CN103592719A - Manufacturing method of metal capillary attenuated total reflection infrared hollow optical fiber and optical fiber obtained through the manufacturing method - Google Patents

Manufacturing method of metal capillary attenuated total reflection infrared hollow optical fiber and optical fiber obtained through the manufacturing method Download PDF

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CN103592719A
CN103592719A CN201310504765.4A CN201310504765A CN103592719A CN 103592719 A CN103592719 A CN 103592719A CN 201310504765 A CN201310504765 A CN 201310504765A CN 103592719 A CN103592719 A CN 103592719A
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metal capillary
optical fiber
total reflection
capillary
attenuated total
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CN103592719B (en
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敬承斌
郭洪
胡志高
杨平雄
褚君浩
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East China Normal University
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Abstract

The invention discloses a manufacturing method of a metal capillary attenuated total reflection infrared hollow optical fiber. The manufacturing method of the metal capillary attenuated total reflection infrared hollow optical fiber comprises the steps that germanium dioxide reflective film is formed on the inner surface of a metal capillary through liquid phase deposition, and heating drying is carried out on the metal capillary processed through deposition. According to the manufacturing method, high-temperature heat treatment is not needed in the optical fiber manufacturing technology; compared with a quartz glass capillary attenuated total reflection hollow optical fiber with the geometric dimension the same as or similar to the optical fiber obtained through the manufacturing method, the optical fiber has the advantages that the fracture toughness and the heat dissipation of the optical fiber are greatly improved, the loss value in the process of CO2 laser transmission through the optical fiber can be close to the loss value of the quartz glass capillary attenuated total reflection hollow optical fiber, and a smaller loss window and a smaller laser transmission loss value can be obtained within the range of the wave length ranging from 9.8 microns to 10.4 microns. The invention further discloses the metal capillary attenuated total reflection infrared hollow optical fiber obtained through the manufacturing method.

Description

Metal capillary attenuated total reflection infrared hollow optical fiber method for making and optical fiber thereof
Technical field
The present invention relates to photoelectron material and devices field, relate in particular to a kind of metal capillary attenuated total reflection infrared hollow optical fiber method for making and optical fiber thereof.
Background technology
LONG WAVE INFRARED electromagnetic wave, the especially wavelength CO in the second atmospheric window (8-14 μ m) 2laser occupies critical role in military and civilian.CO 2laser line is abundant, approximately have 140 spectral lines, and line width is narrow, in addition CO in 9.1-11.3 micrometer range 2energy of lasers conversion efficiency and output power are higher, and this laser can be applied to the fields such as active infra-red laser acquisition, the medical treatment of laser life, low-gap semiconductor electron spin regulation and control, laser weapon, laser ignition, forming materials processing and LONG WAVE INFRARED optical transmission of information.And with Optical Fiber Transmission LONG WAVE INFRARED CO 2laser is one of key issue of these applications always.
For many years, scientists is for CO 2laser Transmission problem has been carried out the research of infrared real core fibre (sulfide, halogenide and fluoride fiber), hollow-core fiber and photonic crystal fiber.Wherein hollow-core fiber be take air as transmission medium, simple in structure, endless reflection.Hollow-core fiber has two kinds, leakage type and attenuated total reflection type.Leakage type hollow-core fiber relies on the mirror-reflection of metal pair light to realize CO 2the transmission of laser.Fully-reflected type hollow-core fiber is by air directive refractive index (n according to light r) be less than the principle that 1 reflectance coating produces total reflection and realize CO 2the transmission of laser.Scientists has been researched and developed the attenuated total reflection hollow-core fibers such as germanate glass, sapphire single-crystal, silit and germanium oxide polycrystalline based on Inorganic Non-metallic Materials such as glass or sapphire single-crystals.Sapphire single-crystal or glass are typical hard brittle materials, and are hot poor conductors, and brittle fracture easily occurs corresponding attenuated total reflection hollow-core fiber, at transmission CO 2also can be because of the optical fiber bad generation fire damage of dispelling the heat during laser.These factors have restricted glass or the deep application of sapphire single-crystal total reflection hollow-core fiber in above-mentioned each field to a certain extent.
Quartz glass capillary is selected as the agent structure of germanium dioxide attenuated total reflection hollow-core fiber conventionally, can be reacted and in quartz glass capillary, be deposited germanium dioxide reflectance coating and make optical fiber by high temperature chemical vapor deposition.Inventor had previously also adopted liquid phase deposition in quartz glass capillary, to deposit germanium dioxide reflectance coating, then film was carried out to densification and improve crystallization thermal treatment obtaining germanium dioxide attenuated total reflection hollow-core fiber through the high temperature of 1115-1150 degree Celsius.Although quartz glass capillary is little through high-temperature heat treatment distortion, can become more crisp, brittle fracture more easily occurs, and it is hot poor conductor.Therefore this class hollow-core fiber has fragility fracture and the poor shortcoming of thermal diffusivity.
In order to overcome these defects of the prior art, the present invention proposes a kind of metal capillary attenuated total reflection infrared hollow optical fiber method for making and optical fiber thereof.With metal capillary, as the agent structure of attenuated total reflection hollow-core fiber, be that general Study personnel are not easy to expect, because previously prepared the refractive indexes such as germanate glass, sapphire single-crystal, silit and germanium dioxide, be less than the high-temperature heat treatment that 1 optical reflecting layer all needs 1,000 degree left and right, obviously can there is serious oxidation distortion and performance loss in metal capillary in this high-temperature heat treatment.And present inventor selects metal capillary as the agent structure of optical fiber, ingenious utilize germanium dioxide in the difference of crystalline state metal surface and amorphous state quartz glass surface liquid growth germanium oxide film (such as the induction crystallization effect of crystalline state metal surface, thermal expansion matching effect etc.), just grow at a lower temperature the germanium dioxide reflectance coating that quality is higher, not needing that film is carried out to high-temperature heat treatment just can be for CO 2the transmission of laser, and the loss of transmission can be compared with the quartz glass capillary germanium dioxide attenuated total reflection hollow-core fiber of identical or approximate geometry size, its low loss window, except having the extraneous feature of the 9.8-11.8 micron wave length of covering, also has lower loss window within the scope of 9.8-10.4 micron wave length.Owing to not needing 1,000 degrees Celsius of left and right high-temperature heat treatment, the toughness of metal capillary is fully retained, and the more identical or approximate geometry size quartz glass capillary germanium dioxide hollow-core fiber of the minimal elastic bending radius of optical fiber significantly reduces.Because the coefficient of heat conductivity of metal material generally exceeds quartz glass 5-50 doubly, such metal capillary attenuated total reflection hollow-core fiber is at transmission CO 2heat dispersion quartz glass capillary hollow-core fiber more identical or approximate geometry size in laser process is also significantly increased.
Summary of the invention
The present invention proposes a kind of metal capillary attenuated total reflection infrared hollow optical fiber method for making and optical fiber thereof, utilize the good metal capillary of toughness and thermal diffusivity to replace traditional glass capillary to manufacture germanium dioxide attenuated total reflection type infrared hollow optical fiber.
The method for making that the present invention proposes a kind of metal capillary attenuated total reflection infrared hollow optical fiber, comprises the following steps:
A. by liquid deposition, at the inside surface of metal capillary, form reflectance coating;
B. post-depositional metal capillary is carried out to heat drying.
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, step a also comprises:
Step 1: the inside of the deposit fluid that contains germanium dioxide being filled with to described metal capillary;
Step 2: at lower described metal capillary, the inside surface formation germanium dioxide reflectance coating by liquid deposition at described metal capillary of rotating of room temperature (about 5-25 degree Celsius); And
Step 3: remove the deposit fluid in described metal capillary;
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, step b also comprises:
Step 4: described post-depositional metal capillary is arranged in sleeve pipe;
Step 5: pass into argon gas or nitrogen to described post-depositional kapillary inside, and it is carried out to heat drying;
Step 6: by taking out after described deposition and through the kapillary that super-dry is processed, obtain metal capillary attenuated total reflection infrared hollow optical fiber from described sleeve pipe.
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, in described step 1, in described deposit fluid, the mass percent of germanium dioxide is 5-8%.
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, in described step 2, the pH value of described deposit fluid is 1-3.
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, in described step 2, the rotating speed of described metal capillary is 0.015-0.1 rev/min.
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, in described step 2, the temperature of carrying out liquid deposition is room temperature (about 5-25 degree Celsius).
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, described step 2 further comprises, forms the described reflectance coating that needs thickness by more than twice or twice liquid deposition process.
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, in described step 2, the time of described liquid deposition is 72-120 hour.
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, in described step 5, to the flow velocity that passes into argon gas or nitrogen in described metal capillary, be 20-60ml/min.
In the method for making of the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, in described step 5, the temperature of described heat drying is 50-150 degree Celsius, and the time is 120 minutes.
The invention allows for a kind of metal capillary attenuated total reflection infrared hollow optical fiber, comprising: metal capillary, it is as the agent structure of described ATR-FTIR hollow-core fiber; Reflectance coating, it covers on the inside surface of described metal capillary, is used for reflects infrared light; Hollow district, the space that it surrounds in metal capillary for described reflectance coating, is used for realizing total reflection transmission infrared light.
In the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, described metal capillary comprises nickel kapillary, copper capillary tube and stainless steel capillary.
In the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, described reflectance coating is germanium dioxide reflectance coating.
In the metal capillary attenuated total reflection infrared hollow optical fiber that the present invention proposes, the thickness of described reflectance coating is not less than 4 microns.
The present invention has following beneficial effect:
The present invention proposes the design of metal capillary attenuated total reflection germanium dioxide hollow-core fiber, and the ingenious difference of germanium dioxide liquid deposition growth germanium oxide film on crystalline state metal surface and amorphous state quartz glass surface under room temperature of utilizing is (such as the induction crystallization effect of crystalline state metal surface, thermal expansion matching effect etc.), on the inside surface of metal capillary, grow the germanium dioxide reflectance coating that quality is higher, then obtain metal capillary attenuated total reflection germanium dioxide infrared hollow optical fiber through being no more than after 150 degrees Celsius of dry heat are processed.This invention has been avoided need to be in the operation of 1,000 degrees Celsius of left and right high-temperature heat treatment in conventional quartz glass capillary attenuated total reflection germanium dioxide hollow-core fiber preparation technology, be in manufacture craft, not need high-temperature heat treatment, and the metal capillary optical fiber obtaining have better toughness and thermal diffusivity than the glass capillary optical fiber of identical or approximate geometry size.The low loss window of this type optical fiber covers 9.8-11.8 micron wave length scope, transmission CO 2the loss of laser can be compared with the quartz glass capillary attenuated total reflection germanium dioxide hollow-core fiber of identical or approximate geometry size, also has lower loss within the scope of 9.8-10.4 micron wave length.
Accompanying drawing explanation
Fig. 1 is the structural representation of metal capillary attenuated total reflection infrared hollow optical fiber of the present invention.
Fig. 2 is the process flow diagram of metal capillary attenuated total reflection infrared hollow optical fiber method for making of the present invention.
Fig. 3 is the loss spectra of metal capillary attenuated total reflection infrared hollow optical fiber of the present invention in embodiment 1.
Fig. 4 is the loss spectra of metal capillary attenuated total reflection infrared hollow optical fiber of the present invention in embodiment 2.
Fig. 5 is the loss spectra of metal capillary attenuated total reflection infrared hollow optical fiber of the present invention in embodiment 3.
Fig. 6 is the loss spectra of metal capillary attenuated total reflection infrared hollow optical fiber of the present invention in embodiment 4.
Fig. 7 is the previously loss spectra of quartz glass capillary (interior diameter 1.5mm, 100 microns of wall thickness) the germanium dioxide attenuated total reflection infrared hollow optical fiber of preparation of inventor.
Note: the loss spectra in Fig. 3-7 is got equal length optical fiber and measured.
Embodiment
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail.Implement process of the present invention, condition, experimental technique etc., except the content of mentioning specially below, be universal knowledege and the common practise of this area, the present invention is not particularly limited content.
As shown in Figure 1, metal capillary attenuated total reflection infrared hollow optical fiber of the present invention is used for realizing infrared light, especially CO 2the Optical Fiber Transmission of infrared laser, metal capillary attenuated total reflection infrared hollow optical fiber comprises metal capillary 1, reflectance coating 2 and hollow district 3.Metal capillary 1 forms the agent structure of ATR-FTIR hollow-core fiber, and the inside surface Shang, hollow district 3 that reflectance coating 2 covers kapillary 1 is the space that reflectance coating 2 surrounds in metal capillary 1.Infrared light forms the air of 3 inside, total reflection ,Yi hollow district as media implementation Optical Fiber Transmission on the interface in reflectance coating 2 and hollow district 3.
Wherein, metal capillary 1 mainly comprises nickel kapillary, copper capillary tube and stainless steel capillary etc.Metal kapillary 1 is compared and is had higher fracture toughness and heat dispersion with the traditional glass kapillary of identical or approximate geometry size.Reflectance coating 2 is germanium dioxide reflectance coating, and its thickness is not less than 4 microns.
The present invention utilizes room temperature liquid deposition to make in the method for metal capillary attenuated total reflection infrared hollow optical fiber, the metal capillary 1 using can be nickel kapillary, copper capillary tube or stainless steel capillary, the interior diameter based on metal material physical strength and bent toughness and the definite metal capillary of liquid deposition technological requirement design is good at 1-2 millimeter, wall thickness in 30-200 micron, length in 1-3 rice.
The deposit fluid that the present invention uses is the acidic aqueous solution that contains germanium dioxide, is specially the germanic acid radical ion aqueous solution that contains germanium dioxide.Wherein the mass percent of germanium dioxide is 5-8%, and the pH value of deposit fluid is 1-3.
As shown in Figure 2, the method for making of metal capillary attenuated total reflection infrared hollow optical fiber of the present invention mainly comprises the following steps.
Step 1: after clean metal kapillary 1, fill with deposit fluid in the inside of clean kapillary 1.
Step 2: with the rotational speed metal capillary 1 of 0.015-0.1 rev/min, form reflectance coating 2 by liquid deposition at the inside surface of metal capillary 1.The time of liquid deposition is 72-120 hour, and temperature is room temperature, about 5-25 degree Celsius.Preferably, step 2 also can be by the thickness of more than twice or twice liquid deposition procedure regulation reflectance coating 2, until reach required film thickness.
Step 3: remove the deposit fluid in metal capillary 1.
Step 4: metal capillary 1 is arranged in sleeve pipe.The tubular apparatus such as wherein, the interior diameter of sleeve pipe is slightly larger than the overall diameter of metal capillary 1, and sleeve pipe is glass tube.Metal capillary 1 is placed in to sleeve pipe, not only can protects metal capillary 1, but also can play the contingent oxidation in metal surface in the following heat drying process of prevention.
Step 5: pass into the inert gases such as argon gas or nitrogen with the flow of 20-60ml/min to the inside of post-depositional metal capillary 1, and it is carried out to heat drying, the temperature of heat drying is 50-150 degree Celsius, and the time is 120 minutes.In metal capillary 1, pass into argon gas or nitrogen, can play and accelerate to be dried and to prevent contingent oxidation.
Step 6: the kapillary 1 after deposition and after drying processing is taken out from sleeve pipe, obtain metal capillary attenuated total reflection infrared hollow optical fiber.
Embodiment 1
This specific embodiment is selected 1.5 millimeters of interior diameters, 50 microns of wall thickness, and the stainless steel capillary that length is 2 meters is made the agent structure of optical fiber.With second alcohol and water, clean after stainless steel capillary successively, by containing the germanic acid radical ion aqueous solution of germanium dioxide mass percent 7% with filling with stainless steel capillary after sulphur acid for adjusting pH value to 2, and lie in a horizontal plane on swinging mounting after both ends open is sealed by thermoplastic tube.
Under room temperature, the liquid deposition under the rotating speed of 0.1 rev/min of (approximately 20 degrees Celsius) stainless steel capillary was poured out deposit fluid after 96 hours; The germanic acid radical ion aqueous solution that re-fills same concentrations, identical pH value is carried out secondary liquid deposition, after 120 hours, pours out deposit fluid.
Post-depositional stainless steel capillary is nested in the glass tube of 1.8 millimeters of interior diameters, then level is put into tubular furnace, by the flow of 30ml/min, in stainless steel capillary, pass into argon gas, at 50 degree, be dried 40 minutes, 100 dry 50 minutes of degree, 150 dry 30 minutes of degree are extracted stainless steel capillary out, thereby are obtained stainless steel capillary attenuated total reflection infrared hollow optical fiber from glass bushing.
The fracture ballistic work of this stainless steel metal kapillary attenuated total reflection hollow-core fiber is greater than 0.2 joule, 28 centimetres of the minimal elastic that do not rupture bending radius, 20 watts of 10.6 microns of CO of stable transfer 2the medial temperature 41 Nie Shi degree (equidistant 6 point measurements are averaged) of laser optical fiber surface length direction after 10 minutes, transmit 20 watts of 10.6 microns of CO 2the loss value of laser is 0.59dB/m, transmits 20 watts of 10.2 microns of CO 2the loss value of laser is 0.48dB/m (corresponding 9.8-10.4 micron is low loss window more).
Embodiment 2
This specific embodiment is selected 1.5 millimeters of interior diameters, 100 microns of wall thickness, and the nickel kapillary that length is 1.3 meters is made the agent structure of optical fiber.With second alcohol and water, clean after nickel kapillary successively, the germanic acid radical ion aqueous solution containing germanium dioxide mass percent 7.5%, with filling with nickel kapillary after sulphur acid for adjusting pH value to 2.5, and is lain in a horizontal plane on swinging mounting after both ends open is sealed by thermoplastic tube.
Room temperature (the approximately 15 degrees Celsius) liquid deposition after 120 hours under the rotating speed of 0.02 rpm of nickel kapillary, pour out deposit fluid, the germanic acid radical ion aqueous solution that to re-fill containing germanium dioxide mass percent 7%, pH value be 1.5 is carried out secondary liquid deposition, after 120 hours, pours out deposit fluid.
After nickel kapillary is nested in 1.9 millimeters of glass tubes of interior diameter, level is put into tubular furnace, by the flow of 40ml/min, in nickel kapillary, pass into nitrogen, at 50 degree, be dried 30 minutes, 100 dry 60 minutes of degree, 150 dry 30 minutes of degree, obtain nickel kapillary attenuated total reflection infrared hollow optical fiber after nickel kapillary is extracted out from glass tube.
The fracture ballistic work of this metallic nickel kapillary attenuated total reflection hollow-core fiber is greater than 0.2 joule, 39 centimetres of the minimal elastic that do not rupture bending radius, 20 watts of 10.6 microns of CO of stable transfer 2medial temperature 38 degree (equidistant 6 point measurements are averaged) of laser optical fiber surface length direction after 10 minutes, transmit 20 watts of 10.6 microns of CO 2the loss value of laser is 0.51dB/m, transmits 20 watts of 10.2 microns of CO 2the loss value of laser is 0.42dB/m (corresponding 9.8-10.4 micron is low loss window more).
Embodiment 3
This specific embodiment is selected 1.5 millimeters of interior diameters, 100 microns of wall thickness, and the copper capillary tube that length is 1.2 meters is made the agent structure of optical fiber.With second alcohol and water, clean after copper capillary tube successively, the germanic acid radical ion aqueous solution containing germanium dioxide mass percent 7.8%, with filling with copper capillary tube after sulphur acid for adjusting pH value to 2.3, and is lain in a horizontal plane on swinging mounting after both ends open is sealed by thermoplastic tube.
Copper capillary tube is carried out room temperature (approximately 8 degrees Celsius) liquid deposition under the rotating speed of 0.08 rev/min, after 120 hours, pours out deposit fluid.
After copper capillary tube is nested in 1.9 millimeters of glass tubes of interior diameter, level is put into tubular furnace, by the flow of 25ml/min, in copper capillary tube, pass into argon gas, at 50 degree, be dried 70 minutes, 100 dry 30 minutes of degree, 150 dry 20 minutes of degree, extract copper capillary tube out outer casing glass tube, thereby obtain copper capillary tube attenuated total reflection infrared hollow optical fiber.
The fracture ballistic work of this metallic copper kapillary attenuated total reflection hollow-core fiber is greater than 0.2 joule, 28 centimetres of the minimal elastic that do not rupture bending radius, 20 watts of 10.6 microns of CO of stable transfer 2medial temperature 38 degree (equidistant 6 point measurements are averaged) of laser optical fiber surface length direction after 10 minutes, transmit 20 watts of 10.6 microns of CO 2the loss value of laser is 0.81dB/m, transmits 20 watts of 10.2 microns of CO 2the loss value of laser is 0.67dB/m (corresponding 9.8-10.4 micron is low loss window more).
Embodiment 4
This specific embodiment is selected 1.4 millimeters of interior diameters, 50 microns of wall thickness, and the nickel kapillary that length is 2 meters is made the agent structure of optical fiber.With second alcohol and water, clean after nickel kapillary respectively, the germanic acid radical ion aqueous solution containing germanium dioxide mass percent 6.4%, with filling with nickel kapillary after sulphur acid for adjusting pH value to 1.6, and is lain in a horizontal plane on swinging mounting after both ends open is sealed by thermoplastic tube.
Room temperature (the approximately 10 degree) liquid deposition 96 hours under the rotating speed of 0.1 rev/min of nickel kapillary, pours out deposit fluid; The germanic acid radical ion aqueous solution that to re-fill containing germanium dioxide mass percent 7.7%, pH value be 2.2 is carried out secondary liquid deposition, after 120 hours, pours out deposit fluid.
After nickel kapillary is nested in to 1.7 millimeters of glass tubes of interior diameter, level is put into tubular furnace, by the flow of 20ml/min, in nickel kapillary, pass into nitrogen, at 50 degree, be dried 40 minutes, 100 dry 40 minutes of degree, 150 dry 40 minutes of degree, extract nickel kapillary out glass tube, obtain the nickel kapillary attenuated total reflection infrared hollow optical fiber of 1.4 millimeters of hollow diameters.
The fracture ballistic work of this metallic nickel kapillary attenuated total reflection hollow-core fiber is greater than 0.2 joule, 29 centimetres of the minimal elastic that do not rupture bending radius, 20 watts of 10.6 microns of CO of stable transfer 2medial temperature 36 degree (equidistant 6 point measurements are averaged) of laser optical fiber surface length direction after 10 minutes, transmit 20 watts of 10.6 microns of CO 2the loss value of laser is 0.62dB/m, transmits 20 watts of 10.2 microns of CO 2the loss value of laser is 0.53dB/m (corresponding 9.8-10.4 micron is low loss window more).
Table 1 is metal capillary germanium dioxide attenuated total reflection hollow-core fiber and quartz glass capillary germanium dioxide attenuated total reflection hollow-core fiber related process and performance parameter comparison
Figure BDA0000400477690000071
Figure BDA0000400477690000081
As shown in table 1, in manufacture craft, metal capillary attenuated total reflection infrared hollow optical fiber of the present invention is compared with quartz glass capillary attenuated total reflection infrared hollow optical fiber, the highest need be 150 degrees Celsius of thermal treatments, avoided needing in existing chemical vapor deposition or liquid deposition method the high-temperature heat treatment of 1,000 degree left and right, metal capillary toughness is originally retained.From the fracture ballistic work of optical fiber and the minimal elastic bending radius that do not rupture, the toughness of metal capillary attenuated total reflection infrared hollow optical fiber will be apparently higher than the quartz glass capillary attenuated total reflection infrared hollow optical fiber with identical or approximate geometry size.In transmission carbon dioxide laser process, metal capillary hollow-core fiber average surface temperature is also obviously low than quartz glass capillary optical fiber, shows that this optical fiber has better heat dispersion.
If Fig. 3 is to as shown in Fig. 7 and table 1, the loss value of metal capillary germanium dioxide attenuated total reflection hollow-core fiber transmission carbon dioxide laser of the present invention can be compared with the quartz glass capillary germanium dioxide total reflection optical fiber with identical or approximate geometry size, also has lower loss window and Laser Transmission loss value within the scope of 9.8-10.4 micron wave length.
Protection content of the present invention is not limited to above embodiment.Do not deviating under the spirit and scope of invention, variation and advantage that those skilled in the art can expect are all included in the present invention, and take appending claims as protection domain.

Claims (15)

1. a method for making for metal capillary attenuated total reflection infrared hollow optical fiber, is characterized in that, comprises the following steps:
A. by liquid deposition, at the inside surface of metal capillary (1), form reflectance coating (2);
B. post-depositional metal capillary (1) is carried out to heat drying.
2. the method for claim 1, is characterized in that, above-mentioned steps a also comprises:
Step 1: the inside of the deposit fluid that contains germanium dioxide being filled with to described metal capillary (1);
Step 2: rotate described metal capillary (1), form germanium dioxide reflectance coating (2) by liquid deposition at the inside surface of described metal capillary (1);
Step 3: remove the deposit fluid in described metal capillary (1).
3. method as claimed in claim 2, is characterized in that, above-mentioned steps b also comprises:
Step 4: described post-depositional metal capillary (1) is arranged in sleeve pipe;
Step 5: the inside to described post-depositional metal capillary (1) passes into argon gas or nitrogen, and it is carried out to heat drying;
Step 6: take out from described sleeve pipe through the metal capillary (1) that deposits and be dried after processing described, obtain metal capillary attenuated total reflection infrared hollow optical fiber.
4. method as claimed in claim 2, is characterized in that, in described step 1, in described deposit fluid, the mass percent of germanium dioxide is 5-8%.
5. method as claimed in claim 2, is characterized in that, in described step 1, the pH value of described deposit fluid is 1-3.
6. method as claimed in claim 2, is characterized in that, in described step 2, the rotating speed of described metal capillary (1) is 0.015-0.1 rev/min.
7. the method for making of ATR-FTIR hollow-core fiber as claimed in claim 2, is characterized in that, in described step 2, the temperature of carrying out liquid deposition is room temperature, i.e. 5-25 degree Celsius.
8. method as claimed in claim 2, is characterized in that, described step 2 further comprises, by the described reflectance coating (2) of twice or twice above liquid deposition process formation desired thickness.
9. method as claimed in claim 2, is characterized in that, in described step 2, the time of described liquid deposition is 72-120 hour.
10. method as claimed in claim 3, is characterized in that, in described step 5, to the flow velocity that passes into argon gas or nitrogen in described metal capillary (1), is 20-60ml/min.
11. methods as claimed in claim 3, is characterized in that, in described step 5, the temperature of described heat drying is 50-150 degree Celsius, and the time is 120 minutes.
The metal capillary attenuated total reflection infrared hollow optical fiber that method described in 12. 1 kinds of any one in claim 1-11 is made, is characterized in that, comprising:
Metal capillary (1), it is as the agent structure of described ATR-FTIR hollow-core fiber;
Reflectance coating (2), it covers on the inside surface of described kapillary (1), is used for reflects infrared light;
Hollow district (3), the space that it surrounds in metal capillary for described reflectance coating (2), and realize total reflection transmission infrared light together with described reflectance coating.
13. metal capillary attenuated total reflection infrared hollow optical fibers as claimed in claim 12, is characterized in that, described metal capillary (1) comprises nickel kapillary, copper capillary tube and stainless steel capillary.
14. metal capillary attenuated total reflection infrared hollow optical fibers as claimed in claim 12, is characterized in that, described reflectance coating (2) is germanium dioxide reflectance coating.
15. metal capillary attenuated total reflection infrared hollow optical fibers as claimed in claim 12, is characterized in that, the thickness of described reflectance coating (2) is not less than 4 microns.
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CN107991733A (en) * 2016-10-27 2018-05-04 华东师范大学 Metal capillary germanium dioxide dielectric film mid and far infrared hollow-core fiber and preparation
CN109507149A (en) * 2018-11-13 2019-03-22 荆门博谦信息科技有限公司 A kind of fibre optic interferometer and preparation method thereof
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CN111061003A (en) * 2019-12-13 2020-04-24 江苏师范大学 Semiconductor germanium core-metal-glass cladding composite material mid-infrared optical fiber and preparation method thereof
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CN107991735A (en) * 2016-10-27 2018-05-04 华东师范大学 Metal capillary cyclic olefin polymer dielectric film Terahertz hollow-core fiber and preparation
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CN107991735B (en) * 2016-10-27 2019-11-15 华东师范大学 Metal capillary cyclic olefin polymer dielectric film Terahertz hollow-core fiber and preparation
CN109507149A (en) * 2018-11-13 2019-03-22 荆门博谦信息科技有限公司 A kind of fibre optic interferometer and preparation method thereof
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CN111061003A (en) * 2019-12-13 2020-04-24 江苏师范大学 Semiconductor germanium core-metal-glass cladding composite material mid-infrared optical fiber and preparation method thereof
CN113113834A (en) * 2021-03-10 2021-07-13 华东师范大学 Mid-infrared hollow optical fiber integrated with electroluminescent structure and preparation method thereof
CN113113834B (en) * 2021-03-10 2023-02-03 华东师范大学 Mid-infrared hollow optical fiber integrated with electroluminescent structure and preparation method thereof

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