including metal waveguide, glass or plastics hair in recent years
Tubule/the coat of metal/dielectric film hollow wave guide, plastics or silicon medium hollow micro-structure band gap waveguide and plastic medium solid core,
Porous or hollow tube waveguide.These waveguides have that structure is complicated, it is difficult to regulation preparation；Some materials are glass or plastics, it is difficult to
It is fastenedly connected with THz source or detector, stability of focusing in use is poor.For these reasons, how to develop structure simpler
List, preparation process is easier, compatibility is connect with THz source or detector, and better Hz optical fiber structure is still the neck
One of the hot issue that domain is paid close attention to the most both at home and abroad.
In order to overcome these defects in the prior art, the invention proposes a kind of metal capillary/cyclic olefin polymers
(COC) dielectric film Terahertz hollow-core fiber and preparation method thereof.The optical fiber includes on metal capillary structure pipe and its inner surface
Electrolyte reflectance coating.In traditional metal/dielectric film Terahertz hollow-core fiber structure, glass or plastics are usually used
Capillary prepares metallic silver reflective layers as structural tube, then by silver mirror reaction on pipe internal surface, finally again on silverskin surface
Form the polymeric dielectrics reflectance coatings such as polystyrene, polycarbonate, polytetrafluoroethylene (PTFE).It is replaced in invention using metal capillary
Traditional glass or plastic construction pipe, while the inner surface of metal capillary directly replaces conventional metals silvered reflective film, structure
It is simpler.In addition, the invention also provides the method and devices for preparing uniform polymeric dielectric film in metal capillary.It should
Method is compared with traditional vacuum pump suction or peristaltic pump promotion polymer solution are in flow in capillary tube film-forming process, in film
It is easier to manipulate in terms of thickness and uniformity controlling.
Summary of the invention
The invention also provides a kind of preparations of metal capillary/cyclic olefin polymer dielectric film Terahertz hollow-core fiber
Method includes the following steps:
Step 1: cyclic olefin polymer is dissolved in toluene solvant, prepares the solution that weight percent is 10-35%；
Step 2: will be in the metal capillary erect of toluene solution injection of cyclic olefin polymer, control solution is from described
The bottom end outflow of metal capillary makes liquid level of solution uniform descent, forms cyclic olefin polymer on the metal capillary inner wall
Solution liquid film；
Step 3: immersing the metal capillary in anisotropic solvent after the discharge of the toluene solution of cyclic olefin polymer,
Toluene solvant molecule in the cyclic olefin polymer solution liquid film diffuses in the anisotropic solvent, in the metal capillary
Solidification film is formed on inner wall；Step 4: it is passed through clean nitrogen or air into the metal capillary after liquid film solidification and slowly does
Dry, flow 1-10ml is per minute, duration 12-24 hour, obtains metal capillary/cyclic olefin polymer dielectric film terahertz
Hereby hollow-core fiber.
The metal capillary proposed by the present invention/cyclic olefin polymer dielectric film Terahertz hollow-core fiber preparation side
In method, the opposite sex solvent cannot dissolve cyclic olefin polymer, but can be miscible with toluene；The opposite sex solvent includes ethyl alcohol or third
Ketone.
The metal capillary proposed by the present invention/cyclic olefin polymer dielectric film Terahertz hollow-core fiber preparation side
In method, the cleaning of the metal capillary includes the following steps:
It is passed through ethyl alcohol or acetone in a: Xiang Suoshu metal capillary of step, flow 5ml per minute, the duration 30 minutes；
It is passed through deionized water in b: Xiang Suoshu metal capillary of step, flow 10ml per minute, the duration 30 minutes；
Clean nitrogen or air, flow 60ml per minute, duration are blown into c: Xiang Suoshu metal capillary of step
30 minutes.
The metal capillary proposed by the present invention/cyclic olefin polymer dielectric film Terahertz hollow-core fiber preparation side
In method, the speed of piston downlink can be pulled by the concentration and metallic rod constant-speed descending for adjusting the cyclic olefin polymer solution
Adjust the thickness of the cyclic olefin polymer deielectric-coating.
The invention also provides a kind of metal capillary made of preparation method/cyclic olefin polymer dielectric films too
Hertz hollow-core fiber, which is characterized in that there is the cyclic olefin polymer dielectric film, the terahertz in the metal capillary
Hereby the position of the low loss window of hollow-core fiber changes with the thickness of the cyclic olefin polymer dielectric film, to realize difference
The transmission of frequency THz wave.
The invention also provides a kind of preparations of metal capillary/cyclic olefin polymer dielectric film Terahertz hollow-core fiber
Device, comprising: piston sleeve, the fixed metal capillary of upper part simultaneously communicate therewith；It is set to inside the piston sleeve
Piston；And the constant-speed drive component being connect with the piston；The constant-speed drive component drives the piston with constant-speed descending,
Make the toluene solution liquid level uniform descent.
The beneficial effects of the present invention are: traditional glass or plastic construction are replaced using metal capillary in the present invention
Pipe, while the inner surface of metal capillary directly replaces conventional metals silvered reflective film, structure is simpler.The dielectric film of optical fiber
A kind of novel cycloolefin optic polymer COC of materials'use.Metal structure pipe is good thermally conductive and heat dissipation performance can make to be proposed
Hz optical fiber also have transmission high power THz wave potentiality.Terahertz hollow-core fiber proposed by the invention with gold
Structure based on category capillary, good toughness, high mechanical strength can pass through welding or the institute on the outer surface of metal capillary one end
The associated metal component of the silk thread mouth opened and Terahertz generator and detector is bonded, and improves the reliable of equipment operation
Property.In addition, the invention also provides the method and devices for preparing uniform polymeric dielectric film in metal capillary.This method
Compared with traditional vacuum pump suction or peristaltic pump promotion polymer solution are in flow in capillary tube film-forming process, in the thickness of film
With more easily manipulation in terms of uniformity controlling.
Detailed description of the invention
Fig. 1 is metal capillary of the present invention/dielectric film Terahertz hollow-core fiber structural schematic diagram.
Fig. 2 is metal capillary of the present invention/cyclic olefin polymer dielectric film Terahertz hollow-core fiber preparation facilities figure.
Fig. 3 is the loss of copper capillary tube/cyclic olefin polymer dielectric film Terahertz hollow-core fiber of the present invention in embodiment 1
Spectrum.
Fig. 4 is the loss of aluminium capillary/cyclic olefin polymer dielectric film Terahertz hollow-core fiber of the present invention in embodiment 2
Spectrum.
Specific embodiment
In conjunction with following specific embodiments and attached drawing, the present invention is described in further detail.Implement process of the invention,
Condition, experimental method etc. are among the general principles and common general knowledge in the art, this hair in addition to what is specifically mentioned below
It is bright that there are no special restrictions to content.
As shown in Figure 1, metal capillary of the invention/cyclic olefin polymer dielectric film Terahertz hollow-core fiber is for real
The optical fiber transmission of existing THz wave, metal capillary/cyclic olefin polymer dielectric film Terahertz hollow-core fiber includes metal kernel
Tubule 1, dielectric reflectance coating 2 and hollow area 3.Metal capillary 1 constitutes the main structure of Terahertz hollow-core fiber, and cycloolefin is poly-
Polymer dielectric reflectance coating 2 is covered on the inner wall of metal capillary 1, and hollow area 3 is reflectance coating 2 in metal capillary 1
The space surrounded.THz wave forms reflection on metal capillary 1 and dielectric reflectance coating 2 and interface with hollow area 3,
Using inside hollow area 3 air or nitrogen as media implementation optical fiber transmit.
Wherein, metal capillary 1 mainly includes stainless steel capillary, nickel capillary, nickel chromium triangle capillary, copper capillary tube, aluminium
Capillary, titanium capillary.Capillary 1 made of metal and identical or approximate geometry size traditional glass or plastic capillary phase
Than fracture toughness with higher and heat dissipation performance.Dielectric reflectance coating 2 is cyclic olefin polymer (COC) reflectance coating.
The present invention utilizes the controllable descending liquid coating method of piston type (including anisotropic solvent assists quickly solidification) production metal capillary
In pipe/cyclic olefin polymer dielectric film Terahertz hollow-core fiber method, the metal capillary 1 used can be stainless steel wool
Tubule, nickel capillary, nickel chromium triangle capillary, copper capillary tube, aluminium capillary, titanium capillary, based on metal material mechanical strength, bending
Toughness, THz wave transmission loss and preparation process require to design the hollow diameter for determining metal capillary at 1-5 millimeters, wall
20-200 microns thick, 10-200 centimetres of length is preferred.
Include three steps and corresponding process parameters to the cleaning of metal capillary in the present invention:
Step a: being passed through ethyl alcohol or acetone into metal capillary, flow 5ml per minute, and the duration 30 minutes
Step b: being passed through deionized water into metal capillary, flow 10ml per minute, and the duration 30 minutes
Step c: being blown into clean nitrogen or air, flow 60ml per minute into metal capillary, and the duration 30 divides
Clock
Metal capillary/cyclic olefin polymer dielectric film Terahertz hollow-core fiber preparation includes following three in the present invention
Step and corresponding process parameters:
Step 1: cyclic olefin polymer is dissolved in toluene solvant, prepares the solution that weight percent is 10-35%.
Step 2: will cyclic olefin polymer toluene solution injection erect metal capillary in, control toluene solution from
The bottom end outflow of the metal capillary makes liquid level of solution uniform descent, and it is poly- that cycloolefin is formed on the metal capillary inner wall
Polymer solution liquid film.
Step 3: immersing the metal capillary in anisotropic solvent after the discharge of the toluene solution of cyclic olefin polymer,
Toluene solvant molecule in the cyclic olefin polymer solution liquid film diffuses in the anisotropic solvent, in the metal capillary
Solidification film is formed on inner wall；Step 4: it is passed through clean nitrogen or air into the metal capillary after liquid film solidification and slowly does
Dry, flow 1-10ml is per minute, duration 12-24 hour.
In order to prepare metal capillary/cyclic olefin polymer dielectric film Terahertz hollow-core fiber, the present invention is innovatively mentioned
A kind of preparation facilities is gone out.The preparation facilities includes piston sleeve, and the fixed metal capillary of upper part simultaneously communicates therewith；
The piston being set to inside the piston sleeve；And the constant-speed drive component being connect with the piston；The constant-speed drive component
It drives the piston with constant-speed descending, makes the toluene solution liquid level uniform descent of the cyclic olefin polymer.Referring to Fig.2, by golden
Belong to and being connected at the top of capillary and piston sleeve, piston is connect with piston.Cyclic olefin polymer solution is injected piston
In casing, the motor for starting constant-speed drive component makes piston rising push piston that solution is filled metal capillary.Then make gold
Belong to bar constant-speed descending and pull piston downlink, liquid level of solution is by uniform descent in capillary.According to Hydrodynamics Theory, in inside pipe wall
It is upper to form one layer of uniform cyclic olefin polymer solution liquid film.Metal capillary is removed and immerse rapidly one be disposed vertically,
And fill insoluble cyclic olefin polymer but can be miscible with toluene anisotropic solvent in, such as ethyl alcohol or acetone.Cyclic olefin polymer
Toluene solvant molecule in liquid film rapidly diffuses into anisotropic solvent, makes liquid film quick solidification and protects the uniform form of liquid film
It holds.
It can be drawn by metallic rod constant-speed descending in the concentration and step 2 of cyclic olefin polymer solution in rate-determining steps one
The speed (5-100cm is per minute) of piston downlink prepares different cyclic olefin polymer solution liquid films, so that preparation has difference
The metal capillary Hz optical fiber of thickness cyclic olefin polymer dielectric film realizes the transmission of different frequency THz wave.
Embodiment 1
This specific embodiment selects 1 millimeter of interior diameter, and 50 microns of wall thickness, the copper capillary tube that 2 meters of length makees the main body of optical fiber
Structure.After successively cleaning copper capillary tube with second alcohol and water, clean nitrogen, flow 60ml per minute, when continuing are blown into pipe
Between 30 minutes.
COC is dissolved in toluene solvant, the solution that configuration weight percent is 10%.Connect by schematic device in Fig. 2
Copper capillary tube is connect, then by piston sleeve of the toluene solution injection shaped like syringe of COC, starting constant velocity motors makes metallic rod
Rise and pushes piston that solution is filled metal capillary.Metallic rod is pulled with 50cm constant-velocity decline per minute to live
Downlink is filled in, liquid level uniform descent in capillary will form one layer of uniform COC solution liquid film on inside pipe wall.By metal capillary
Pipe remove and immerse rapidly one be disposed vertically and fill insoluble COC but can be miscible with solution solvent ethyl alcohol in.COC solution liquid
Toluene solvant molecule in film rapidly diffuses into anisotropic solvent, makes liquid film quick solidification and keeps the uniform form of liquid film
Get off.Capillary is taken out after ten minutes, and clean air is passed through into pipe and is slowly dried, flow 2ml is per minute, continues drying out 15
Copper capillary tube/COC dielectric film Terahertz hollow-core fiber is obtained after hour.
Prepared copper capillary tube/COC dielectric film Terahertz hollow-core fiber COC film thickness is about 6 microns, refering to figure
3, predicting (2.8 degree of angles of divergence) according to ray model, it in 1.5-10 Terahertz (30-200 microns) range has low loss window,
Loss value is in 0.47~3.3dB/m.
Embodiment 2
This specific embodiment selects 1.5 millimeters of interior diameter, and 200 microns of wall thickness, 30 centimetres of length of aluminium capillary makees optical fiber
Main structure.After successively cleaning copper titanium capillary with second alcohol and water, clean nitrogen is blown into pipe, flow is per minute
60ml, the duration 30 minutes.
COC is dissolved in toluene solvant, the solution that configuration weight percent is 31%.Connect by schematic device in Fig. 2
Aluminium capillary is connect, then by piston sleeve of the toluene solution injection shaped like syringe of COC, starting constant velocity motors makes metallic rod
Rise and pushes piston that solution is filled metal capillary.Metallic rod is pulled with 15cm constant-velocity decline per minute to live
Downlink is filled in, liquid level will decline in capillary, and one layer of COC solution liquid film will be formed on inside pipe wall.Aluminium capillary is removed and fast
Speed immerse one be disposed vertically and fill insoluble COC but can be miscible with toluene solvant acetone in.Toluene in COC solution liquid film
Solvent molecule rapidly diffuses into acetone, makes liquid film quick solidification and remains behind the uniform form of liquid film.After ten minutes
Capillary is taken out, clean air is passed through into pipe and is slowly dried, flow 3ml is per minute, obtains aluminium after continuing drying out 15 hours
Capillary/COC dielectric film Terahertz hollow-core fiber.
Prepared aluminium capillary/COC dielectric film Terahertz hollow-core fiber COC film thickness is about 15 microns, refering to
Fig. 4 predicts (4 degree angles of divergence) its low-loss window there are two 1.5-10 Terahertz (30-200 microns) ranges according to ray model
Mouthful, loss value is in 0.42~1.4dB/m.
Protection content of the invention is not limited to above embodiments.Without departing from the spirit and scope of the invention, originally
Field technical staff it is conceivable that variation and advantage be all included in the present invention, and with appended claims be protect
Protect range.
Claims (4)
1. a kind of preparation facilities of metal capillary cyclic olefin polymer dielectric film Terahertz hollow-core fiber, which is characterized in that
It includes
Piston sleeve, the fixed metal capillary of upper part simultaneously communicate therewith；
The piston being set to inside the piston sleeve；And
The constant-speed drive component being connect with the piston；The constant-speed drive component drives the piston with constant-speed descending.
2. preparation facilities according to claim 1 prepares metal capillary cyclic olefin polymer dielectric film Terahertz hollow
The preparation method of optical fiber, which comprises the steps of:
Step 1: cyclic olefin polymer is dissolved in toluene solvant, prepares the solution that weight percent is 10-35%；
Step 2: will be in the metal capillary erect of toluene solution injection of cyclic olefin polymer, control toluene solution is from described
The bottom end outflow of metal capillary makes toluene solution liquid level uniform descent, and it is poly- that cycloolefin is formed on the metal capillary inner wall
Polymer solution liquid film；
Step 3: immersing the metal capillary in anisotropic solvent after the discharge of the toluene solution of cyclic olefin polymer, described
Toluene solvant molecule in cyclic olefin polymer solution liquid film diffuses in the anisotropic solvent, in the metal capillary inner wall
Upper formation solidifies film；
Step 4: being passed through clean nitrogen or air into the metal capillary after liquid film solidification and slowly dry, flow 1-10ml
Per minute, duration 12-24 hours, metal capillary cyclic olefin polymer dielectric film Terahertz hollow-core fiber is obtained；
The speed tune of piston downlink is pulled by the concentration and metallic rod constant-speed descending that adjust the cyclic olefin polymer solution
Save the thickness of the cyclic olefin polymer deielectric-coating.
3. the preparation side of metal capillary cyclic olefin polymer dielectric film Terahertz hollow-core fiber as claimed in claim 2
Method, which is characterized in that the opposite sex solvent cannot dissolve cyclic olefin polymer, but can be miscible with toluene solvant；The opposite sex is molten
Agent includes ethyl alcohol or acetone.
4. the preparation side of metal capillary cyclic olefin polymer dielectric film Terahertz hollow-core fiber as claimed in claim 2
Method, which is characterized in that the cleaning of the metal capillary includes the following steps: to be passed through in a: Xiang Suoshu metal capillary of step
Ethyl alcohol or acetone, flow 5ml per minute, the duration 30 minutes；It is passed through deionized water in b: Xiang Suoshu metal capillary of step,
Flow 10ml per minute, the duration 30 minutes；Clean nitrogen or air, stream are blown into c: Xiang Suoshu metal capillary of step
Measure 60ml per minute, the duration 30 minutes.
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| CN111719143B (en) * | 2020-06-02 | 2021-07-27 | 华东师范大学 | ABS plastic capillary hollow optical fiber and preparation method thereof |
| CN112751152B (en) * | 2021-02-03 | 2021-09-17 | 复旦大学 | Terahertz waveguide and preparation method thereof |
| CN114420521A (en) * | 2022-01-14 | 2022-04-29 | 深圳奥镨科技有限公司 | Terahertz vacuum electronic device output window and manufacturing method thereof |
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