CN109052972B - Bismuth-doped quartz optical fiber preform and preparation method thereof - Google Patents

Bismuth-doped quartz optical fiber preform and preparation method thereof Download PDF

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CN109052972B
CN109052972B CN201811012617.XA CN201811012617A CN109052972B CN 109052972 B CN109052972 B CN 109052972B CN 201811012617 A CN201811012617 A CN 201811012617A CN 109052972 B CN109052972 B CN 109052972B
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贾宝楠
朱朋飞
刘刚
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Beijing Sushui Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00—Fibre or filament compositions
    • C03C13/04—Fibre optics, e.g. core and clad fibre compositions
    • C03C13/045—Silica-containing oxide glass compositions
    • C03C13/046—Multicomponent glass compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • 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
    • C03B37/012—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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi

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Abstract

The application discloses a bismuth-doped silica optical fiber pre-coatingA rod and a preparation method thereof relate to the field of optical fibers. A bismuth-doped silica optical fiber preform comprising: an outer layer and a core layer. The outer layer is made of silicon dioxide. The core layer material is a silica material doped with Bi atoms, so that the Bi atoms are in a balance position to obtain near-infrared luminescence. The preparation method comprises the following steps: core region deposition step using O2SiCl as carrier gas4The raw material is fed into a deposition tube and carried with Bi by He2O3Mixing with CO, feeding into a deposition tube, mixing with other raw materials, heating the deposition tube, and reacting to obtain the near-infrared light-emitting optical fiber. The core layer material is a silica material doped with Bi atoms, so that the Bi atoms are in a balance position, and near infrared rays can be obtained. The preparation method adopts the improved chemical vapor deposition technology for preparation, and other doping aids are not required to be introduced, so the structure and the operation process are simple and easy to control.

Description

Bismuth-doped quartz optical fiber preform and preparation method thereof
Technical Field
The application relates to the field of optical fibers, in particular to a bismuth-doped silica optical fiber preform and a preparation method thereof.
Background
Rare earth doped silica fibers are very effective active media in the near infrared region. Recent research on optical fiber amplifiers has focused on ytterbium ion (Yb)3+) Neodymium ion (Nd)3+) Erbium ion (Er)3+) Thulium ion (Tm)3+) The working wavelength range of the doped optical fiber covers 900-2100nm, but a spectral gap exists in the 1150-1500nm band. The praseodymium-doped optical fiber amplifier (PDFA) can work in a 1300nm wave band, but the quantum efficiency is low, and as the host is fluoride glass, the connection with the common optical fiber is difficult, and the mechanical strength is poor. The bismuth-doped glass can emit light in an extremely wide region of 1100-1600nm, the bandwidth can reach 200-300nm, and the bismuth-doped glass has potential advantages in the aspect of realizing a high-efficiency broadband optical fiber amplifier. The bismuth-doped silica optical fiber manufactured based on the Modified Chemical Vapor Deposition (MCVD) technology has a more practical prospect and is highly concerned by researchers. The adoption of the bismuth-doped optical fiber is expected to realize the ultra-wide range light amplification of 1100-1600nm wave band by using a single wavelength pumping source, thereby undoubtedly expanding the optical communication bandwidth, improving the communication capacity and bringing a new revolution to the existing optical fiber transmission system.
For bismuth-doped optical fibers, various proposals have been made by researchersThe association between Bismuth Active Centers (BAC) and the near-infrared emission mechanism, these luminescence centers are essentially classified into the following three categories: 1) higher valent Bi, e.g. Bi5+And related molecules; 2) bismuth in lower valence state, e.g. Bi3+、Bi2+、Bi+BiO, Bi clusters; 3) point defects such as Si-ODC and Ge-ODC. Researchers generally believe that the near-infrared luminescence of bismuth-doped fibers is probably caused by bismuth element groups with trivalent or lower valence states, but the exact luminescence mechanism of the near-infrared luminescence of bismuth-doped fibers is still controversial.
At present, Bi is mostly doped in experiments by Bi2O3The form of (A) causes the difficulty of doping to be increased, the doping concentration is limited, and the co-action of other doping promoters is usually required to increase the doping concentration of Bi atoms. Therefore, it is urgently needed to develop a preparation method of bismuth-doped silica optical fiber preform and bismuth-doped silica optical fiber preform with simple operation process and easy control.
Disclosure of Invention
It is an object of the present application to overcome the above problems or to at least partially solve or mitigate the above problems.
According to one aspect of the present application, there is provided a bismuth-doped silica optical fiber preform comprising:
an outer layer made of silicon dioxide; and
and the core layer is made of a silicon dioxide material doped with Bi atoms, so that the Bi atoms are in a balance position to obtain near-infrared luminescence.
Optionally, the inner wall of the outer layer is etched to remove organic matter or other impurities at the inner wall.
Optionally, the bismuth-doped silica optical fiber preform further includes an isolation layer located between the outer layer and the core layer, and the isolation layer is made of silicon dioxide.
Optionally, the near-infrared emission wavelength is 1265 nm.
According to another aspect of the present application, there is provided a method for preparing the bismuth-doped silica optical fiber preform, comprising the following steps:
core area deposition: with oxygen O2Silicon chloride SiCl as carrier gas4The raw material is sent into a deposition tube and bismuth oxide Bi carried by helium He2O3Mixing the carbon monoxide gas with CO, feeding the mixture into a deposition tube, mixing the mixture with other raw materials, heating the deposition tube, and carrying out the following reactions:
SiCl4+O2→SiO2+2Cl2，
Bi2O3+3CO→2Bi+3CO2，
obtaining a near-infrared luminous bismuth-doped silica optical fiber preform;
wherein the deposition tube is a quartz tube.
Optionally, the step of depositing the core region further comprises a step of polishing the deposition tube by using sulfur hexafluoride (SF)6And etching the inner wall of the deposition tube to remove organic matters or other impurities on the inner wall of the tube.
Optionally, the core region deposition step further comprises an isolation layer deposition step of silicon chloride SiCl4Heating in a raw material tank, carrying with oxygen O in a carrier gas2Mixing into the deposition tube, and reacting under heating:
SiCl4+O2→SiO2+2Cl2and obtaining the silicon dioxide isolation layer.
Optionally, the method further comprises an isolation layer deposition step of depositing silicon chloride SiCl after the step of polishing the deposition tube and before the step of depositing the core region4Heating in a raw material tank, mixing with oxygen O2 into the deposition tube under the carrying of carrier gas, and reacting under the heating condition:
SiCl4+O2→SiO2+2Cl2and obtaining the silicon dioxide isolation layer.
Optionally, the step of depositing the core region further comprises a step of collapsing the deposition tube, wherein the pressure in the deposition tube is maintained at a positive pressure, the pressure is gradually reduced in the collapsing process, and finally, necking and compressing are performed in a negative pressure state to form a rod.
Optionally, the collapsing step of the deposition tube further comprises a mother tube rod sleeving step, and a layer of quartz tube is sleeved outside the rod formed in the collapsing step of the deposition tube to form a mother rod with a proper core-cladding ratio.
According to the bismuth-doped silica optical fiber preform rod, the core layer material is a silica material doped with Bi atoms, so that the Bi atoms are in a balance position, and near-infrared luminescence can be obtained. The preparation method of the bismuth-doped silica optical fiber preform is prepared by adopting an improved chemical vapor deposition technology, and other doping aids are not required to be introduced, so that the structure and the operation process are simple and easy to control.
The above and other objects, advantages and features of the present application will become more apparent to those skilled in the art from the following detailed description of specific embodiments thereof, taken in conjunction with the accompanying drawings.
Drawings
Some specific embodiments of the present application will be described in detail hereinafter by way of illustration and not limitation with reference to the accompanying drawings. The same reference numbers in the drawings identify the same or similar elements or components. Those skilled in the art will appreciate that the drawings are not necessarily drawn to scale. In the drawings:
FIG. 1 is a schematic block diagram of a bismuth-doped silica optical fiber preform according to one embodiment of the present application;
FIG. 2 is a schematic block diagram of a bismuth-doped silica optical fiber preform according to one embodiment of the present application;
FIG. 3a is a graph of the system of the present application as a function of ring size;
FIG. 3b is a graph of the system of the present application as a function of radial distance from the center of the ring;
FIG. 4 is a diagram of energy level transitions for a Bi-doped silica optical fiber of the present application;
FIG. 5 is a schematic diagram of a process for fabricating a Bi-doped silica optical fiber preform according to one embodiment of the present application;
fig. 6 is a schematic flow chart of a method of fabricating a Bi-doped silica optical fiber preform according to one embodiment of the present application.
The symbols in the drawings represent the following meanings:
10 of a bismuth-doped silica optical fiber preform,
1 outer layer, 2 core layer, 3 isolating layer,
a represents SiCl4，
B represents Bi2O3，
101 O2，
102 He，
103 CO，
104 a deposition tube is arranged in the chamber,
105 oxyhydrogen flame burner.
Detailed Description
FIG. 1 is a schematic block diagram of a bismuth-doped silica optical fiber preform according to one embodiment of the present application. A bismuth-doped silica optical fiber preform 10 may generally include: an outer layer 1 and a core layer 2. The material of the outer layer 1 is silicon dioxide. The core layer 2 is made of silica doped with Bi atoms, so that the Bi atoms are in a balance position to obtain near-infrared luminescence.
According to the bismuth-doped silica optical fiber preform 10, the core layer 2 is made of silica doped with a small amount of Bi atoms, so that the Bi atoms are in a balance position, and near-infrared luminescence can be obtained.
Further, referring to fig. 1, in this embodiment, the inner wall of the outer layer 1 is etched to remove organic matters or other impurities at the inner wall.
FIG. 2 is a schematic block diagram of a bismuth-doped silica optical fiber preform according to one embodiment of the present application. In this embodiment, the bismuth-doped silica optical fiber preform 10 is different from the embodiment shown in fig. 1 in that the bismuth-doped silica optical fiber preform 10 in this embodiment further includes an isolation layer 3, the isolation layer 3 is located between the outer layer 1 and the core layer 2, and the isolation layer 3 is made of silicon dioxide.
More specifically, the near-infrared emission wavelength is 1265 nm. Of course, in other embodiments, the near-infrared emission wavelength is 1265 nm.
Figure 3a is a graph of the system of the present application as it generally varies with the size of the ring. Figure 3b is a graph of the system of the present application as a function of radial distance from the center of the ring. In the calculations of fig. 3a and 3b, the inventors considered the effect of the quartz ring size and the radiation distance on the equilibrium position of the interstitial Bi atoms. First, the inventors investigated the nature of the interstitial Bi atoms in the rings, which is related to the size of the n rings in the silica network. The interstitial Bi atoms are initially centered between 4 and 7 rings and then fully structurally optimized. Figure 3a is a graph of the system of the present application as it generally varies with the size of the ring. The curves show that as the size of the circle increases, the total energy decreases rapidly and approaches a nearly constant value in a six-circle or larger circle. In fact, as the size of the ring increases, the stability of the interstitial Bi atoms within the ring increases. Thus, when the system reaches equilibrium, the interstitial Bi atoms are most likely located around the six rings.
The inventors also investigated the effect of radial distance on the equilibrium position of the interstitial Bi atoms in the silica network using the hill-climbing micromotion elastic band (CI-NEB) method. To eliminate errors in the silica network in interacting with surrounding atoms, the inventors chose as large a network of voids as possible. Figure 3b is a graph of the system of the present application as a function of radial distance from the center of the ring. The inventors chose 6 to center the circle as zero. There are two energy barriers and a lowest saddle point on the curve. The first barrier is about 0.6eV, which is mainly due to the effect of a six-circle ring. The second barrier is about 0.4eV, which is mainly due to the effect of the six-ring pair on the interaction with the other surrounding rings. It is known to find a stable structure by finding the saddle point with the lowest energy. Therefore, the interstitial Bi atoms are most likely to stay at about the center of the six-ring
Figure BDA0001785377740000041
To (3). There is no Si-O bond rupture throughout the silica network and the interstitial Bi atoms maintain charge balance with the surrounding Si and O by adjusting the shape of their atomic orbitals.
Table 1 is a table of Bader charge population analysis for defect-free and Bi-doped silica fibers. In table 1, the inventors introduced the Bader charge population method to analytically determine the valence state of the interstitial Bi atom. In SiO doped with Bi atoms2In the above formula, the effective charge of Bi atom is +0.014| e |, and the effective charge of the adjacent O atom is-1.944 | e |L. In defect-free SiO2In the case of the O atom, the effective charge is-1.957. mu.e. And defect-free SiO2In contrast, the adjacent O atom transfers about +0.013| e | to the Bi atom. Thus, about +0.027| e | is around the Bi atom, indicating that the interstitial Bi atom is near zero valence in the center.
TABLE 1 Bader Charge population analysis of defect-free and Bi-doped silica fibers
Figure BDA0001785377740000051
Fig. 4 is a diagram of energy level transitions for a Bi-doped silica fiber of the present application. In FIG. 4, the inventors calculated the energy level diagram of a Bi-doped silica fiber by the time-density functional theory (TDDFT), which explains the near-infrared luminescence at 1265 nm. The electronic structure of the Bi atom is [ Xe]4f145d106s26p3With excited states formed by outer layers of electronic structures 6s26p3And (4) calculating. For free Bi atoms, ground state 6p3Splitting to ground state due to spin-orbit coupling4S3/2And excited state2D3/2，2D5/2，2P1/2，2P3/2. The excitation state energy levels calculated by the inventor are 317nm, 472nm, 657nm and 865nm and are matched with the atomic spectrum data of Bi atoms. These excitation levels are therefore mainly due to interstitial Bi atoms2D3/2，2D5/2，2P1/2And2P3/2a contribution. When Bi atoms are introduced into the silica network,2D3/2will be split into two sub-energy levels by crystal field splitting in order of increasing energy2D3/2(1) And2D3/2(2). The ground state electrons are first excited to different excited states and then relaxed to the lowest excited state by rapid non-radiative relaxation2D3/2(1) Finally, the electron radiation in the lowest excited state emits light, having a wavelength of about 1265nm, in the range of the second telecommunications window. The absorption bands centered at 317nm, 472nm, 657nm and 865nm are mainly attributed to4S3/2→2P3/2，4S3/2→2P1/2，4S3/2→2D5/2And4S3/2→2D3/2(2). The reason why the near-infrared emission is 1265nm is that2D3/2(1)→4S3/2The result is. Therefore, the inventors believe that in a Bi-doped silica fiber, interstitial Bi atoms may be active centers for near-infrared emission, with an emission wavelength of about 1265 nm.
FIG. 5 is a schematic diagram of a process for fabricating a Bi-doped silica optical fiber preform according to one embodiment of the present application. Fig. 6 is a schematic flow chart of a method of fabricating a Bi-doped silica optical fiber preform according to one embodiment of the present application. A preparation method for the bismuth-doped silica optical fiber preform comprises the following steps:
step 100, polishing the deposition tube: using sulfur hexafluoride SF6The inner wall of the deposition tube is preferably etched in an oxygen-containing environment at a high temperature to remove organic matter or other impurities from the inner wall of the tube.
Step 200, deposition of an isolation layer: adding silicon chloride SiCl4Heating in raw material tank, preferably maintaining the heating temperature at about 1550 deg.C to ensure uniform evaporation, and carrying with oxygen O2Mixing into the deposition tube, and reacting under heating:
SiCl4+O2→SiO2+2Cl2and obtaining the silicon dioxide isolation layer.
Step 300, core region deposition: with oxygen (O)2)101 silicon chloride (SiCl) as carrier gas4) Feeding A raw material into deposition tube, and carrying bismuth oxide (Bi) with helium (He)1022O3) Mixing with carbon monoxide gas (CO)103, entering a deposition tube 104, mixing with other raw materials, adjusting the flow of oxyhydrogen flame torch 105, heating the deposition tube 104, preferably, stabilizing the heating temperature at about 1800 ℃, and reacting:
SiCl4+O2→SiO2+2Cl2，
Bi2O3+3CO→2Bi+3CO2，
obtaining a near-infrared luminous bismuth-doped silica optical fiber preform;
wherein the deposition tube 104 is a quartz tube.
Step 400, collapse of the deposition tube: the pressure in the fixed tube is maintained at positive pressure, the pressure is gradually reduced in the collapse process, and finally necking is carried out and the fixed tube is compressed into a rod in the negative pressure state. Preferably, the heating temperature during the collapsing process is maintained at about 2100 ℃.
Step 500, a mother pipe sleeve rod step: and sleeving a layer of quartz tube with proper thickness outside the rod formed in the collapsing step of the deposition tube to form a mother rod with proper core-wrapping wall. Preferably, sufficient negative pressure within the tube is achieved during the sleeving process by a vacuum pump.
The preparation method for the bismuth-doped silica optical fiber preform is prepared by adopting an improved chemical vapor deposition technology, and other doping aids are not required to be introduced, so that the structure and the operation process are simple and easy to control.
The above description is only for the preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present application should be covered within the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.

Claims (6)

1. The preparation method for the bismuth-doped silica optical fiber preform is characterized in that the bismuth-doped silica optical fiber preform comprises the following steps:
an outer layer made of silicon dioxide; and
the core layer is made of a silica material doped with Bi atoms, so that the Bi atoms are in a balance position to obtain near-infrared luminescence;
the bismuth-doped silica optical fiber preform is operated according to the following steps:
core area deposition: with oxygen O2Silicon chloride SiCl as carrier gas4Feeding the raw material into the settlerDepositing tube, carrying bismuth oxide Bi with helium He2O3Mixing the carbon monoxide gas with CO, feeding the mixture into a deposition tube, mixing the mixture with other raw materials, heating the deposition tube, and carrying out the following reactions:
SiCl4+O2→SiO2+2Cl2，
Bi2O3+3CO→2Bi+3CO2，
obtaining a near-infrared luminous bismuth-doped silica optical fiber preform;
wherein the deposition tube is a quartz tube.
2. The method of claim 1, wherein said core region deposition step is preceded by a deposition tube polishing step using sulfur hexafluoride (SF)6And etching the inner wall of the deposition tube to remove organic matters or other impurities on the inner wall of the tube.
3. The method of claim 1, wherein said core region depositing step is preceded by a spacer depositing step of silicon chloride SiCl4Heating in a raw material tank, carrying with oxygen O in a carrier gas2Mixing into the deposition tube, and reacting under heating:
SiCl4+O2→SiO2+2Cl2and obtaining the silicon dioxide isolation layer.
4. The method of claim 2, further comprising a spacer deposition step of depositing SiCl after the tube polishing step and before the core deposition step4Heating in a raw material tank, carrying with oxygen O in a carrier gas2Mixing into the deposition tube, and reacting under heating:
SiCl4+O2→SiO2+2Cl2and obtaining the silicon dioxide isolation layer.
5. The method of claim 1, wherein the core region deposition step is followed by a collapse step of the deposition tube, wherein the pressure in the deposition tube is maintained at a positive pressure, the pressure is gradually reduced during the collapse step, and finally the deposition tube is shrunk and compressed into a rod under a negative pressure state.
6. The preparation method according to claim 5, characterized in that the collapsing step of the deposition tube is followed by a rod sleeving step of a mother tube, and a layer of quartz tube is sleeved outside the rod formed in the collapsing step of the deposition tube to form the mother rod with a proper core-to-package ratio.
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CN110316954B (en) * 2019-06-28 2020-09-04 北京涑水科技有限公司 Bismuth-aluminum co-doped quartz optical fiber preform and preparation method thereof
CN115108717A (en) * 2022-06-02 2022-09-27 浙江超晶晟锐光电有限公司 Novel bismuth-erbium co-doped quartz optical fiber preform, application and preparation method

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EP1921047A1 (en) * 2005-09-01 2008-05-14 Sumitomo Electric Industries, Ltd. Process for producing glass material and process for producing optical fiber
CN101351934A (en) * 2005-09-22 2009-01-21 俄罗斯科学院纤维光学科研中心 Amplifying optical fiber operating at a wavelength in the range of 1000-1700 nm, methods of fabricating the same, and fiber laser
CN103601364B (en) * 2013-11-16 2016-01-13 华中科技大学 Composition and controlled the mixing bismuth silica fibre preparation method and mix bismuth silica fibre of valence state

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Publication number Priority date Publication date Assignee Title
CN1483007A (en) * 2000-12-22 2004-03-17 康宁股份有限公司 Treating soot preforms with a reducing agent
EP1921047A1 (en) * 2005-09-01 2008-05-14 Sumitomo Electric Industries, Ltd. Process for producing glass material and process for producing optical fiber
CN101351934A (en) * 2005-09-22 2009-01-21 俄罗斯科学院纤维光学科研中心 Amplifying optical fiber operating at a wavelength in the range of 1000-1700 nm, methods of fabricating the same, and fiber laser
CN103601364B (en) * 2013-11-16 2016-01-13 华中科技大学 Composition and controlled the mixing bismuth silica fibre preparation method and mix bismuth silica fibre of valence state

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