CN115818950B - Multimode erbium-ytterbium co-doped optical fiber, core rod, preparation method and application thereof - Google Patents
Multimode erbium-ytterbium co-doped optical fiber, core rod, preparation method and application thereof Download PDFInfo
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- KWMNWMQPPKKDII-UHFFFAOYSA-N erbium ytterbium Chemical compound [Er].[Yb] KWMNWMQPPKKDII-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000013307 optical fiber Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
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- 230000008021 deposition Effects 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 45
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002019 doping agent Substances 0.000 claims abstract description 14
- 238000005253 cladding Methods 0.000 claims abstract description 10
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000151 deposition Methods 0.000 claims description 65
- 239000012159 carrier gas Substances 0.000 claims description 47
- 239000013522 chelant Substances 0.000 claims description 43
- 239000002994 raw material Substances 0.000 claims description 21
- 229910052691 Erbium Inorganic materials 0.000 claims description 17
- 239000012792 core layer Substances 0.000 claims description 17
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 16
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 15
- 239000010453 quartz Substances 0.000 claims description 15
- 229910052684 Cerium Inorganic materials 0.000 claims description 11
- RLOWWWKZYUNIDI-UHFFFAOYSA-N phosphinic chloride Chemical compound ClP=O RLOWWWKZYUNIDI-UHFFFAOYSA-N 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 6
- 229910019213 POCl3 Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 22
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- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000003044 adaptive effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
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- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The application discloses a multimode erbium-ytterbium co-doped optical fiber, a core rod, a preparation method and application thereof, and belongs to the technical field of optical fiber preparation, wherein the erbium-ytterbium co-doped optical fiber comprises a fiber core and a cladding, wherein the fiber core main body is SiO 2, dopants are contained in the fiber core main body, the dopants specifically comprise P 2O5、Er2O3 and Yb 2O3, the molar concentration of P 2O5 is 10-15 mol%, the molar concentration of Er 2O3 is 0.02-0.1 mol%, and the molar concentration of Yb 2O3 is 0.8-1.6 mol%; the cladding is disposed on the outer periphery of the core, and the cladding is preferably quartz glass. According to the application, the high doping of P 2O5 and Yb 2O3 in the optical fiber is realized through a one-step forward deposition gas phase doping process, the solubility of Er 3+ and Yb 3+ in silicon dioxide is improved by using P 2O5 so as to avoid clustering, the high doped Yb 3+ is further surrounded around Er 3+ so as to further avoid clustering, the advantage of wider absorption band of Yb 3+ and the energy transfer effect between Er 3+ and Yb 3+ are utilized, and the energy conversion efficiency of Er 3+ is improved so as to realize the high-power laser output of the high-power laser in the wave band of 1540-1560 nm.
Description
Technical Field
The invention belongs to the technical field of optical fiber preparation, and particularly relates to a preparation method of a multimode erbium-ytterbium co-doped core rod, an optical fiber, a preparation method and application of the multimode erbium-ytterbium co-doped core rod.
Background
With the development of related technologies such as space communication, laser radar, medical treatment and military industry, the market demand for high-power continuous or pulsed 1550nm laser light sources is becoming urgent. Particularly with the determination of unmanned business models. The 1550nm band laser radar has attracted wide attention in the intelligent driving field by virtue of the advantages of eye safety, high reliability and the like.
The erbium-ytterbium co-doped fiber laser is a key device for reducing the cost of 1550 nm-band laser radar and realizing popularization. In the case of conventional erbium-doped fibers for telecommunications, on the one hand, only 980nm and 1480nm lasers are commonly used because of the narrow absorption band of Er 3+ so that the pump source is first; on the other hand, the absorption and emission cross sections of Er 3+ are very narrow, so that the output power of the optical fiber is very limited, and the application of the optical fiber in the field of laser radars is limited. Through co-doping of high-concentration Yb 3+, the advantage of wider absorption band of Yb 3+ and the energy transfer effect between Er 3+ and Yb 3+ are utilized, more pumping sources can be selected, the energy conversion efficiency of Er 3+ is improved, and high-power output of 1550nm wave bands is realized.
In the prior art, the erbium-ytterbium co-doped optical fiber is prepared by adopting a reverse deposition mode, namely, the flame moving direction is consistent with the raw material deposition direction, a loose layer is formed firstly and then solution soaking doping is carried out, but the high-temperature flame moves through the loose layer deposited at the downstream in the deposition process, so that P 2O5 in the loose layer can be volatilized in a large amount, the purpose of high doping of P 2O5 cannot be achieved, P 2O5 can improve the solubility of Er 3+ and Yb 3+ in silicon dioxide and avoid clusters, and therefore, the conventional preparation method cannot obtain the erbium-ytterbium co-doped optical fiber with high doping erbium.
Disclosure of Invention
Aiming at one or more of the defects or improvement demands of the prior art, the invention provides a preparation method of a multimode erbium-ytterbium co-doped optical fiber, which realizes high doping of P 2O5 by a high-efficiency deposition process so as to solve the problems of easy clustering and large attenuation in the erbium-ytterbium co-doped optical fiber.
In order to achieve the above purpose, the invention provides a preparation method of a multimode erbium ytterbium co-doped fiber core rod, comprising the following steps:
S1, uniformly mixing raw materials, introducing the raw materials into a quartz glass tube for forward deposition, and depositing and sintering at 1300-1600 ℃ to obtain a core layer; the raw materials comprise SiCl 4、POCl3, erbium ion chelate, ytterbium ion chelate, O 2 and He;
s2, melting and shrinking the core layer obtained by sintering in the quartz liner tube to obtain the core rod.
As a further improvement of the invention, the carrier gas flow rate of POCl 3 in the step S1 is 250-280 sccm, the carrier gas flow rate of the erbium ion chelate is 400-550 sccm, and the carrier gas flow rate of the ytterbium ion chelate is 400-600 sccm.
As a further improvement of the present invention, the carrier gas flow rate of SiCl 4 in the step S1 is 25-30 sccm.
As a further improvement of the invention, the flow ratio of O 2/He in the step S1 is 1.2-1.5.
As a further improvement of the invention, the raw materials in the step S1 also comprise AlCl 3, and the carrier gas flow rate of AlCl 3 is 0-100 sccm.
As a further improvement of the invention, the raw material in the step S1 also comprises cerium ion chelate, and the carrier gas flow rate of the cerium ion chelate is 0-100 sccm.
The application also comprises the multimode erbium-ytterbium co-doped fiber core rod prepared by the preparation method of the multimode erbium-ytterbium co-doped fiber core rod.
The application also comprises a preparation method of the multimode erbium ytterbium co-doped optical fiber, which further comprises the following steps:
S3, selecting a sleeve, putting the core rod into the sleeve, and preparing a prefabricated rod by adopting a tubular rod method;
And S4, drawing the preform rod at a certain temperature to obtain the multimode erbium-ytterbium co-doped optical fiber.
The application also includes a multimode erbium ytterbium co-doped fiber comprising:
A fiber core comprising dopants P 2O5、Er2O3 and Yb 2O3, wherein the molar concentration of P 2O5 is 10-15 mol%; the molar concentration of Er 2O3 is 0.02-0.1 mol%, the molar concentration of Yb 2O3 is 0.8-1.6 mol%, and the concentration ratio of Yb 2O3 to Er 2O3 is 25-40;
and the cladding is coated on the periphery of the fiber core, and the cladding is quartz glass.
As a further improvement of the invention, the fiber core further comprises dopants of Al 2O3 and/or CeO 2; the molar concentration of the Al 2O3 is 0 to 0.4mol percent, and the molar concentration of the CeO 2 is 0 to 0.25mol percent.
The application also comprises the application of the multimode erbium-ytterbium co-doped fiber in 1540-1560 nm-band fiber lasers.
The above-mentioned improved technical features can be combined with each other as long as they do not collide with each other.
In general, the above technical solutions conceived by the present invention have the beneficial effects compared with the prior art including:
(1) According to the multimode erbium-ytterbium co-doped fiber, the P 2O5 in the erbium-ytterbium co-doped fiber is highly doped, so that the solubility of Er 3+ and Yb 3+ in silicon dioxide is improved, and clustering is avoided; and the Yb 3+ in the optical fiber is surrounded by the Er 3+ by the high-doped Yb 3+, so that the cluster phenomenon is further avoided, and the high-efficiency energy transmission is realized.
(2) The multimode erbium-ytterbium co-doped optical fiber is prepared by doping a small amount of Al 2O3 and CeO 2 in the optical fiber, wherein a small amount of Al 2O3 can play roles in stabilizing a glass structure and improving the solubility of rare earth ions; part of CeO 2 can replace P 2O5 which is easy to volatilize, and plays roles in inhibiting energy reverse conversion and Er 3+ ion up-conversion luminescence; and Al 2O3 and CeO 2 are more stable than P 2O5, so that the problem of optical fiber refractive index depression caused by volatilization of P 2O5 can be reduced to a certain extent, and the optical performance of the optical fiber is improved.
(3) The preparation method of the multimode erbium-ytterbium co-doped fiber core rod provided by the invention realizes simultaneous deposition-vapor phase doping-vitrification by adopting a forward deposition combined vapor phase doping mode and controlling the forward deposition temperature to 1300-1600 ℃ on the premise of ensuring vitrification, and reduces volatilization of P 2O5 in the deposition process by reducing the deposition temperature, so that P 2O5 in the erbium-ytterbium co-doped fiber core rod is highly doped, and the problem of central depression of a refractive index profile of the core rod is solved.
Drawings
FIG. 1 is a refractive index profile of a core rod in an erbium ytterbium co-doped fiber in a blank example of the invention;
FIG. 2 is a refractive index profile of a core rod of the multimode erbium ytterbium co-doped fiber of example 1 of the present invention;
FIG. 3 is a refractive index profile of a core rod of the multimode erbium ytterbium co-doped fiber of example 2 of the present invention;
FIG. 4 is a refractive index profile of a core rod of the multimode erbium ytterbium co-doped fiber of example 3 of the present invention;
FIG. 5 is a refractive index profile of the core rod of the multimode erbium ytterbium co-doped fiber of example 4 of the present invention;
FIG. 6 is a refractive index profile of the core rod of the multimode erbium ytterbium co-doped fiber of example 5 of the present invention;
FIG. 7 is a graph showing the refractive index axial uniformity of the core rod of the multimode erbium ytterbium co-doped fiber of example 5 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
Referring to fig. 1 to 7, the multimode erbium-ytterbium co-doped optical fiber in the preferred embodiment of the present invention includes a fiber core and a cladding, wherein the body of the fiber core is SiO 2, and the dopant is contained therein, and specifically includes P 2O5、Er2O3 and Yb 2O3, wherein the molar concentration of P 2O5 is 10 to 15mol%, the molar concentration of Er 2O3 is 0.02 to 0.1mol%, and the molar concentration of Yb 2O3 is 0.8 to 1.6mol%; the cladding is disposed on the outer periphery of the core, and the cladding is preferably quartz glass.
According to the application, through realizing high doping of P 2O5 in the optical fiber, the solubility of Er 3+ and Yb 3+ in silicon dioxide is improved by utilizing P 2O5 to avoid clusters, so that the high doped Yb 3+ surrounds the periphery of Er 3+ to further avoid cluster phenomenon, and the energy conversion efficiency of Er 3+ is improved by utilizing the advantage of wider absorption band of Yb 3+ and the energy transfer effect between Er 3+ and Yb 3+, so that the high-power laser output of the high-power laser in 1540-1560 nm wave band is realized.
Further, as a preferred embodiment of the present application, the core of the present application further includes dopants Al 2O3 and/or CeO 2, wherein the molar concentration of Al 2O3 is 0 to 0.4mol% and the molar concentration of CeO 2 is 0 to 0.25mol%. The application utilizes a small amount of doped Al 2O3 to stabilize the glass structure and improve the solubility of rare earth element ions by doping Al 2O3 in the fiber core. In addition, the molar concentration of Al 2O3 in the application needs to be strictly controlled, and excessive Al 2O3 is doped to reduce phonon energy in a glass system, so that the energy conversion efficiency is reduced. And CeO 2 can partially replace volatile P 2O5, plays roles in inhibiting energy reverse conversion and Er 3+ ion up-conversion luminescence, and improves the optical performance of the multimode erbium-ytterbium co-doped optical fiber. And the Al 2O3 and the CeO 2 are more stable than P 2O5, so that the problem of optical fiber refractive index depression caused by volatilization can be improved to a certain extent.
Further, the ratio of the molar concentration of Yb 2O3 to the molar concentration of Er 2O3 of the multimode erbium-ytterbium co-doped fiber is 25-40, so that the multimode erbium-ytterbium co-doped fiber has enough Yb 3+ surrounding Er 3+ and ensures high energy conversion efficiency. The proportion is above 25, so that enough Yb 3+ can be wrapped around Er 3+, high-efficiency energy transfer is realized, and meanwhile, the optical fiber with the proportion is suitable for devices with short-wave signal light (1540-1560 nm) and low output power (1-2W). When the ratio is less than 25, the working wavelength of the optical fiber moves towards the long wave direction, and the light conversion efficiency under the low power output condition is reduced; when the ratio is greater than 40, the concentration of Er 3+ is low, which results in low light-to-light conversion efficiency of the whole fiber.
Further, the application comprises the application of the multimode erbium-ytterbium co-doped fiber in 1540-1560 nm wave band fiber lasers. In particular, in the conventional erbium-doped fiber, the absorption band of Er 3+ is narrow so that the pump source is firstly a 980nm laser and a 1480nm laser, and the absorption-emission interface of Er 3+ is very narrow, so that the output power of the fiber is very limited, and the application of the fiber in fiber lasers is limited. The co-doping of the high-concentration Yb 3+ in the application can select more pumping sources and improve the energy conversion efficiency of Er 3+ by utilizing the characteristic of wider absorption band of Yb 3+ and the energy transfer effect between Er 3+ and Yb 3+, namely, the application of the multimode erbium-ytterbium co-doped fiber in 1540-1560 m-band fiber lasers is realized.
The application also comprises a preparation method of the multimode erbium-ytterbium co-doped fiber core rod, which is used for preparing the multimode erbium-ytterbium co-doped fiber and specifically comprises the following steps:
S1, uniformly mixing raw materials, introducing the raw materials into a quartz glass tube for forward deposition, and depositing and sintering at 1300-1600 ℃ to obtain a core layer; wherein the raw materials comprise SiCl 4、POCl3, erbium ion chelate, ytterbium ion chelate, O 2 and He;
S2, melting and shrinking the core layer obtained by sintering in the quartz liner tube to obtain a core rod; and the melt shrinkage temperature is 1900-2100 ℃.
Furthermore, the application correspondingly comprises the multimode erbium-ytterbium co-doped fiber core rod aiming at the preparation method of the multimode erbium-ytterbium co-doped fiber core rod.
The preparation method of the multimode erbium-ytterbium co-doped fiber core rod also comprises the preparation method of the multimode co-doped fiber, and the preparation method further comprises the following steps:
s3, selecting a sleeve, cleaning the core rod and the sleeve, sleeving the core rod into the sleeve, and preparing a prefabricated rod by adopting a pipe rod method;
And S4, drawing the preform rod at a certain temperature to obtain the multimode erbium-ytterbium co-doped optical fiber.
Specifically, the application realizes high doping by carrying out forward deposition in the environment of 1300-1600 ℃ and simultaneously realizing deposition-gas phase doping-vitrification by reducing the forward deposition temperature on the premise of ensuring vitrification, and reduces the volatilization problem of P 2O5 in the optical fiber, meanwhile, the solubility of Er 3+ and Yb 3+ in silicon dioxide (fiber core main body) can be improved by the highly doped P 2O5 to avoid the occurrence of clusters, thereby realizing the structure of the erbium-ytterbium co-doped optical fiber with high doping Yb 3+ and surrounding Er 3+, and realizing the high power laser output of the optical fiber in the wave band of 1540-1560 nm.
Specifically, in order to realize high doping of P 2O5 and Yb 2O3, the flow rate of SiCl 4 needs to be reduced to 25-30 sccm, and when the flow rate of SiCl 4 is too high, the doping solubility of the SiCl is limited by the existing gas phase doping process. According to the application, the erbium ion chelate and the ytterbium ion chelate are required to be generated into gas and introduced into the quartz glass tube, the erbium ion chelate and the ytterbium ion chelate are required to be heated to be gaseous through equipment, the heating temperature is not higher than 200 ℃, the saturated vapor pressure is limited, so that the saturated amount exists in the amount of the evaporant of the erbium ion chelate and the ytterbium ion chelate brought out by carrier gas, and the proportion of doping substances (POCl 3, ytterbium chelate and erbium chelate) and a doping main body (SiCl 4) in the reaction is ensured to be large enough to realize high doping, and the flow of SiCl 4 is correspondingly limited.
Meanwhile, in order to reduce volatilization of P 2O5 in the deposition process, the deposition temperature needs to be correspondingly controlled to 1300-1600 ℃, the reactant cannot fully react due to the too low deposition temperature, and volatilization of P 2O5 is caused due to the too high deposition temperature. The reaction temperature limited in the application can ensure that the deposition, the gas phase doping and the vitrification are simultaneously carried out by reducing the forward deposition temperature on the premise of ensuring the vitrification, so that the volatilization of P 2O5 is reduced, and the high doping in the optical fiber is realized. In the deposition process, O 2 is used as a reaction gas and carrier gases of SiCl 4 and POCl 3, and provides an oxidizing atmosphere, and He is used as a carrier gas of ytterbium ions and erbium ion chelates, plays a role in heat conduction, and provides a reducing atmosphere; further, the He has relatively high heat conductivity coefficient, so that the raw materials in the quartz glass tube are heated uniformly for reaction after the flame heats the quartz glass tube. The ratio of O 2 to He is controlled to be 1.2 to 1.5 to ensure that the reaction proceeds sufficiently to produce SiO2、Er2O3、Yb2O3、P2O5、Al2O3、CeO2. When the ratio of the two is too high, the concentration of O 2 is too high, the reaction rate is uncontrollable, and when the concentration of O 2 is too low, oxygen ion vacancies are generated in the generated SiO 2, so that the loss of the generated erbium-ytterbium co-doped optical fiber is influenced.
The high-doped P 2O5 in the invention can improve the solubility of Er 3+ and Yb 3+ in the fiber core main body to avoid clusters, realize high doping of Yb 3+ and surround Er 3+, form an erbium-ytterbium co-doped fiber structure, and realize high-power laser output of the fiber in 1540-1560 nm wave bands.
Specifically, if the conventional MCVD deposition process adopts a forward deposition mode and a solution doping process, that is, the flame moving direction is consistent with the raw material deposition direction, when the deposition mode moves through a loose layer deposited downstream by high-temperature flame, P 2O5 in the loose layer is volatilized in a large amount, so that the purpose of high doping P 2O5 cannot be achieved. In order to avoid the problem, the current preparation method of the mainstream erbium-ytterbium co-doped fiber is a method of combining MCVD reverse deposition and solution doping. The reverse deposition is a deposition mode in which the flame moving direction is opposite to the raw material deposition direction, and in the mode, high-temperature flame cannot move through a deposited loose layer, so that the secondary volatilization of P 2O5 can be reduced, and the high doping of P 2O5 can be realized. However, MCVD reverse deposition requires the combination of solution doping techniques, which are cumbersome and disadvantageous for preparing large core preforms and reduce production efficiency.
And a gas phase doping method combining a chelate evaporation system (CDS) with reverse distribution doping deposition is also provided, wherein a loose layer of high-doped P 2O5 is deposited by a reverse deposition mode, rare earth chelate is then passed through the loose layer by the CDS, and finally vitrification and fusion shrinkage are carried out to realize gas phase doping. This approach eliminates the cumbersome process of soaking and repeated take-over of the solution process, but the step-by-step deposition approach can result in a substantial increase in deposition time, about twice that of the one-step forward deposition approach, which also limits the production efficiency of the fiber.
Based on the above, the preparation method is based on the conventional MCVD combined with the conventional CDS system, and adopts a forward high-temperature deposition direct vitrification one-step gas phase doping method, which can successfully prepare the highly doped multimode erbium-ytterbium co-doped optical fiber by reducing volatilization of P 2O5 and other dopants in the preparation process through relatively low deposition vitrification temperature.
Specifically, the forward deposition manner in step S1 in the present application is as follows:
Heating the quartz glass tube in a mode that the moving direction of the flame is consistent with the depositing direction of the raw material to enable the raw material to react and deposit, wherein the moving speed of the flame is 120-130 mm/min. Preferably, the flame movement rate is 128mm/min.
Further, in the step S1, the deposition time is 1-2 h, and the deposition layer number is 20-30. The conventional gas phase doping process combining MCVD and CDS is deposited and sintered at a high temperature of 1800-2000 ℃, which can lead to a great deal of volatilization of P 2O5 in the gas phase doping process, so that the P 2O5 doping concentration in the erbium-ytterbium co-doped optical fiber is lower. According to the application, through reducing the deposition rate and the deposition temperature, the deposition is carried out in one step under the environment of 1300-1600 ℃ and vitrification is realized, the secondary volatilization of P 2O5 forming a loose layer is avoided, the secondary volatilization of P 2O5 under the high deposition temperature is reduced, and finally, the liner tube is fused and contracted under the high temperature of 1900-2100 ℃ to obtain the core rod structure.
Further preferably, in the present application, the flow rate of carrier gas of POCl 3 is 250 to 280sccm, the flow rate of carrier gas of erbium ion chelate is 400 to 550sccm, and the flow rate of carrier gas of ytterbium ion chelate is 400 to 600sccm.
Furthermore, the raw materials in the application also comprise AlCl 3, and the carrier gas flow rate of the AlCl 3 is 0-100 sccm. The introduction of AlCl 3 is to introduce Al 2O3 into the core rod through reaction so as to improve the effect of stabilizing the glass structure and improving the solubility of rare earth ions.
Further, the raw material in the application also comprises cerium ion chelate, and the carrier gas flow rate of the cerium ion chelate is 0-100 sccm. The cerium ion chelate is introduced to introduce CeO 2 into the core rod by reaction to inhibit the reverse conversion of energy and the up-conversion luminescence of Er 3+ ions.
Further, the specific process of the pipe-bar method adopted in the step S3 is as follows: and selecting a sleeve with an adaptive size according to the diameter of the prepared core rod, washing the sleeve and the core rod with water and acid for 1-2 h, drying for 6-12 h, inserting the core rod into the sleeve, and tapering one end to prepare the preform. Preferably, the inside diameter of the jacket tube, here of the adapted size, is 2 to 10mm larger than the diameter of the core rod.
Optionally, after the core rod is prepared, besides selecting a sleeve with an adaptive size, the core rod can be corroded into a core rod with a corresponding size, and in the corrosion process, a short quartz rod can be connected to two ends of the core rod for avoiding the cone fracture of the core rod.
Further, the specific drawing process in step S4 in the present application includes: fixing the preform on a drawing tower, and introducing argon for protection, wherein the drawing temperature is 1600-1900 ℃, and the diameter of the drawn optical fiber is 120-130 mu m; the outer periphery of the optical fiber is coated with ultraviolet light curing resin coating, and the coating diameter is 230-255 mu m.
Preferably, the ultraviolet curable resin coating applied to the outer periphery of the optical fiber here is a low refractive index resin coating, and the refractive index thereof is preferably 1.1 to 1.4.
And preparing the multimode erbium-ytterbium co-doped fiber according to the preparation direction of the multimode erbium-ytterbium co-doped fiber.
Blank examples:
the erbium-ytterbium co-doped optical fiber prepared by the prior art is used as a comparison object, and the erbium-ytterbium co-doped optical fiber preform core rod is prepared by adopting a reverse deposition combined solution method doping process.
1. Based on the MCVD reverse deposition process, a loose layer is deposited in a quartz liner tube of 28 x 3, wherein the SiCl 4 carrier gas flow rate is 200sccm, the POCl 3 carrier gas flow rate is 300sccm, the deposition temperature is 1450 ℃, the deposition pressure is 100Pa, and the flame moving speed is 128mm/min.
2. The pump end of the deposited liner tube is tapered, and then the mixed solution of YbCl 3 and ErCl 3 with the concentration of 1.5mol/L and 0.05mol/L is poured into the liner tube, and the liner tube is rotated and soaked for 2 hours.
3. After soaking for 2 hours, the cone part of the pump end is knocked out, the solution is poured out, and then the liner tube is naturally dried for 4 hours under the condition of introducing nitrogen.
4. And (3) re-connecting the dried liner tube with a pump end extension tube on MCVD equipment, and preparing the prefabricated rod core rod through drying, dewatering, sintering and shrinking processes.
5. The core rod is matched with the sleeve to form a prefabricated rod and is pulled into an optical fiber.
The refractive index profile of the core rod of the optical fiber prepared by the method is shown in figure 1.
Example 1:
1. Depositing a glass core layer in a 28 x 3 quartz liner tube based on MCVD and conventional CDS technology, wherein the flow rate of SiCl 4 carrier gas in the deposition process is 25sccm; the carrier gas flow rate of POCl 3 is 250sccm, the carrier gas flow rate of erbium ion chelate is 400sccm, the carrier gas flow rate of ytterbium ion chelate is 400sccm, the deposition temperature is 1300 ℃, the deposition pressure is 100Pa, and the flame moving speed is 128mm/min.
2. And (3) melting the quartz liner tube of the deposited glass core layer into a solid glass rod at the temperature of 1900-2100 ℃.
3. And cleaning the prepared core rod and the sleeve with matched size, and then combining the core rod and the sleeve into a prefabricated rod by adopting a pipe rod method.
4. The preform was drawn into an optical fiber at 1800 ℃.
The multimode erbium-ytterbium co-doped fiber obtained in the mode comprises the core dopants of P 2O5、Er2O3 and Yb 2O3, wherein the concentration of P 2O5 is 10.0mol%, the concentration of Er 2O3 is 0.02mol%, and the concentration of Yb 2O3 is 0.8mol%.
The refractive index profile of the core rod of the optical fiber prepared by the method is shown in fig. 2.
Example 2:
1. and depositing a glass core layer in a 28 x 3 quartz liner tube based on MCVD and a conventional CDS technology, wherein the flow rate of SiCl 4 carrier gas is 30sccm, the flow rate of POCl 3 carrier gas is 280sccm, the flow rate of erbium ion chelate carrier gas is 450sccm, the flow rate of ytterbium ion chelate carrier gas is 450sccm, the flow rate of cerium ion chelate carrier gas is 100sccm, the deposition temperature is 1600 ℃, the deposition pressure is 100Pa, and the flame moving speed is 128mm/min.
2. And (3) melting the quartz liner tube of the deposited glass core layer into a solid glass rod at the temperature of 1900-2100 ℃.
3. And cleaning the prepared core rod and the sleeve with matched size, and then combining the core rod and the sleeve into a prefabricated rod by adopting a pipe rod method.
4. The preform was drawn into an optical fiber at 1800 ℃.
The multimode erbium-ytterbium co-doped fiber obtained in the mode comprises the core dopants of P 2O5、CeO2、Er2O3 and Yb 2O3, wherein the concentration of P 2O5 is 10.0mol%, the concentration of CeO 2 is 0.25 mol%, the concentration of Er 2O3 is 0.04mol%, and the concentration of Yb 2O3 is 1.1mol%.
The refractive index profile of the core rod of the optical fiber prepared by the method is shown in fig. 3.
Example 3:
1. Depositing a glass core layer in a quartz liner tube of 28 x 3 based on MCVD and conventional CDS technology, wherein the flow rate of SiCl 4 carrier gas in the deposition process is 30sccm; the carrier gas flow rate of POCl 3 is 280sccm, the carrier gas flow rate of erbium ion chelate is 450sccm, the carrier gas flow rate of ytterbium ion chelate is 450sccm, the carrier gas flow rate of cerium ion chelate is 100sccm, the deposition temperature is 1850 ℃, the deposition pressure is 100Pa, and the flame moving speed is 128mm/min.
2. And (3) melting the quartz liner tube of the deposited glass core layer into a solid glass rod at the temperature of 1900-2100 ℃.
3. And cleaning the prepared core rod and the sleeve with matched size, and then combining the core rod and the sleeve into a prefabricated rod by adopting a pipe rod method.
4. The preform was drawn into an optical fiber at 1800 ℃.
The multimode erbium-ytterbium co-doped fiber obtained in the mode comprises the core dopants of P 2O5、CeO2、Er2O3 and Yb 2O3, wherein the concentration of P 2O5 is 8.0mol%, the concentration of CeO 2 is 0.25 mol%, the concentration of Er 2O3 is 0.03mol%, and the concentration of Yb 2O3 is 0.9mol%.
The refractive index profile of the core rod of the optical fiber prepared by the method is shown in fig. 4.
Example 4:
1. and depositing a glass core layer in a 28 x 3 quartz liner tube based on MCVD and a conventional CDS technology, wherein the flow rate of SiCl 4 carrier gas is 25sccm, the flow rate of POCl 3 carrier gas is 260sccm, the flow rate of AlCl 3 carrier gas is 50sccm, the flow rate of erbium ion chelate carrier gas is 500sccm, the flow rate of ytterbium ion chelate carrier gas is 500sccm, the deposition temperature is 1550 ℃, the deposition pressure is 100Pa, and the flame moving speed is 128mm/min.
2. And (3) melting the quartz liner tube of the deposited glass core layer into a solid glass rod at the temperature of 1900-2100 ℃.
3. And cleaning the prepared core rod and the sleeve with matched size, and then combining the core rod and the sleeve into a prefabricated rod by adopting a pipe rod method.
4. The preform was drawn into an optical fiber at 1800 ℃.
The multimode erbium-ytterbium co-doped fiber obtained in the mode comprises P 2O5、Er2O3 and Yb 2O3 as dopants in a fiber core, wherein the concentration of P 2O5 is 14.0mol%, the concentration of Al 2O3 is 0.3 mol%, the concentration of Er 2O3 is 0.04mol%, and the concentration of Yb 2O3 is 1.3mol%.
The refractive index profile of the core rod of the optical fiber prepared by the method is shown in fig. 5.
Example 5:
1. The glass core layer was deposited in a 28 x 3 quartz liner tube based on MCVD and conventional CDS techniques, during deposition, siCl 4 carrier gas flow was 25sccm, pocl 3 carrier gas flow was 260sccm, alcl 3 carrier gas flow was 100sccm, cerium ion chelate carrier gas flow was 50sccm, erbium ion chelate carrier gas flow was 550sccm, ytterbium ion chelate carrier gas flow was 600sccm, deposition temperature was 1600 ℃, deposition pressure was 100Pa, and flame movement speed was 128mm/min.
2. And (3) melting the quartz liner tube of the deposited glass core layer into a solid glass rod at the temperature of 1900-2100 ℃.
3. And cleaning the prepared core rod and the sleeve with matched size, and then combining the core rod and the sleeve into a prefabricated rod by adopting a pipe rod method.
4. The preform was drawn into an optical fiber at a high temperature of 1820 ℃.
The multimode erbium-ytterbium co-doped fiber obtained in the mode comprises P 2O5、Al2O3、CeO2、Er2O3 and Yb 2O3 as dopants in a fiber core, wherein the concentration of P 2O5 is 14.0mol%, the concentration of Al 2O3 is 0.4mol%, the concentration of CeO 2 is 0.1mol%, the concentration of Er 2O3 is 0.05mol%, and the concentration of Yb 2O3 is 1.5mol%.
The refractive index profile of the core rod of the optical fiber prepared by this method is shown in fig. 6.
The preparation process conditions of the multimode erbium-ytterbium co-doped fiber in examples 1 to 5 in the application are as follows:
meanwhile, the multimode erbium-ytterbium co-doped optical fibers in examples 1 to 5 were prepared according to the above manner, and the element contents were as follows:
Specifically, fig. 1 is a refractive index profile of a core rod in an erbium ytterbium co-doped fiber prepared by a blank method, wherein the core rod is prepared by a reverse deposition combined solution method. Fig. 2, fig. 3, fig. 5 and fig. 6 are refractive index profile views of core rods in erbium-ytterbium co-doped optical fibers prepared in examples 1,2, 4 and 5 according to the method of the present invention, wherein the core rods are prepared by adopting a one-step gas phase doping method of forward deposition direct vitrification by combining MCVD with CDS technology. FIG. 4 is a refractive index profile of a core rod in an erbium ytterbium co-doped fiber prepared in example 3, wherein the core rod is directly vitrified by forward deposition using MCVD in combination with CDS, but the deposition temperature exceeds the 1300-1600 ℃ range defined by the present invention.
By comparing the examples 1,2, 4, 5 and blank and referring to fig. 2,3, 5, 6 and 1, it can be seen that the core diameter of the optical fiber core rod prepared by the method of the present invention is larger, so that the preparation efficiency is high, and more optical fibers can be drawn from a single core rod under the condition of larger core diameter.
By comparing example 3 with example 2 and referring to fig. 4 and 3, it can be seen that when the core layer deposition temperature is too high, P 2O5 volatilizes largely, resulting in a decrease in doping concentration and a decrease in core rod refractive index, as shown in fig. 4; when the deposition temperature is 1300-1600 ℃, P 2O5 cannot volatilize in a large amount, and the refractive index of the core rod is high, as shown in figure 3.
By comparing examples 2, 4, 5 with example 1 and referring to fig. 3,5, 6 and2, the problem of dishing in the refractive index profile of the core rod is improved to some extent when cerium ion chelate and/or AlCl 3 gas is added during the preparation of the core rod. The benefits of fiber refractive index dip optimization include ① to improve fiber optical quality, such as beam energy uniformity and transmission mode stability; ② The absorption coefficient of the optical fiber is improved; ③ And the conversion efficiency of the optical fiber pump light and the signal light is improved.
In addition, fig. 7 represents the refractive index axial uniformity curve of the core rod in the erbium-ytterbium co-doped fiber prepared by the method of the present application, and it can be seen that the overall stability of the doping axial uniformity of the fiber in embodiment 5 of the present application is better. The delta percent of the core rod between 50mm and 450mm sections is 1.2 plus or minus 0.05, and the core rod can be used as an effective core rod for wire drawing.
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (9)
1. The preparation method of the multimode erbium-ytterbium co-doped fiber core rod is characterized by comprising the following steps of:
S1, uniformly mixing raw materials, introducing the raw materials into a quartz glass tube for forward deposition, and depositing and sintering at 1300-1600 ℃ to obtain a core layer; the raw materials comprise SiCl 4、POCl3, erbium ion chelate, ytterbium ion chelate, O 2 and He; the carrier gas flow rate of SiCl 4 is 25-30 sccm, the carrier gas flow rate of POCl 3 is 250-280 sccm, the carrier gas flow rate of erbium ion chelate is 400-550 sccm, and the carrier gas flow rate of ytterbium ion chelate is 400-600 sccm;
s2, melting and shrinking the core layer obtained by sintering in the quartz liner tube to obtain the core rod.
2. The method for preparing a multimode erbium ytterbium co-doped fiber core rod according to claim 1, wherein the flow ratio of O 2/He in the step S1 is 1.2-1.5.
3. The method for preparing a multimode erbium ytterbium co-doped fiber core rod according to claim 1, wherein in the step S1, the raw materials further comprise AlCl 3, and the carrier gas flow rate of AlCl 3 is 0-100 sccm.
4. The method for preparing a multimode erbium ytterbium co-doped fiber core rod according to claim 1 or 3, wherein in the step S1, the raw material further comprises cerium ion chelate, and the carrier gas flow rate of the cerium ion chelate is 0-100 sccm.
5. A multimode erbium ytterbium co-doped fiber core rod, characterized in that it is formed by the method of any one of claims 1 to 4.
6. A method for preparing a multimode erbium-ytterbium co-doped optical fiber, comprising the method for preparing an erbium-ytterbium co-doped optical fiber core rod according to any one of claims 1 to 4, characterized by further comprising the following steps:
S3, selecting a sleeve, putting the core rod into the sleeve, and preparing a prefabricated rod by adopting a tubular rod method;
And S4, drawing the preform rod at a certain temperature to obtain the multimode erbium-ytterbium co-doped optical fiber.
7. A multimode erbium ytterbium co-doped fiber formed by the preparation method of the multimode erbium ytterbium co-doped fiber according to claim 6, comprising:
The fiber core comprises a dopant P 2O5、Er2O3 and Yb 2O3, wherein the molar concentration of the P 2O5 is 10-15 mol%; the molar concentration of Er 2O3 is 0.02-0.1 mol%, the molar concentration of Yb 2O3 is 0.8-1.6 mol%, and the concentration ratio of Yb 2O3 to Er 2O3 is 25-40;
and the cladding is coated on the periphery of the fiber core, and the cladding is quartz glass.
8. The multimode erbium ytterbium co-doped fiber of claim 7, wherein the core further comprises dopants Al 2O3 and/or CeO 2; the molar concentration of the Al 2O3 is 0-0.4 mol%, and the molar concentration of the CeO 2 is 0-0.25 mol%.
9. An application of a multimode erbium-ytterbium co-doped fiber in a 1540-1560 nm-band fiber laser, which is characterized by comprising the multimode erbium-ytterbium co-doped fiber according to claim 7 or 8.
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