CN115893830B - High-phosphorus-doped optical fiber preform and preparation method thereof - Google Patents
High-phosphorus-doped optical fiber preform and preparation method thereof Download PDFInfo
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 80
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000000151 deposition Methods 0.000 claims abstract description 36
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 34
- 230000008021 deposition Effects 0.000 claims abstract description 30
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 27
- 239000011574 phosphorus Substances 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000010453 quartz Substances 0.000 claims abstract description 12
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims abstract description 4
- 239000012159 carrier gas Substances 0.000 claims description 46
- 230000002441 reversible effect Effects 0.000 claims description 21
- 239000013522 chelant Substances 0.000 claims description 20
- 229910052691 Erbium Inorganic materials 0.000 claims description 19
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 18
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 14
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 14
- 238000010304 firing Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 7
- 230000001502 supplementing effect Effects 0.000 claims description 6
- 238000005137 deposition process Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 3
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 86
- 239000010410 layer Substances 0.000 description 39
- 239000000835 fiber Substances 0.000 description 11
- KWMNWMQPPKKDII-UHFFFAOYSA-N erbium ytterbium Chemical compound [Er].[Yb] KWMNWMQPPKKDII-UHFFFAOYSA-N 0.000 description 10
- -1 erbium ion Chemical class 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 238000005253 cladding Methods 0.000 description 8
- 229910019213 POCl3 Inorganic materials 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- 238000004453 electron probe microanalysis Methods 0.000 description 4
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical group [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- 238000007740 vapor deposition Methods 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910003910 SiCl4 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 150000004697 chelate complex Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 230000008313 sensitization Effects 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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- Manufacture, Treatment Of Glass Fibers (AREA)
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Abstract
The application relates to a high phosphorus doped optical fiber preform and a preparation method thereof, comprising the following steps: introducing a first raw material into a quartz reaction tube by adopting an MCVD gas phase doping process, and positively depositing a silicon dioxide loose layer, wherein the first raw material comprises silicon tetrachloride and phosphorus oxychloride; introducing phosphorus oxychloride and oxygen, and reversely sintering to vitrify the silica loose layer, so as to finish the deposition of a phosphorus doped layer; repeating the deposition of the phosphorus doped layer for a plurality of times; and performing rod forming treatment to obtain the high-phosphorus-doped optical fiber preform. The application can solve the problem of lower P deposition concentration in the related technology.
Description
Technical Field
The application relates to the technical field of optical fiber preform manufacturing, in particular to a high-phosphorus-doped optical fiber preform and a preparation method thereof.
Background
In recent years, with the continuous progress of high-power fiber lasers, high-power fiber lasers are being used in more and more fields. In particular, in the emerging optical access network, free space optical communication, laser radar, earth gravitational wave detection, ground searching, laser ranging, etc., a 1.5 μm band high power continuous or pulsed optical fiber amplifier is required.
Ytterbium-doped high power fiber amplifiers, while technically mature, operate in the 1.06 μm band and appear to be frustrating in these applications where the 1.5 μm band is required. The damage threshold of human eyes in the 1.5 mu m wave band is higher than that in the 1.06 mu m wave band by more than 4 orders of magnitude, and the method has the characteristic of 'human eye safety', which is of great significance in the fields requiring personnel participation, such as laser ranging, laser radar, remote sensing, space communication and the like, so that people are paying attention to and developing high-power 1.5 mu m wave band optical fiber amplifiers more and more.
The erbium-ytterbium co-doped fiber is suitable for application in a 1.5 mu m wave band, and has high doping concentration and high energy conversion. Because of its high absorptivity, the product is an ideal choice for designing high-power optical amplifiers, and is widely used in different application markets, such as CATV for telecommunications and low-power laser radar.
The individually erbium-doped gain fiber cannot meet the high power operation requirements due to the concentration quenching effect. Based on the double-clad fiber cladding pumping concept, erbium-ytterbium (Er/Yb) co-doped double-clad fiber appears. The double-cladding gain fiber has the advantages that one erbium ion is surrounded by a plurality of ytterbium ions because the ytterbium ion concentration is larger than the erbium ion concentration, thereby avoiding the clustering of the erbium ions and improving the doping concentration of the erbium ions. In the doped fiber, ytterbium ions absorb pumping light first, then the erbium ions are excited through sensitization, and the population inversion of erbium wave band particles is formed, so that the advantages of wide ytterbium ion absorption band, large pumping absorption coefficient and high-power multimode pumping permission are fully utilized. Meanwhile, the erbium-ytterbium co-doped fiber has higher Yb doping concentration, and when the MCVD technology is used for preparing the prefabricated rod, the high Yb doping concentration can cause 'clusters'. Therefore, when preparing the erbium-ytterbium co-doped fiber core rod, high-concentration phosphorus P is required to be doped to improve the solubility of Yb, and meanwhile, the photodarkening is favorably inhibited. However, in actual preparation, the introduced P deposition concentration is low, so that the doping concentration of Yb cannot meet the design requirement, and how to increase the doping concentration of P becomes a problem to be solved.
Disclosure of Invention
The embodiment of the application provides a high-phosphorus-doped optical fiber preform and a preparation method thereof, which are used for solving the problem of lower P deposition concentration in the related technology.
In a first aspect, a method for preparing a high phosphorus doped optical fiber preform is provided, comprising:
introducing a first raw material into a quartz reaction tube by adopting an MCVD gas phase doping process, and positively depositing a silicon dioxide loose layer, wherein the first raw material comprises silicon tetrachloride and phosphorus oxychloride;
introducing phosphorus oxychloride and oxygen, and reversely sintering to vitrify the silica loose layer, so as to finish the deposition of a phosphorus doped layer;
repeating the deposition of the phosphorus doped layer for a plurality of times;
and performing rod forming treatment to obtain the high-phosphorus-doped optical fiber preform.
In some embodiments, the carrier gas flow rate of phosphorus oxychloride in the first raw material is 200-500 sccm, and the carrier gas flow rate of silicon tetrachloride is 200-500 sccm.
In some embodiments, the carrier gas flow rate of phosphorus oxychloride is 100-500 sccm and the flow rate of oxygen is 200-1000 sccm during reverse sintering.
In some embodiments, the first feedstock is fed simultaneously with a second feedstock comprising chelates of ytterbium and/or chelates of erbium.
In some embodiments, the carrier gas flow rate of ytterbium chelate is 200-1000 sccm and the carrier gas flow rate of erbium chelate is 200-1000 sccm.
In some embodiments, the second feedstock further comprises an aluminum chelate or aluminum trichloride.
In some embodiments, the carrier gas flow of aluminum chelate or aluminum trichloride is 100-500 sccm.
In some embodiments, the method further comprises the following steps of: oxygen of 500-2000 sccm was additionally blown.
In some embodiments, performing a rod forming process includes: and (3) carrying out rod shrinkage for a plurality of times under the condition of introducing phosphorus oxychloride and oxygen, and firing to obtain the solid optical fiber preform.
In a second aspect, there is provided a highly phosphorus doped optical fiber preform prepared by the method of preparing a highly phosphorus doped optical fiber preform as described in any one of the above.
The technical scheme provided by the application has the beneficial effects that:
The embodiment of the application provides a high-phosphorus-doped optical fiber preform and a preparation method thereof, wherein during forward deposition, a first raw material is sent into a quartz reaction tube by using carrier gas flow, silicon tetrachloride in the first raw material reacts to generate a silica loose layer with proper pores and uniform distribution, the doping uniformity is improved, phosphorus pentoxide P2O5 generated after phosphorus oxychloride reaction is doped in the silica loose layer, when ytterbium or erbium and the like are doped in the silica loose layer, the solubility of ytterbium and erbium can be improved due to the doping of P2O5, and photodarkening is inhibited.
During reverse sintering, because the P2O5 doped in the silica loose layer has a tendency to escape from the silica loose layer due to high volatility, phosphorus oxychloride and oxygen are introduced during reverse sintering so as to react to generate P2O5, and the concentration of the P2O5 in the quartz reaction tube is higher than that of the P2O5 doped in the silica loose layer, so that the volatilization of the P2O5 in the silica loose layer can be inhibited by the concentration difference in the first aspect. In the second aspect, under the action of the concentration difference, P2O5 in the quartz reaction tube with higher concentration can enter the silica loosening layer with lower concentration of P2O5 to supplement P2O5 in the silica loosening layer, so that the concentration of P2O5 in the silica loosening layer is improved, the solubility of ytterbium and erbium is further improved, and the preparation of the rare earth optical fiber perform with high doping concentration is facilitated. In the third aspect, when phosphorus oxychloride and oxygen are introduced to react to generate P2O5, the P2O5 can float forward along with the carrier gas flow, so that the P2O5 stays in the quartz reaction tube for a longer time by utilizing a reverse sintering mode, and the probability of the P2O5 entering the silica loose layer is increased. In the fourth aspect, cracks and even breakage are extremely easy to occur due to overlarge stress in the process of preparing the core rod, and the method can be used for releasing the stress of the loose layer during reverse sintering, so that breakage caused by overlarge stress accumulation is avoided.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing a high-phosphorus-doped optical fiber preform according to an embodiment of the present application;
FIG. 2 is a schematic diagram of a P2O5 concentration test according to an embodiment of the present application;
FIG. 3 is a schematic diagram of an end face of an optical fiber according to an embodiment of the present application;
fig. 4 is a schematic diagram of refractive index distribution of an optical fiber according to an embodiment of the present application.
In the figure: 1. a core region; 2. a germanium ring; 3. an inner cladding; 4. an outer cladding; 5. and (3) a protective layer.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Referring to fig. 1, an embodiment of the present application provides a method for preparing a high phosphorus doped optical fiber preform, including the steps of:
101: introducing a first raw material into a quartz reaction tube by adopting an MCVD gas phase doping process, and positively depositing a silicon dioxide loose layer, wherein the first raw material comprises silicon tetrachloride and phosphorus oxychloride.
102: And introducing phosphorus oxychloride and oxygen, and reversely sintering to vitrify the silica loose layer, so as to finish the deposition of the phosphorus doped layer.
103: The deposition of the phosphorus doped layer was repeated multiple times.
104: And performing rod forming treatment to obtain the high-phosphorus-doped optical fiber preform.
In the preparation method provided by the embodiment of the application, the carrier gas flow direction is taken as the forward direction, the forward direction deposition is understood to be the same as the carrier gas flow direction in the deposition process, and the reverse sintering is understood to be the opposite direction to the carrier gas flow direction in the sintering process.
The principle of the application is as follows:
In the application, during forward deposition, the first raw material is sent into the quartz reaction tube by using carrier gas flow, silicon tetrachloride in the first raw material reacts to generate a silica loosening layer with proper pores and uniform distribution, so that the doping uniformity is improved, phosphorus pentoxide P2O5 generated after phosphorus oxychloride reaction is doped in the silica loosening layer, when ytterbium or erbium and the like are doped in the silica loosening layer, the solubility of ytterbium and erbium can be improved due to the doping of P2O5, and photodarkening is favorably inhibited.
During reverse sintering, because the P2O5 doped in the silica loose layer has a tendency to escape from the silica loose layer due to high volatility, phosphorus oxychloride and oxygen are introduced during reverse sintering so as to react to generate P2O5, and the concentration of the P2O5 in the quartz reaction tube is higher than that of the P2O5 doped in the silica loose layer, so that the volatilization of the P2O5 in the silica loose layer can be inhibited by the concentration difference in the first aspect. In the second aspect, under the action of the concentration difference, P2O5 in the quartz reaction tube with higher concentration can enter the silica loosening layer with lower concentration of P2O5 to supplement P2O5 in the silica loosening layer, so that the concentration of P2O5 in the silica loosening layer is improved, the solubility of ytterbium and erbium is further improved, and the preparation of the rare earth optical fiber perform with high doping concentration is facilitated. In the third aspect, when phosphorus oxychloride and oxygen are introduced to react to generate P2O5, the P2O5 can float forward along with the carrier gas flow, so that the P2O5 stays in the quartz reaction tube for a longer time by utilizing a reverse sintering mode, and the probability of the P2O5 entering the silica loose layer is increased. In the fourth aspect, cracks and even breakage are extremely easy to occur due to overlarge stress in the process of preparing the core rod, and the method can be used for releasing the stress of the loose layer during reverse sintering, so that breakage caused by overlarge stress accumulation is avoided.
In the application, the carrier gas is mainly high-purity nitrogen, high-purity oxygen, high-purity helium and the like, and specific carrier gas is selected according to actual preparation requirements.
In some preferred embodiments, the carrier gas flow rate of phosphorus oxychloride in the first raw material is 200-500 sccm, and the carrier gas flow rate of silicon tetrachloride is 200-500 sccm.
During the reverse sintering, the flow rate of carrier gas of phosphorus oxychloride is 100-500 sccm, and the flow rate of oxygen is 200-1000 sccm.
For preparing rare earth doped optical fiber preforms, in some preferred embodiments, a first feedstock is fed together with a second feedstock comprising a chelate of ytterbium and/or a chelate of erbium.
Wherein the carrier gas flow rate of the ytterbium chelate is 200-1000 sccm, and the carrier gas flow rate of the erbium chelate is 200-1000 sccm.
In some preferred embodiments, the second feedstock further comprises an aluminum chelate or aluminum trichloride, and the carrier gas flow rate of the aluminum chelate or aluminum trichloride is from 100 to 500sccm. According to the actual preparation requirement, carrier gas can be used for introducing aluminum chelate or aluminum trichloride, so that the solubility of ytterbium and erbium is further improved.
In order to ensure the full reaction of the raw materials, the method further comprises the following steps of: oxygen of 500-2000 sccm was additionally blown.
After the multi-pass deposition, a tubular hollow semi-finished product is obtained, which is required to be shrunk and becomes solid, and since the inner wall of the tubular hollow semi-finished product is shrunk at a high temperature, volatilization of P2O5 occurs to a certain extent, so that the P concentration of the core region is reduced, as shown in fig. 2, wherein the abscissa unit of fig. 2 is um, and the doping concentration curve of P is concave at the central region, in some preferred embodiments, the rod forming process in step 104 includes: and (3) carrying out rod shrinkage for a plurality of times under the condition of introducing phosphorus oxychloride and oxygen, and firing to obtain the solid optical fiber preform. During rod shrinkage, phosphorus oxychloride is introduced, so that P2O5 volatilization in the central area is inhibited by supplementing P.
Example 1:
a preparation method of a high phosphorus doped optical fiber preform rod comprises the following steps:
And (3) using MCVD vapor deposition equipment to set the program as forward deposition and reverse sintering. The first pass main lamp is rapidly moved to the air inlet end and forward deposition is started. POCl3 carrier gas flow rate was set to 380sccm, siCl4 carrier gas flow rate was set to 325sccm, supplementary blown O2 flow rate was set to 2000sccm, and main lamp flame temperature was set to 1800 ℃. After the first pass of forward deposition is completed, a loose layer of SiO2 containing P is formed. When the main lamp moves reversely to perform reverse sintering, the carrier gas flow of phosphorus oxychloride is set to be 100sccm, the flow of introduced O2 is 1000sccm, and the flame temperature of the main lamp is 1950 ℃. And the cycle is repeated for a plurality of times.
And (3) inhibiting volatilization of P2O5 in the central area by adopting a P supplementing mode during rod shrinkage, and finally firing the solid single-doped P optical fiber preform through a 7-pass rod shrinkage and death firing process.
The end face was cut out by an attenuation process for electron probe concentration (EPMA) testing. The test results show that the highest P2O5 doping concentration reaches 10.83mol%.
Example 2:
a preparation method of a high phosphorus doped optical fiber preform rod comprises the following steps:
And (3) using MCVD vapor deposition equipment to set the program as forward deposition and reverse sintering. The first pass main lamp is rapidly moved to the air inlet end and forward deposition is started. The carrier gas flow rate of POCl3 was set to be 380sccm, the carrier gas flow rate of SiCl4 was set to be 325sccm, the flow rate of O2 to be additionally blown in was set to be 2000sccm, the carrier gas flow rate of Yb chelate in the high temperature material cabinet was set to be 600sccm, and the main lamp flame temperature was set to be 1800 ℃. After the first pass of forward deposition is completed, a loose layer of SiO2 containing P is formed. When the main lamp moves reversely to perform reverse sintering, the carrier gas flow of phosphorus oxychloride is set to be 100sccm, the flow of introduced O2 is 1000sccm, and the flame temperature of the main lamp is 1950 ℃. And the cycle is repeated for a plurality of times.
P2O5 volatilization in the central area is restrained by adopting a P supplementing mode during rod shrinkage, and finally the solid P and ytterbium doped optical fiber preform is fired through a 7-pass rod shrinkage and death firing process.
The end face was cut out by an attenuation process for electron probe concentration (EPMA) testing. The test result shows that the doping concentration of P2O5 at the highest point reaches 11.44mol percent, and the doping concentration of Yb2O3 is 0.81mol percent.
Example 3:
a preparation method of a high phosphorus doped optical fiber preform rod comprises the following steps:
And (3) using MCVD vapor deposition equipment to set the program as forward deposition and reverse sintering. The first pass main lamp is rapidly moved to the air inlet end and forward deposition is started. The carrier gas flow rate of POCl3 was set to be 380sccm, the carrier gas flow rate of SiCl4 was set to be 325sccm, the flow rate of O2 for supplementary blowing was set to be 2000sccm, the carrier gas flow rate of the chelate complex of Er in the high temperature cabinet was set to be 200sccm, and the main lamp flame temperature was set to be 1800 ℃. After the first pass of forward deposition is completed, a loose layer of SiO2 containing P is formed. When the main lamp moves reversely to perform reverse sintering, the carrier gas flow of phosphorus oxychloride is set to be 100sccm, the flow of introduced O2 is 1000sccm, and the flame temperature of the main lamp is 1950 ℃. And the cycle is repeated for a plurality of times.
P2O5 volatilization in the central area is restrained by adopting a P supplementing mode during rod shrinkage, and finally the solid P and erbium-doped optical fiber preform is fired through a 7-pass rod shrinkage and dead firing process.
The end face was cut out by an attenuation process for electron probe concentration (EPMA) testing. The test result shows that the doping concentration of the P2O5 at the highest point reaches 11.15mol percent, and the doping concentration of the Er2O3 is 0.078mol percent.
Example 4:
Referring to fig. 3 and 4, a method for preparing a high phosphorus doped optical fiber preform includes:
And preparing the erbium-ytterbium co-doped core rod by using MCVD vapor deposition equipment. The erbium-ytterbium co-doped core rod is firstly deposited with a matched cladding layer, then a germanium ring with NA of 0.2 is deposited, and the two parts adopt a forward deposition mode. And finally, depositing an erbium-ytterbium co-doped core region with high P doping, and depositing the erbium-ytterbium co-doped core region by adopting a forward deposition and reverse sintering mode. The first pass main lamp is rapidly moved to the air inlet end and forward deposition is started. POCl3 carrier gas flow rate was 400sccm, siCl4 carrier gas flow rate was 325sccm, supplementary blown O2 flow rate was 2000sccm, yb chelate carrier gas flow rate in the high temperature cabinet was 600sccm, er chelate carrier gas flow rate was 200sccm, and main lamp flame temperature was 1800 ℃. After the first pass of forward deposition is completed, a loose layer of SiO2 containing P is formed. When the main lamp moves reversely to perform reverse sintering, the carrier gas flow of phosphorus oxychloride is set to be 100sccm, the flow of introduced O2 is 1000sccm, and the flame temperature of the main lamp is 1950 ℃. And the cycle is repeated for a plurality of times.
P2O5 volatilization in the central area is restrained by adopting a P supplementing mode during rod shrinkage, and finally the solid P-doped erbium-ytterbium co-doped optical fiber preform is fired through a 7-pass rod shrinkage and death firing process.
The end face of the optical fiber drawn by the optical fiber preform is shown in fig. 3, and comprises a high-P erbium-ytterbium co-doped core region, a germanium ring, an octagonal Dan Yingna cladding layer, a low-refraction coating outer cladding layer and a protective layer. In fig. 4, D1 is the diameter of the core region, D2 is the diameter of the germanium ring, and D3 is the diameter of the inner cladding.
The end face was cut out by an attenuation process for electron probe concentration (EPMA) testing. The test result shows that the doping concentration of P2O5 at the highest point reaches 11.62mol percent, the doping concentration of Yb2O3 is 0.83mol percent, and the doping concentration of Er2O3 is 0.077mol percent. The main parameters of the drawn optical fiber are shown in Table 1.
TABLE 1
In the description of the present application, it should be noted that the azimuth or positional relationship indicated by the terms "upper", "lower", etc. are based on the azimuth or positional relationship shown in the drawings, and are merely for convenience of describing the present application and simplifying the description, and are not indicative or implying that the apparatus or element in question must have a specific azimuth, be constructed and operated in a specific azimuth, and thus should not be construed as limiting the present application. Unless specifically stated or limited otherwise, the terms "mounted," "connected," and "coupled" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art according to the specific circumstances.
It should be noted that in the present application, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The foregoing is only a specific embodiment of the application to enable those skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The preparation method of the high phosphorus doped optical fiber preform is characterized by comprising the following steps:
introducing a first raw material into a quartz reaction tube by adopting an MCVD gas phase doping process, and positively depositing a silicon dioxide loose layer, wherein the first raw material comprises silicon tetrachloride and phosphorus oxychloride;
introducing phosphorus oxychloride and oxygen, and reversely sintering to vitrify the silica loose layer, so as to finish the deposition of a phosphorus doped layer;
repeating the deposition of the phosphorus doped layer for a plurality of times;
Performing rod forming treatment to obtain a high-phosphorus-doped optical fiber preform;
The forward deposition is that the flame moving direction is the same as the carrier gas flow direction in the deposition process;
The reverse sintering is that the flame moving direction is opposite to the carrier gas flow direction in the sintering process;
introducing a first raw material and a second raw material at the same time, wherein the second raw material comprises ytterbium chelate and/or erbium chelate;
the second feedstock also includes an aluminum chelate or aluminum trichloride.
2. The method for preparing a highly phosphorus doped optical fiber preform according to claim 1, wherein: the carrier gas flow rate of phosphorus oxychloride in the first raw material is 200-500 sccm, and the carrier gas flow rate of silicon tetrachloride is 200-500 sccm.
3. The method for preparing a highly phosphorus doped optical fiber preform according to claim 1, wherein: and during the reverse sintering, the flow rate of carrier gas of the phosphorus oxychloride is 100-500 sccm, and the flow rate of the oxygen is 200-1000 sccm.
4. The method for preparing a highly phosphorus doped optical fiber preform according to claim 1, wherein: the carrier gas flow rate of the ytterbium chelate is 200-1000 sccm, and the carrier gas flow rate of the erbium chelate is 200-1000 sccm.
5. The method for preparing a highly phosphorus doped optical fiber preform according to claim 1, wherein: the flow rate of carrier gas of the introduced aluminum chelate or aluminum trichloride is 100-500 sccm.
6. The method for preparing a highly phosphorus doped optical fiber preform according to claim 1, wherein: in the forward deposition, the method further comprises the following steps: and (5) supplementing 500-2000 sccm of oxygen.
7. The method for preparing a highly phosphorus doped optical fiber preform according to claim 1, wherein the rod forming process comprises: and (3) carrying out rod shrinkage for a plurality of times under the condition of introducing phosphorus oxychloride and oxygen, and firing to obtain the solid optical fiber preform.
8. A high phosphorus doped optical fiber preform is characterized in that: which is prepared by the method for preparing the high phosphorus doped optical fiber preform according to any one of claims 1 to 7.
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