CN115259652A - Preparation method of erbium-bismuth co-doped special optical fiber with wide measurement temperature range and high concentration - Google Patents
Preparation method of erbium-bismuth co-doped special optical fiber with wide measurement temperature range and high concentration Download PDFInfo
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- CN115259652A CN115259652A CN202210525326.0A CN202210525326A CN115259652A CN 115259652 A CN115259652 A CN 115259652A CN 202210525326 A CN202210525326 A CN 202210525326A CN 115259652 A CN115259652 A CN 115259652A
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 98
- OXEOYJOKKOUHOJ-UHFFFAOYSA-N bismuth erbium Chemical compound [Er].[Bi] OXEOYJOKKOUHOJ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title abstract description 27
- 238000005259 measurement Methods 0.000 title description 11
- 238000000034 method Methods 0.000 claims abstract description 51
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- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 14
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- 238000002189 fluorescence spectrum Methods 0.000 claims abstract description 7
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001622 bismuth compounds Chemical class 0.000 description 1
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- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
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- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
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- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
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- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
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- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
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Abstract
The invention provides a preparation method of a wide-measurement-temperature-range high-concentration erbium-bismuth co-doped special optical fiber, which combines a chemical vapor deposition (MCVD) method and an NHS (polyethylene-vinyl sulfide) gas-phase high-temperature doping method to manufacture an optical fiber preform, wherein erbium and bismuth doping in a fiber core is realized by introducing erbium-bismuth chelate, the Er doping concentration is 6000-30000ppm, and the Bi doping concentration is 150-500 ppm. Under the action of 260-300 deg.C, the erbium bismuth chelate is uniformly deposited in molecular form according to a certain proportion, and the prefabricated bar is collapsed by adopting low-temperature, small negative pressure or flat pressing method, so that it is more favourable for production. The special optical fiber has the characteristics of wide temperature detection range, capability of measuring high temperature and ultralow temperature, opposite monotonous mapping relation of characteristics in two wave bands of a fluorescence spectrum to the temperature under the action of fixed pumping power, capability of being used in a sensor with self-reliability self-diagnosis and temperature early warning functions, and capability of being widely applied to the fields of ammunition storehouses, aluminum powder storehouses and the like which cause potential safety hazards in electric detection.
Description
(I) technical field
The invention belongs to the technical field of optical fibers, and particularly relates to a preparation method of a wide-temperature-measurement-range high-concentration erbium-bismuth co-doped special optical fiber.
(II) background of the invention
In the field of temperature detection, methods used by people are divided into contact and non-contact measurement, and non-contact thermometers are called radiation thermometers based on the basic law of black body radiation. Radiation thermometry includes luminance, radiation and colorimetric methods. The measurement principle is generally based on the fields of metal expansion, resistance sensing and other electronics, such as measurement by using thermocouples and resistors. However, the use of the electrical effect has a great safety hazard, and when the temperature sensor is applied to ammunition depots, grain depots, ship fuel tanks and other fields, safety accidents are easily caused, and life and property losses are caused. In addition to electrical aspects, there are sensors that are applied in the temperature sensing direction based on optical principles, such as sensing measurement of temperature by using single mode fiber, fiber grating, hollow fiber, etc.
Along with the continuous improvement and innovation of the preparation process of the rare earth doped optical fiber by researchers in recent years, the rare earth doped optical fiber amplifier and the laser are continuously and rapidly developed, and fresh blood is added again to the sensing field due to the rise of the erbium-bismuth co-doped optical fiber. At present, erbium-doped optical fibers on the market are usually prepared by using MCVD (modified chemical vapor deposition) and solution doping methods on a substrate tube, but rare earth ions are difficult to be uniformly distributed in a fiber core, and the preparation time is long, so that the production and the manufacture are not facilitated.
Document CN201510055355.5 discloses a method for preparing a rare earth ion co-doped optical fiber preform, which can flexibly and accurately control the distribution of the ion co-doping ratio and the doping concentration in the axial direction of the core of the preform, and find the optimal ion co-doping ratio for different types of rare earth ion co-doped optical fibers, but the method for preparing the optical fibers by the liquid phase method is complicated, has excessive steps, takes long time, takes 4-12 hours for doping time, and can be used for preparing the optical fibers well only by accurately and often adjusting the length of the rod body entering the solution.
Document CN201610251260.5 discloses a method for efficiently preparing a doped optical fiber preform and a doped optical fiber preform, which provide a method for preparing a precursor by mixing a doping solution in a proportion and then mixing the mixture with high-purity quartz powder, and introducing the precursor into a plasma external spraying device for heating deposition, but the preparation at the early stage is too complicated.
Document CN202010073619.0 discloses a Bi/Er/La/Al co-doped L-band or C + L-band silica fiber and a preparation method thereof, which proposes to prepare the fiber by alternately depositing different doped ions by using high temperature doping MCVD and ALD techniques, and the fiber has a wide application prospect in the fields of broadband fiber communication transmission, light amplification, light sensing and the like, but the high temperature rod-shrinking method adopted by the rod-shrinking process cannot inhibit the volatilization of bismuth ions, so that the doping effect of bismuth is not ideal.
Document CN202010230893.4 discloses a composite coating low temperature measuring optical fiber and its preparation method, which proposes to use polymer coating and metal coating, but the optical fiber is only a single mode optical fiber, and has disadvantages for measuring range and resolution of temperature.
The document CN202110548892.9 discloses a temperature calibration method for an infrared temperature measurement system and an infrared temperature measurement system, which propose a method using an infrared temperature measurement method and a temperature calibration method, but the temperature measurement range only lies in measuring the external environment and human body, and the range is very small, and is not suitable for industrial production and military industry.
Document CN202110364029.8 discloses a device and a method for preparing a multi-glass clad fiber, which mention the preparation of a multi-component glass clad fiber doped with F in the fiber, but the doped substance can not make the rare earth elements doped into the fiber more uniformly and prepare the fiber.
Document CN202111197789.0 discloses a temperature sensor and a temperature measuring device, the invention is based on a self-measuring unit and a module unit to perform a self-measuring function of temperature, and the invention proposes that the spectral characteristics of a temperature-sensitive optical fiber can provide a warning function when the sensor fails.
Document CN202110680587.5 discloses a high-temperature and hydrogen-loss resistant polyimide coating process for an optical fiber surface, which comprises cleaning, pre-coating, pre-curing, pre-coating, high-temperature curing, secondary coating and final coating, wherein three sets of pre-coating devices and three sets of pre-curing components are arranged and connected in series in sequence, and the effect is achieved through coating-curing circulation, but the process is complicated and the acting temperature is high.
Document CN201410190533.0 discloses an apparatus for manufacturing a polyimide coated optical fiber, which, although the operating temperature is reduced compared with other apparatuses, is complicated in the whole apparatus and coating manner, requires an excessively delicate operation, and is not favorable for production.
The temperature sensitive coefficient calibration of the fiber bragg grating under the ultralow temperature condition is researched by ' Kincay, ding Li Yu, and the like ' [ J ]. Optical precision engineering, 2022,30 (1): 56-61. ', and the temperature range is-180.15-19.85 ℃ for low-temperature monitoring, but the temperature measurement range is concentrated on the low-temperature side amount, the range is only 200 ℃, the precision of temperature measurement is lower, and the sensor provides a warning function when no self fault occurs.
The document ' Chen Yun, wan hong Dan, chen gan, etc. ' high-sensitivity optical fiber temperature sensor [ J ] based on rare earth optical fiber double peanut knot, chinese laser, 2020,47 (1): 267-272 ' researches the high-sensitivity optical fiber temperature sensor based on rare earth optical fiber double peanut knot, realizes the high-sensitivity temperature measurement at 22-70 ℃, but has smaller temperature measurement range and can not realize the function of self-detecting the fault and providing warning of the sensor.
The research on the preparation process of gradient rare earth-doped optical fibers in the literature ' Gunn Pengcheng, panglan, wuyang and the like ' [ J ]. Laser and infrared 2021,51 (2): 222-226 ' researches the preparation method of rare earth-doped optical fibers with the rare earth ion doping concentration in gradient distribution on the longitudinal distance of the optical fibers, and the preparation method is based on an ion liquid phase doping method, adopts a loose layer partition multiple soaking technology, but is essentially a high-temperature liquid phase doping method, has too high temperature requirements on actions such as rod shrinkage, wire drawing and the like, and is not beneficial to large-scale preparation.
The document "Xuefang Z, zengyang L, chaoqun G, et al, multi-wave long Brillouin organic-porous fiber laser sensor with high temperature sensing synergistic Electron, opt quantum Electron,2019, 51" proposes a method of measuring temperature by using a multi-wavelength Brillouin erbium-doped fiber laser sensor, but the range of temperature detection for erbium-doped fiber is not very wide.
In summary, most of the existing preparation methods of the optical fiber use a simple application high temperature liquid phase doping method, the action temperature is high, the uniformity of doped rare earth elements and the prevention of bismuth ion volatilization cannot be guaranteed, the method used for achieving the ideal effect on the coating process of the optical fiber coating is too complicated, most of the prepared erbium-bismuth co-doped optical fiber applied to the field of temperature sensing monitoring is concentrated in a high-temperature part at present, the part subjected to ultralow temperature detection rarely relates, the temperature range involved in hunting is narrow, and the method is a problem which needs to be solved urgently for military plants, civil departments and the like.
Therefore, the problems that the temperature measuring range of the existing special optical fiber is narrow, the preparation cost is high, the preparation process is complex, the preparation temperature is high and the like are solved. The invention prepares the erbium-bismuth co-doped optical fiber with high doping concentration by combining MCVD and NHS high temperature gas phase doping methods, realizes the accurate high doping of rare earth elements into an optical fiber preform according to the design requirement, ensures the high doping to be uniform without quenching, reduces the reaction temperature, improves the rod shrinking process, applies a proper optical fiber coating, and carries out a great deal of experimental study on the temperature range of the optical fiber, so that the prepared optical fiber has the characteristics of wide temperature range and strong temperature sensitivity, and has great significance for the fields that the future temperature sensor can be applied to certain extreme specific environments, such as ammunition storehouses, aluminum powder storehouses and the like which can cause potential safety hazards in electricity detection.
Disclosure of the invention
The invention aims to provide a preparation method of a wide-measurement-temperature-range high-concentration erbium-bismuth-codoped special optical fiber, which is characterized in that an MCVD (modified chemical vapor deposition) and NHS (polyethylene-NHS) high-temperature gas phase doping system is used for preparing the optical fiber, a compound containing rare earth elements is accurately controlled and conveyed to a prefabricated rod by using specific gas, and a reaction area of a base tube is manufactured, so that the rare earth elements are doped into the optical fiber prefabricated rod according to design requirements, the effect on the research and development and the production of a gain optical fiber prefabricated rod is achieved, and the prepared erbium-bismuth-codoped optical fiber with high doping concentration has the characteristic of wide applicable temperature range and has great significance for being applied to a sensing detection system in the future.
In order to achieve the purpose, the technical scheme adopted by the implementation of the invention is as follows:
a method for preparing a special high-concentration erbium-bismuth co-doped fiber with a wide temperature measurement range combines a chemical vapor deposition (MCVD) method and an NHS (chemical vapor deposition) gas-phase high-temperature doping method to manufacture a high-temperature sensitive erbium-bismuth co-doped fiber (EBDF), and improves a rod-shrinking process. The erbium ions and the bismuth ions in the fiber core are doped in a gas phase through erbium and bismuth chelates, wherein the doping concentration of the erbium ions is 6000-30000 ppm, the doping concentration of the bismuth ions is 150-500 ppm, and the proportionality coefficient of the erbium ions and the bismuth ions is 40-60. The temperature range measured by the special optical fiber is wide, and the characteristics in two wave bands of the fluorescence spectrum have opposite monotone mapping relation to the temperature under the action of fixed pumping power.
Firstly, the high temperature sensitive characteristic of the special optical fiber is that through experimental verification of the erbium-bismuth co-doped optical fiber, the erbium-bismuth co-doped optical fiber with high doping concentration is found to show good temperature sensitive characteristic, the principle of the erbium-bismuth co-doped optical fiber is explored, and the Er of the erbium-bismuth co-doped optical fiber is found3+Containing ground states in energy levels4I15/2Excited state of4I11/2Metastable state of4I13/2. When the erbium-doped fiber does not absorb energy from the outside, most of the Er3+In the ground state. When the outside temperature rises, the ground state ions are excited to transition to an excited state. However, ions in the excited state are unstable, undergo non-radiative relaxation, and transition to a metastable state. In a metastable state, ions are stable and have long service life. The metastable state ions jump to the ground state through spontaneous radiation and radiate outPhotons. As the temperature increases, the bismuth compound is decomposed into Bi0，Bi+，Bi3+，Bi5 +The bismuth element in the bismuth-doped material is more easily reduced, so that the bismuth material exists in a lower valence state. Then, after the doping concentration of erbium bismuth is increased, more ground state particles are transited on the energy level, the erbium ions can still see the fluorescence characteristic at 1560-1590 nm and the bismuth ions can still see the fluorescence characteristic at 1400-1435 nm, and the optimized fluorescence characteristic is shown.
Furthermore, the high doping concentration of the special optical fiber is mainly selected from 6000 to 30000ppm of erbium ion doping concentration, 150 to 500ppm of bismuth ion doping concentration and 40 to 60 of the proportion coefficient of erbium ions and bismuth ions. The selection range of the doping concentration of the invention not only ensures high concentration, so that the erbium-bismuth co-doped fiber has higher resolution and temperature sensitivity coefficient in a large temperature measurement range, but also ensures that erbium ions are not quenched due to high concentration, and the invention can be prepared in large quantity and has low cost.
In the above, we have introduced the feasibility of erbium bismuth highly doped in special optical fiber and the doping concentration value of the present invention, and the following is the specific process flow of the preparation method:
in general, the combination of chemical vapor deposition (MCVD) and NHS vapor phase high temperature doping is selected, the erbium bismuth raw material is mainly changed into high temperature steam through a high temperature processing unit, so that the high concentration of reaction gas can be realized, the erbium bismuth jellyfish is uniformly mixed with other reaction gas in molecular order, the erbium bismuth jellyfish and the like are conveyed to a reaction area of a base tube manufactured by a prefabricated rod by accurately controlling specific gas, and the rare earth elements are doped into the optical fiber prefabricated rod according to the design requirement. The method can realize the high-concentration uniform doping of erbium and bismuth, greatly improve the performance of doped optical fibers and is beneficial to realizing the temperature measurement application of the invention.
Because the invention needs to prepare the high-doped and high-concentration erbium-bismuth co-doped special optical fiber, the preparation of the base tube adopts multi-component glass K2O-SiO2-X (X is GeO)2、B2O3、La2O3、Sb2O3、 ZrO2、Al2O3One or more) with the aim of developing novel glass parent materials for low temperature (relative to quartz glass) shaping. On the premise of ensuring the basic strength of the glass network body, the K is improved2The concentration of O and the operation temperature are reduced to below 1800 ℃ for smelting in a high-temperature molten state, the rare earth doping uniformity of the multi-component glass is better, the multi-component glass can be uniformly distributed in the whole fiber core glass, the doping concentration is easily improved, and concentration quenching can not occur. The volatilization of bismuth can be reduced by operating below 1800 ℃, so that the final bismuth content in the doped optical fiber is large and the distribution is uniform.
On the optical fiber base tube adopted by people, the invention can safely dope rare earth elements, and the deposition mode of the erbium bismuth chelate of the special optical fiber is that under the action of the temperature of 260-400 ℃, the erbium bismuth chelate is uniformly deposited on the inner wall of the base tube in a molecular form by a vapor phase method to generate erbium bismuth compounds BiO and Bi2O3，Er2O3And compared with other methods, the MCVD and NHS are combined to reduce the doping reaction temperature, so that the method is simple and easy to operate and react, erbium and bismuth can be uniformly deposited without too high temperature, the preform deposition operation and the rare earth chelate deposition operation are carried out together, the time and the operation difficulty are saved compared with a liquid phase deposition method and other gas phase methods, and the manufacturing cost can be reduced.
The invention improves the rod-shrinking process and adopts the mode of low temperature, small negative pressure or flat pressure to perform the rod-shrinking in order to ensure that the special optical fiber is highly doped and has less volatilization in the preparation process. Due to the characteristic that bismuth is volatile at high temperature and can be known based on theory, the method reduces the volatilization of bismuth, accelerates the rod shrinkage speed, and avoids the phenomenon by optimizing parameters although the out-of-roundness of the preform shape is possibly increased.
After the rod is contracted, the optical fiber needs to be coated, in order to achieve the characteristic of high temperature sensitivity, the PMI coating is selected as the erbium-bismuth co-doped optical fiber coating, and the maximum working temperature of the PMI coating is 350 ℃. The preparation method is a method of sectional coating and sectional heating curing, the coating speed is controlled below 10mm/min, the thickness of each layer is not more than 20 mu m, and the maximum curing temperature is 380 ℃. The PMI coating can be used for repeatedly and stably measuring the temperature-sensitive optical fiber at-200-350 ℃, an aluminum-plated coating can be replaced, the temperature range is continuously enlarged, and the temperature sensed by the special optical fiber can be increased to 800 ℃ by the aluminum-plated coating at present.
The doping elements in the special optical fiber are not limited to only doping erbium bismuth jellyfish, ge, al and La can be added for co-doping according to proportion, the solubility of the rare earth elements in the prefabricated rod is increased, and meanwhile, the temperature sensitive coefficient can also be increased, so that the special optical fiber disclosed by the invention has a better temperature sensitive effect when being applied to practice.
The erbium-bismuth co-doped optical fiber with wide measurement temperature range and high concentration prepared by the preparation method has the following characteristic parameters: the diameter of the fiber core is 5.0-20.0 μm, the diameter of the cladding is 80.0-400.0 μm, the numerical aperture is 0.08-0.22, obvious up-conversion luminescence can be seen under pumping, the fiber is green, and the up-conversion spectrum has spectral lines of 532nm and 438 nm.
The wide-temperature-measuring-range high-concentration erbium-bismuth-codoped special optical fiber has the monotonic relation range of the fluorescence intensity change to the temperature of-200-350 ℃. The temperature test of the prepared high-concentration doped erbium-bismuth co-doped optical fiber can obtain a fluorescence spectrum at high temperature. The fluorescence spectrum of the optical fiber can still be tested in a liquid nitrogen low-temperature environment.
When the temperature is the same, the fluorescence intensity values of the two wave bands have opposite trend along with the temperature, and can be obtained through experimental data and later data processing, and the measurement precision of the temperature is less than or equal to 0.2 ℃, which shows the precision degree of the optical fiber on the temperature and the ideal effect in a sensor applied in the future.
The high-concentration erbium-bismuth co-doped special optical fiber has opposite monotone mapping relation to temperature in two wave bands of a fluorescence spectrum of the high-concentration erbium-bismuth co-doped special optical fiber, compared with the prior co-doped optical fiber, the opposite monotone relation can realize high resolution through a program algorithm, the temperature measurement precision is high, the temperature measurement range is wide, the high-concentration erbium-bismuth co-doped special optical fiber is 1400-1435 nm, and the fluorescence intensity value is in a rising trend along with the temperature change. At 1560-1590 nm, the fluorescence intensity value shows a descending trend along with the temperature change, and has an opposite monotone mapping relation to the temperature, and at-200-350 ℃, the relation can realize self-diagnosis of the temperature sensor through a custom algorithm, namely, the function of providing warning when the sensor breaks down is realized.
According to the technical scheme, compared with the prior art, the invention has the following advantages:
the invention discloses a preparation method and detailed preparation parameters of a special erbium-bismuth co-doped optical fiber with a wide measurement temperature range and high concentration, which improves the doping process of rare earth elements, changes a liquid phase deposition method into a vapor phase deposition method, reduces the reaction temperature, simplifies the operation flow, and can obviously improve the concentrations of doped bismuth and erbium compared with the prior preparation method of the rare earth-doped optical fiber without causing concentration quenching. Due to the high-concentration doping of erbium bismuth ions, the fluorescence of the optical fiber has the characteristic of wide measurement range on the temperature characteristic, and the temperature measurement range can cover 350 ℃ high temperature and-200 ℃ low temperature. Under the action of fixed pump power, the characteristics in two wave bands of the fluorescence spectrum have opposite monotone mapping relation to temperature. When the method is applied to the field of sensors, the sensors can be made to perform self reliability diagnosis.
(IV) description of the drawings
FIG. 1 is a flow chart of MCVD and NHS gas phase doping method for preparing special optical fiber.
FIG. 2 is a system diagram for testing a high-concentration erbium-bismuth co-doped special optical fiber. The device consists of a pump laser 1, an isolator 2, a bent single-mode fiber 3, an erbium-bismuth co-doped fiber 4, a spectrometer 5 and a temperature measuring box 6. During measurement, the erbium-bismuth co-doped optical fiber is put into a temperature measuring box for temperature measurement.
Fig. 3 is a graph of the linear relationship of temperature in two bands. As can be seen, the opposite monotonic mapping relationship is present.
(V) detailed description of the preferred embodiments
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be clearly and completely described below with reference to the specific embodiments and the accompanying drawings. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by persons of ordinary skill in the art based on the embodiments of the present invention without any creative efforts shall fall within the protection scope of the embodiments of the present invention.
Example 1:
a process for preparing the high-concentration erbium-bismuth co-doped special optical fibre with wide temp range includes such steps as improving chemical vapour deposition (MCVD) at 1600-1800 deg.C and flame speed of 100mm/min, rotating speed R =35rpm, and coating the glass K with multi-component2O-SiO2-GeO2And carrying out core layer deposition on the liner pipe. Meanwhile, under the action of the temperature of 260-300 ℃, the erbium bismuth chelate is uniformly deposited on the inner wall of the base tube by a vapor phase method, wherein the Er ion concentration is 6000 ppm, the Bi ion concentration is 150ppm, and the uniform doping prefabricated rod is formed by doping according to the proportion coefficient of 40. Then, rod forming is carried out at the temperature of 1700-1750 ℃ and the pressure of 0-50 pa, and the rotating speed R =35rpm. Finally, placing the mixture in a wire drawing tower to preserve heat for 10 minutes at 400 ℃, then slowly opening and vacuumizing, and maintaining the vacuum degree at-0.2 Bar (the negative sign represents the differential pressure lower than the atmospheric pressure); and continuously heating, keeping the temperature at 1800 ℃ for 30 minutes, maintaining the vacuum degree at-0.2 Bar, wherein the drawing speed is 10mm/min, and finally performing operations such as coating an aluminum coating and the like by an explosion spraying method to prepare the erbium-bismuth co-doped special optical fiber with the fiber core diameter of 5.0 mu m, the cladding diameter of 80.0 mu m and the numerical aperture of 0.08.
Example 2:
a process for preparing the erbium-bismuth codoped special optical fibre with wide temp range for measurement and high concentration includes such steps as improving chemical vapour deposition (MCVD) at 1600-1800 deg.C and flame speed of 100mm/min, rotating speed R =35rpm, and multi-component glass K2O-SiO2-GeO2And carrying out core layer deposition on the liner pipe. Meanwhile, under the action of the temperature of 260-300 ℃, erbium bismuth chelate is uniformly deposited on the inner wall of the base tube by a vapor phase method, wherein the Er ion concentration is 30000ppm, the Bi ion concentration is 500ppm, and the uniform doped oxide is formed by doping according to the proportion coefficient of 60. Secondly, adding oxides of Ge, al, la and other elements, and codoping in proportion. Then at a temperature of 1700EPerforming rod forming operation at 1750 ℃ under the pressure of 0 to-50 pa, wherein the rotating speed R =35rpm. And finally, placing the fiber in a wire drawing tower, keeping the temperature at 1800 ℃ for 30 minutes, maintaining the vacuum degree at-0.2 Bar, wherein the drawing speed is 10mm/min, and finally performing PMI coating to prepare the erbium-bismuth co-doped special optical fiber with the fiber core diameter of 20.0 mu m, the cladding diameter of 400.0 mu m and the numerical aperture of 0.22 by adopting operations of sectional coating, sectional heating curing and the like.
Example 3:
as shown in fig. 3, the experimental procedure for testing the temperature of the special optical fiber includes first stripping off the coating layer of the EBDF, connecting the pump laser 1 to the isolator 2, emitting laser of 974nm and 300mW by using a single-mode pump light source, bending the single-mode optical fiber 3 to the erbium-bismuth co-doped optical fiber 4 placed in the temperature measurement box 6, and finally displaying the result in the spectrometer 5. The method is specifically implemented by placing the processed EBDF on an optical fiber bracket for fixing, tensioning and straightening the optical fiber as much as possible, avoiding bending and preventing the bare EBDF optical fiber from being broken in the heating process. After the fiber is fixed, the spectrum is measured once with the spectrometer 5 and recorded as the original spectrum of the EBDF fiber. And (3) placing the EBDF in a temperature measuring box 6, controlling the temperature change, uniformly heating the optical fiber at the temperature of-200-350 ℃, raising the temperature by 10 ℃ per liter, recording the fluorescence intensity value once 30min after the temperature is stabilized, and finally leading out the data from a spectrometer 5 for mapping.
Claims (10)
1. A method for preparing a high-concentration erbium-bismuth co-doped special optical fiber with a wide temperature measurement range combines a chemical vapor deposition (MCVD) method and an NHS (chemical vapor deposition) high-temperature gas-phase doping method to manufacture a high-temperature sensitive erbium-bismuth co-doped optical fiber (EBDF), and improves a rod-shrinking process. The erbium and bismuth doping in the fiber core realizes gas phase doping through erbium and bismuth chelates, wherein the erbium ion doping concentration is 6000-30000 ppm, the bismuth ion doping concentration is 150-500 ppm, the erbium and bismuth ion proportionality coefficient is 40-60, and characteristics in two wave bands of a fluorescence spectrum have opposite monotone mapping relation to temperature under the action of fixed pumping power.
2. The fiber core doping of claim 1, wherein the doping concentration range ensures a high doping concentration, which enables the erbium-bismuth co-doped fiber to have a high resolution over a large temperature measurement range, and ensures that erbium ions are not quenched by the high doping concentration.
3. The NHS hpc of claim 1, wherein the erbium bismuth chelate and oxygen are homogeneously mixed on a molecular scale.
4. The gas-phase high-temperature doping process as claimed in claim 1, wherein under the action of the temperature of 260-300 ℃, erbium bismuth chelate participates in the reaction in the form of gaseous raw material.
5. A collapsing process according to claim 1, wherein the collapsing is carried out by means of lower temperature, small negative pressure or flat pressure.
6. The special optical fiber temperature measurement range according to claim 1, wherein the temperature measurement range is-200 to 350 ℃.
7. The temperature mapping relation according to claim 1, wherein the temperature measurement accuracy is 0.2 ℃ or less, and the temperature measurement accuracy can be used for self-diagnosis of the reliability of the sensor itself.
8. The high-concentration erbium-bismuth-co-doped special optical fiber according to claim 1, wherein parameters are that the diameter of a core is 5.0-20.0 μm, the diameter of a cladding is 80.0-400.0 μm, the numerical aperture is 0.08-0.22, obvious up-conversion luminescence can be seen under pumping, the up-conversion spectrum is green, and the up-conversion spectrum has spectral lines of 532nm and 438 nm.
9. The coating for the special high-concentration erbium-bismuth co-doped optical fiber according to claim 1, wherein the PMI coating is simple to operate, so that the temperature measurement of the temperature-sensitive optical fiber can be stably and accurately performed in a temperature range from low temperature to high temperature.
10. The special high-concentration erbium-bismuth-co-doped optical fiber according to claim 1, characterized in that opposite monotone mapping relations are provided for temperature in two wave bands of 1400-1435 nm and 1560-1590 nm, and the relation can realize self-diagnosis of the temperature sensor through a custom algorithm between-200 ℃ and 350 ℃, namely, the function of providing warning when the sensor breaks down is realized.
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