CN1458099A - Method for producing low water peak optic fiber prefabricated piece - Google Patents
Method for producing low water peak optic fiber prefabricated piece Download PDFInfo
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- CN1458099A CN1458099A CN 03128870 CN03128870A CN1458099A CN 1458099 A CN1458099 A CN 1458099A CN 03128870 CN03128870 CN 03128870 CN 03128870 A CN03128870 A CN 03128870A CN 1458099 A CN1458099 A CN 1458099A
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- core rod
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- optical fiber
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 239000000835 fiber Substances 0.000 title description 10
- 239000013307 optical fiber Substances 0.000 claims abstract description 84
- 238000005245 sintering Methods 0.000 claims abstract description 69
- 238000001035 drying Methods 0.000 claims abstract description 55
- 239000000460 chlorine Substances 0.000 claims abstract description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 25
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 15
- 239000011521 glass Substances 0.000 claims abstract description 14
- 239000005373 porous glass Substances 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 125000001309 chloro group Chemical group Cl* 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 65
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 51
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 19
- 238000010926 purge Methods 0.000 claims description 16
- 229910052805 deuterium Inorganic materials 0.000 claims description 12
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims description 11
- 239000012159 carrier gas Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 5
- 238000005253 cladding Methods 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims 5
- 239000001307 helium Substances 0.000 claims 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 description 12
- 239000000843 powder Substances 0.000 description 9
- 238000007740 vapor deposition Methods 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 239000002274 desiccant Substances 0.000 description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012792 core layer Substances 0.000 description 2
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000004155 Chlorine dioxide Substances 0.000 description 1
- 229910006113 GeCl4 Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910006124 SOCl2 Inorganic materials 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019398 chlorine dioxide Nutrition 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- XLYOFNOQVPJJNP-DYCDLGHISA-N deuterium hydrogen oxide Chemical compound [2H]O XLYOFNOQVPJJNP-DYCDLGHISA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229920006240 drawn fiber Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007496 glass forming Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- -1 hydrogen compound Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003534 oscillatory effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Classifications
-
- 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]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
-
- 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
- C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
- C03B2201/22—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with deuterium
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Thermal Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The production process of the present invention can further lower the OH content in prefabricated optical fiber piece, and includes the steps of preparing loose core rod body, chlorine drying, sintering the core rod body, drawing to form glass core rod, coating with silica layer, drying porous glass prefabricated part and sintering. It features the isotope D-H interchange drying step completed and the secondary chlorine drying step between the chlorine drying step and the core rod body sintering step. The isotope D-H interchange drying step is completed inside the sintering furnace and at least one of D2O gas or D2 is introduced into the furnace. Through the said process, low water peak prefabricated optical fiber piece with light attenuation at 1383 nm wavelength less than 0.32 dB/km may be produced. The process is economic and introduces no excessive environmental pollution.
Description
[ technical field]A method for producing a semiconductor device
The present invention relates to the field of optical fibers, and in particular to a method for manufacturing an optical fiber preform.
[ background of the invention]
Currently, inorganic optical fibers are widely used in the communication industry, wherein quartz optical fibers are the main body of inorganic optical fibers due to their characteristics of low optical loss, wide applicable light wave range, and long-distance communication. In recent years, the preparation of silica-based optical fibers has been significantly advanced, eliminating most of the extrinsic attenuation (except for hydroxyl ion absorption), and improving the ability of optical fibers to transmit usable light, and the attenuation caused by hydroxyl groups becomes an important factor of the total attenuation of optical fibers.
On the attenuation spectrum of the silica-based optical fiber, a higher water absorption peak, generally called a water peak, is generally formed in the 1383nm wavelength range between the 1310nm region (1280 nm-1325 nm) of the second transmission window and the 1550nm region (1380 nm-1565 nm) of the third transmission window, and the usable electromagnetic wave is prevented from passing through the 1380nm window. Hydrogen atoms and SiO in the glass matrix2、GeO2And oxygen in other oxygen-containing compounds combine to form OH/OH2. Due to OH/OH in the glass2The resulting attenuation is about 0.5-1.0 dB/km, with the peak attenuation typically being within the "1380 nm window" (defined as the wavelength range of about 1330-1470 nm). With recent advances in Wavelength Division Multiplexing (WDM), amplifier technology, and laser sources, it is increasingly important to eliminate the 1380nm water peak.
Silica optical fibers are obtained by drawing optical fiber preforms having a structure similar to that of optical fibers. The preparation of the quartz-based optical fiber preform comprises the following steps: the hydrolyzed silicon compound is first vaporized and then introduced into a combustion gas flame where the gas is thermally decomposed to form fine silica powder, which is finally vitrified to form a transparent article. This process, the powder method, can be used for the manufacture of quartz glass doped with oxides containing higher gas pressures, such as B2O3、P2O5、GeO2. Currently, there are three main types of powder processes in use, namely: outside Vapor Deposition (OVD), modified chemical vapor deposition process (MCVD), and axial vapor deposition process (VAD).
At present, a loose body of a core rod of an optical fiber preform is generally manufactured by one of powder processes, and the loose body is sintered in an atmosphere containing chlorine gas after being chemically dried, thereby forming a core rod preform; the core rod preform is then placed in a redraw furnace and heated to a temperature sufficient to draw it into a smaller diameter cylindrical glass body, the core rod. After the drawing step, the resulting core rod is coated with a soot of silica powder around it, typically by any one of Outside Vapor Deposition (OVD), Modified Chemical Vapor Deposition (MCVD) and axial vapor deposition (VAD), such as by OVD deposition. The soot coated core rod is chemically dried and then sintered to forman optical fiber preform, which may then be drawn into an optical fiber. Despite the use of chemical drying and sintering steps, the attenuation of such optical fibers measured at about 1380nm is still considerable.
The hydrogen-containing impurities and hydroxyl impurities in the raw material halide, the water gas in the carrier gas and OH in the quartz glass tube are diffused, so that the optical fiber preform prepared by the powder method process has high hydroxyl content, and the drawn optical fiber is polluted by the hydroxyl. In order to prevent the optical fiber from being contaminated by hydroxyl groups and reduce the attenuation caused by water peaks, various measures are taken, such as refining the raw material gas and purifying the carrier gas to remove the water gas contained in the gas; the pipeline is closed, and a quartz glass tube with low OH content and the like are adopted. Among them, it is most effective to perform chemical dehydration by using thionyl chloride (SOCl) before vitrification2) Chlorine (Cl)2) And the substitution reaction of the chemical reagent on hydroxyl radical to halogenate the prefabricated optical fiber product. Since the fundamental vibration absorption peak of Si-Cl generated as a result of the reaction is located in the vicinity of 25 μm, the absorption attenuation by the vibration of Si-Cl bond does not have a significant influence on the transmission attenuation of the optical fiber in the wavelength region in which the optical fiber is used. Chemical stripping by halogenationWater is very effective in reducing the residual OH content. For example, in the VAD method, moisture is mainly derived from gases produced by the flame hydrolysis reaction. Although most of the gas is exhausted through the exhaust outlet, there is still considerable H2O is adsorbed in the optical fiber preform, and the optical fiber preform prepared by VAD is subjected to Cl2After chemical dehydration, the OH contentcan be reduced to 10 ppb; the attenuation of the drawn fiber in the "1380 nm window" was 0.5 dB/km.
However, the halogenated dehydration method cannot meet the technical requirements of further reducing the OH content of the optical fiber preform and further greatly reducing the water peak attenuation under the current process conditions.
[ summary of the invention]
The technical problem to be solved by the invention and the technical task are to overcome the technical defects existing in the manufacturing of the existing optical fiber prefabricated member and provide a manufacturing method capable of further reducing the OH content in the optical fiber prefabricated member so as to obtain the low water peak optical fiber prefabricated member more conveniently on the premise of not influencing the main quality of the optical fiber prefabricated member.
The manufacturing method of the low water peak optical fiber preform comprises the following steps:
(1) preparing a loose core rod body, namely preparing a loose core rod body,
(2) the loose core rod body adopts chlorine (Cl)2) Or thionyl chloride (SOCl)2) The mixture is dried and then is dried,
(3) sintering and stretching the loose core rod body to form a vitreous core rod,
(4) coating a silica cladding on the outer surface of the glass core rod to form a porous glass prefabricated member,
(5) the porous glass preform is dried and,
sintering the porous glass preform into an optical fiber preform, characterized in that chlorine (Cl) is used as the core rod loose material2) Or thionyl chloride (SOCl)2) After the drying step, performing isotope D-H exchange drying on the loose core rod body, wherein the isotope D-H exchange drying is performed in a sintering furnace, and heavy water (D) is introduced into a gas inlet of the sintering furnace2O) gas and deuterium gas (D)2) At least one of (a) and (b),temperature in the furnaceKeeping the temperature at 1200-1300 ℃, and drying for 60-360 minutes. (isotopic D-H exchange drying means subjecting a loose mass of porous preform rods in D-enriched state at elevated temperature2O or D2Is infiltrated in an atmosphere of (1), wherein isotope D atoms are substituted for H atoms adsorbed in the loose body, is defined as carrying out isotope D-H exchange drying)
In order to achieve better effect, the core rod loose body is subjected to an isotope D-H exchange drying step and then secondary chlorine (Cl) is carried out2) Drying step, secondary chlorine (Cl)2) The drying time is 180-360 minutes (according to the length of the loose core rod body). Chlorine dioxide (Cl)2) And drying, and then sintering and stretching the loose core rod into a glass core rod.
Preparation of a core rod bulk as in the prior art of silica optical fiber core rods for making optical fiber preforms, even though a flowing gas mixture containing at least one glass-forming precursor compound undergoes a flame hydrolysis reaction to form a stream of silica-based powder; the reaction product is partially deposited on the end surface of the seed rod to form a growth surface and is gradually stacked in the axial direction to form a loose body of the core rod for manufacturing the optical fiber preform. The core rod loose body is then chlorine gas (Cl) at the appropriate concentration2) Or thionyl chloride (SOCl)2) Carrying out primary chemical drying in the atmosphere; thereafter, chlorine is switched to heavy water (D)2O) gas or deuterium gas (D)2) Or heavy water (D)2O) gas and deuterium gas (D)2) The loose body of the porous preform rod core rod is enriched in D2O or D2Or the mixture of the two, and fully carrying out isotope D-H exchange drying; and finally, sintering and stretching the glass body into a cylindrical glass body with a smaller diameter in an atmosphere containing chlorine gas to form the glass body core rod. The core rod has an average hydroxyl content of less than about 1ppb by weight. And coating a silica cladding around the obtained core rod, performing conventional chemical drying on the porous glass preform covered with the soot layer, and sintering to form the optical fiber preform. Forming a low water peak optical fiber preform capable of being used to produce an optical attenuation at a wavelength of 1383nm of less than 0.32 dB/km.
The isotope D-H exchange drying step can also be carried outChlorine (Cl) of loose core rod body2) Or thionyl chloride (SOCl)2) The same effect can be achieved by performing the chemical drying in the atmosphere before the primary chemical drying.
The "water peak" is essentially caused by the harmonic wave caused by the O-H absorption vibration. The stretching vibration of the O-H bond can be approximated as a simple harmonic vibration. According to the definition of simple harmonic vibration and the method of classical mechanics, the vibration of diatomic molecules is discussed, and the calculation formula of the vibration frequency of the diatomic molecules as harmonic vibration is as follows:
v＝1304(k/M)0.5
the substitution of atoms in the molecule by its isotopes has little effect on interatomic distances and the chemical bond force constant (k). The vibration frequency of the OD can thus be determined from the relationship between the vibration frequencies of the two isotopesand the reduced mass of the molecule (v1/v2 — M1/M2) 0.5).
vH＝10000/2.72＝3676cm-1；
MH＝16*1/(16+1)＝0.94；
MD＝16*2/(16+2)＝1.78；
The calculated OD fundamental frequency is vD 2671cm-1And the wavelength is 3.74 mu m.
From the formula, replacing the H atom with the heavier isotope D atom increases the reduced mass and reduces the fundamental frequency, and thus the frequency of each harmonic is also reduced correspondingly, i.e. the corresponding wavelength is increased. Therefore, the water peak moves towards the long wave direction, and the calculation result shows that the water peak moves out of the 1280-1600 nm area. While OD contributes little to the light absorption in the relevant wavelength range, since the specific absorption of OD is about 2 orders of magnitude less than the specific absorption of OH in the relevant wavelength range, i.e. the 1380nm window. In addition, D2O and H2The exchange reaction efficiency of O is high, and the content of H in the optical fiber preform can be greatly reduced in a short time.
TABLE 1H-D interchange results in a shift in the wavelength of the relevant oscillatory wave (vibrational part closely related to the "1380 Window")
Frequency H-wavelength D-wavelength
(μm) (μm)
v1+2v3 1.24 1.62
2v3 1.38 1.87
2v1+v3 1.90 2.31
v1+v3 2.22 2.85
v3 2.72 3.74
In the optical fiber preform preparation chamber, a halide raw material, such as SiCl4、GeCl4And the like, wherein argon is used for carrying current through a gas supply system, and the gas is sprayed out of an oxyhydrogen burner to form fine glass powder through flame hydrolysis reaction. These fine glass powders are deposited on the growing end of a quartz target rod that is rotated in the axial direction, thereby growing a cylindrical, porous optical fiber preform core rod. The flame hydrolysis reaction equation is as follows:
the obtained porous core rod of optical fiber preform is in a state of containing a large amount of H2O molecule preparation chamber atmosphere, so that the optical fiber preform itself adsorbs water (H) by physical adsorption2O) and/or chemisorbed water (β OH) adsorbs much H2And O molecules are required to be dried to be sintered to obtain the core rod with low water content. Meanwhile, once the optical fiber preform core rod is exposed to the atmosphere or the atmosphere containing a hydrogen compound before sintering, the optical fiber preform core rod adsorbs water again and becomes "wet" regardless of the short exposure time.
At present, the dehydrating agent used for chemical drying is generally Cl2Or SOCl2And the like. Practice proves that the catalyst is subjected to Cl2The VCD method core rod obtained by sintering after drying still remains until10ppb less OH; the attenuation of the optical fiber obtained by drawing the prefabricated member made of the core rod is still more than or equal to 0.5dB/km at the wavelength of 1383 nm.
The invention adopts Cl for the core rod of the optical fiber prefabricated part2Drying and using D2O or D2Performing D-H exchange drying, and performing two drying methods, wherein the optical fiber preform core rod is processed twice (Cl)2Drying and using D2O or D2D-H exchange drying) or more than two times (Cl)2Drying,By D2O or D2D-H exchange drying and secondary Cl2Drying) to reduce 10ppb OH in the optical fiber preform to about 1ppb, and the attenuation of the prepared optical fiber at about 1383nm is reduced from the current more than or equal to 0.5dB/km to less than or equal to 0.32dB/km
The invention has the beneficial effects that: 1) the water content in the optical fiber preform can be greatly reduced, especially the central part of the optical fiber preform, i.e. GeO2Water content of the core portion. The optical field distribution of the optical fiber shows that the transmission of the light beam is almost concentrated on the core layer of the optical fiber, the water content of the core layer part of the optical fiber prefabricated part is reduced, and the effect of achieving twice the result with half the effort on reducing the light attenuation can be achieved. Optical fibers made from such optical fiber preforms can exhibit much smaller water peaks at 1380nm and generally in the 1380nm window, and thus, exhibit lower optical attenuation in the 1380nm window than optical fibers made from preforms produced by conventional preform production methods (e.g., VAD, MCVD, OVD, etc.). 2) The optical fiber manufactured by the optical fiber preform manufactured by the method can work under a certain arbitrarily selected wavelength within the wavelength range of about 1300-1680 nm, and does not have large optical attenuation. Specifically, such fibers exhibit an attenuation of less than about 0.32dB/km, preferably less than about 0.30dB/km,at each wavelength in the wavelength range of about 1300 to 1680 nm. 3) The method of the invention is very economical to implement and does not additionally generate environmentally unfriendly waste during implementation. The invention will now be further described by way of example with reference to the accompanying drawings.
[ description of the drawings]
FIG. 1 is a schematic illustration of a loose body of a mandrel suspended in a sintering furnace.
The reference numerals in the figures illustrate: 1-a mandrel loose mass; 2-sintering furnace; 3-furnace atmosphere; 4-gas inlet.
[ detailed description]embodiments
Example 1 a cylindrical loose core rod body having a length of about 500mm, which was prepared in a conventional manner, was placed above the interior of a sintering furnace, the temperature of the sintering furnace was maintained at about (1260 ± 20) ° c, He was initially introduced from a gas inlet at a flow rate of 30SLPM to purge the loose core rod body of a porous preform for about 15 minutes in advance, and after the purging, a drying agent Cl was introduced2Drying was carried out for 60 minutes. While, the flow rate was 0.25SLPM Cl2And 20SLPM of He was passed through a sintering furnace to complete the primary drying. Then, the sintering furnace is purged by He with the flow rate of 30SLPM for 15 minutes; the sintering furnace gas is converted into heavy water (D)2O) gas for 360 minutes, D-H exchange drying was performed. D2O gas was generated by a heavy water bubbler, which was maintained at 85 deg.C; he at a flow rate of 3.5SLPM was passed through the bubbler as a carrier gas, while a flow of He at 20SLPM was passed through the sintering furnace. And then, descending the porous preform core rod loose body, enabling the porous preform core rod loose body to enter a furnace hot zone (1560 +/-20 ℃), and enabling He with the flow rate of 20SLPM to flow through a sintering furnace for sintering to obtain a compact core rod. The rod is redrawn, coated by OVD and other modes to obtain a porous glass prefabricated member, dried and sintered to obtain a cylindrical glassy optical fiber prefabricated rod with a low water peak, and the rod is drawn into an optical fiber through wire drawing, wherein the optical attenuation is as follows:
| 1310nm | 1383nm | 1550nm | cut-off wavelength | Diameter of fiber |
| 0.369dB/km | 0.312dB/km | 0.239dB/km | 1300nm | 125μm |
Example 2 a cylindrical porous preform rod loose body having a length of about 500mm was placed above the interior of a sintering furnace, the temperature of the sintering furnace was maintained at about 1200 to 1300 ℃, and at the beginning, the porous preform rod loose body was purged with He at a flow rate of 30SLPM for about 15 minutes in advance. After purging, a drying agent Cl is introduced2Drying was carried out for 60 minutes. While, the flow rate was 0.25SLPM Cl2And 20SLPM of He was flowed through the sintering furnace. Then, the introduction of Cl was stopped2Heavy water (D) was introduced into the furnace in the He sintering furnace at a flow rate of 30SLPM for about 15 minutes2O) gas (flow rate of He carrier gas is 3L/min, bubbler temperature is maintained at 80 ℃), while flow of He at 20SLPM through the sintering furnace, after 300 minutes, switching to purge the furnace with He at flow rate of 30SLPM for about 15 minutes; after purging, Cl was switched at a flow rate of 0.250SLPM2And 20SLPM in He, dried for 240 minutes. Raising the furnace temperature to 1560 ℃, closing the chlorine gas, and sintering to obtain the compact core rod. The rod is redrawn, coated by OVD and other modes, dried and sintered to obtain the cylindrical glass optical fiber with low water peakThe rod is made, and drawn into an optical fiber by drawing, and the optical attenuation of the optical fiber is as follows:
| 1310nm | 1383nm | 1550nm | cut-off wavelength | Diameter of fiber |
| 0.351dB/km | 0.318dB/km | 0.203dB/km | 1284nm | 125μm |
Example 3 a cylindrical porous preform rod loose body prepared in a conventional manner was placed above the inside of a sintering furnace, the temperature was maintained at about 1200 to 1300 ℃, and at the beginning, the porous preform rod loose body was previously purged with He at a flow rate of 30SLPM for about 15 minutes. After purging, a drying agent Cl is introduced2Drying was carried out for 60 minutes. While, the flow rate was 0.25SLPM Cl2And 20SLPM He flow through the sintering furnace; thereafter, with a flow rate of 30SLPMHe purging the sintering furnace for 15 minutes; then, deuterium (D) gas of 0.4-0.8 SLPM is introduced2) And 20SLPM He gas flow through a sintering furnace, and the mixed gas is used for purging the preform core rod loose body for more than 120 minutes; d2At a partial pressure of at least 1333 Pa. And descending the loose body of the core rod of the porous preform rod, enabling the loose body to enter a hot zone of a furnace, and enabling the He with the flow rate of 20SLPM to flow through a sintering furnace for sintering to obtain the compact core rod. The rod was redrawn, clad by OVD, chemically dried, sintered, and drawn into optical fiber with optical attenuation as follows:
| 1310nm | 1383nm | 1550nm | cut-off wavelength | Diameter of fiber |
| 0.382dB/km | 0.314dB/km | 0.245dB/km | 1310nm | 125μm |
Example 4 a cylindrical porous preform rod loose mass prepared in a conventional manner was placed above the inside of a sintering furnace, the temperature was maintained at about 1200 to 1300 ℃, and at the beginning, the porous preform rod was previously purged with Heat a flow rate of 30SLPMThe mandrel loosens for about 15 minutes. After purging, a drying agent Cl is introduced2Drying was carried out for 60 minutes. While, the flow rate was 0.25SLPM Cl2And 20SLPM He flow through the sintering furnace; then, the sintering furnace is purged by He with the flow rate of 30SLPM for 15 minutes; then, 0.4SLPM deuterium gas (D)2) Flows through D with 3-4 SLPM2Carrier gas He (containing D) of O bubbler (bubbler temperature is kept at 75-85℃)2O gas) is introduced into the sintering furnace at the same time, and mixed gas is blown to the prefabricated part for more than 60-360 minutes together with the He gas flow of 20 SLPM; and descending the loose body of the porous preform rod, enabling the loose body to enter a hot zone of a furnace, and enabling the He with the flow rate of 20SLPM to flow through a sintering furnace for sintering to obtain the compact core rod. The rod is redrawn, clad, dried, sintered, and then drawn into an optical fiber.
Its light attenuation is as follows:
| 1310nm | 1383nm | 1550nm | cut-off wavelength | Diameter of fiber |
| 0.341dB/km | 0.317dB/km | 0.225dB/km | 1281nm | 125μm |
Example 5 a cylindrical porous preform core rod loose body having a length of about 500mm was placed above the interior of a sintering furnace, the temperature of the sintering furnace was maintained at about 1200 to 1300 ℃, and He at a flow rate of 30SLPM was initially introduced into a gas inlet to purge the porous preform core rod loose body in advance for about 15 minutes. After purging, D is introduced2O。D2The O gas is composed of heavy water (D)2O) bubbler generation, flow rate of carrier gas He is 4SLPM, bubbler temperature is kept at 75 ℃; at the same time, a flow of He at 20SLPM is passed through the sintering furnace. Stopping introducing the heavy water after 240 minutes, and then purging the heating furnace for about 15 minutes by He with the flow rate of 30 SLPM; cl switching flow of 0.25SLPM2And 20SLPM in He, dried for 180 minutes. And raising the furnace temperature to 1560 ℃, closing the chlorine gas, and sintering to obtain the compact core rod. The rod is redrawn, coated by VAD and other modes to obtain a porous glass preform, dried and sintered to obtain a cylindrical glassy optical fiber preform with a low water peak, and drawn into an optical fiber by drawing, wherein the optical attenuation is as follows:
| 1310nm | 1383nm | 1550nm | cut-off wavelength | Diameter of fiber |
| 0.364dB/km | 0.335dB/km | 0.214dB/km | 1308nm | 125μm |
Example 6 differs from example 4 in that after the D-H exchange is completed, 0.25SLPM Cl is used2And 20SLPM of He, and drying the loose body again for 180 to 360 minutes (the loose body passes through the high-temperature zone at a speed of about 3.3 mm/min). The final cylindrical glassy state optical fiber preform with low water peak is drawn into an optical fiber by drawing, and the optical attenuation is as follows:
| 1310nm | 1383nm | 1550nm | cutting blockStop wavelength | Diameter of fiber |
| 0.346dB/km | 0.317dB/km | 0.219dB/km | 1311nm | 125μm |
Example 7 is different from example 5 in that deuterium gas of 0.4 to 0.8 is used to perform D-H exchange on the loose bodyD-H exchange, wherein the treatment time is 180-300 minutes. The final cylindrical glassy state optical fiber preform with low water peak is drawn into an optical fiber by drawing, and the optical attenuation is as follows:
| 1310nm | 1383nm | 1550nm | cut-off wavelength | Diameter of fiber |
| 0.346dB/km | 0.317dB/km | 0.219dB/km | 1311nm | 125μm |
Example 8 differs from example 5 in that the flow rate was 3SLPM passing D at 85 ℃2Carrier gas He of O bubbler, deuterium gas (D) of 0.4SLPM2) Mixing, and jointly acting on the loose bodies for about 120-360 minutes to perform D-H exchange, and simultaneously, enabling the He gas flow of 20SLPM to pass through a sintering furnace. The final cylindrical glassy state optical fiber preform with low water peak is drawn into an optical fiber by drawing, and the optical attenuation is as follows:
| 1310nm | 1383nm | 1550nm | cut-off wavelength | Diameter of fiber |
| 0.358dB/km | 0.32dB/km | 0.213dB/km | 1324nm | 125μm |
Generally, the time for introducing heavy water is different from 60min to 360min according to the length of the loose core rod body, and the long-acting effect is better. D carried by carrier gas2The mass of O is at least 0.27g/min (as listed in the table below), i.e.the partial pressure is greater than 1333 Pa. The effects as in the above table can be achieved.
TABLE 2 carry D at different He flows2Mass of O (g/min)
Claims (10)
1. A method of making a low water peak optical fiber preform comprising the steps of:
(1) preparing a loose core rod body, namely preparing a loose core rod body,
(2) the loose core rod body adopts chlorine (Cl)2) Or thionyl chloride (SOCl)2) The mixture is dried and then is dried,
(3) sintering and stretching the loose core rod body to form a vitreous core rod,
(4) coating a silica cladding on the outer surface of the glass core rod to form a porous glass prefabricated member,
(5) the porous glass preform is dried and,
(6) sintering the porous glass preform into an optical fiber preform, characterized in that chlorine (Cl) is used as the core rod loose material2) Or thionyl chloride (SOCl)2) After the drying step, performing isotope D-H exchange drying on the loose core rod body, wherein the isotope D-H exchange drying is performed in a sintering furnace, and heavy water (D) is introduced into a gas inlet of the sintering furnace2O) gas and deuterium gas (D)2) At least one of the above-mentioned (B) is dried for 60-360 minutes while the temperature in the furnace is kept at 1200-1300 ℃.
2. The method of claim 1 in which the core rod bulk is subjected to an isotope D-H exchange drying step and in step (3) the core rod bulk is sintered and drawn to a vitreous core rod with secondary chlorine (Cl) gas between the core rods2) Drying step, secondary chlorine (Cl)2) The drying time is 180-360 minutes.
3. The method of claim 1 or 2, wherein the core rod bulk isotope D-H exchange drying is performed by first using Cl at a flow rate of 0.25SLPM2And (3) enabling the He of the 20SLPM to flow through the sintering furnace, then blowing the sintering furnace for 10-20 minutes by using the He (20-30 SLPM) with a large flow rate, and converting the sintering furnace gas into heavy water (D)2O) gas for 60-360 minutes.
4. A method of manufacturing a low water peak optical fiber preform according to claim 3, characterized in that the sintering furnace gas is switched to heavy water (D)2O) heavy water bubbler was used for the gas, the temperature setting range of the bubbler was: introducing He with the flow rate of 2-4L/min as carrier gas into a sintering furnace at the temperature of 75-85 ℃ to obtain D2The mass of O is 0.3-0.9 g/min.
5. A method for manufacturing a low water peak optical fiber preform according to claim 1 or 2, wherein D-H exchange drying is performed by introducing D into a sintering furnace during D-H exchange drying of the bulk isotope of the core rod2Gas for 60-360 minutes, D2The partial pressure of (A) is 1333 Pa-4000 Pa.
6. A method of manufacturing a low water peak optical fiber preform according to claim 1 or 2, wherein heavy water (D) is introduced at a gas inlet of a sintering furnace during D-H exchange drying of the bulk isotope of the core rod2O) and D2Mixing the gas, and the specific process is as follows: blowing the sintering furnace by He with the flow rate of 20-30 SLPM for 10-20 minutes, then,he as carrier gas at 3SLPM flows through D2O bubbler (bubbler temperature is set at 75-85 ℃), and the bubbler outputs gas (containing D)2O gas and He) and deuterium gas (D) of 0.4SLPM2) And blowing the loose core rod body together for 60-360 minutes, and simultaneously passing the He gas of 20SLPM through a sintering furnace.
7. A method of making a low water peak optical fiber preform comprising the steps of:
(1) preparing a loose core rod body, namely preparing a loose core rod body,
(2) the loose core rod body adopts chlorine (Cl)2) Or thionyl chloride (SOCl)2) The mixture is dried and then is dried,
(3) sintering and stretching the loose core rod body to form a vitreous core rod,
(4) coating a silica cladding on the outer surface of the glass core rod to form a porous glass prefabricated member,
(5) the porous glass preform is dried and,
(6) sintering the porous glass preform into an optical fiber preform, characterized in that chlorine (Cl) is used as the core rod loose material2) Or thionyl chloride (SOCl)2) Before the drying step, isotope D-H exchange drying is carried out on the loose core rod body, the isotope D-H exchange drying is carried out in a sintering furnace, and heavy water (D) is introduced into a gas inlet of the sintering furnace2O) gas and deuterium gas (D)2) At least one of the above-mentioned (B) is dried for 60-360 minutes while the temperature in the furnace is kept at 1200-1300 ℃.
8. The method of claim 7, wherein the step of drying the loose core rod by isotope D-H exchange comprises blowing He at a gas inlet of the sintering furnace at a flow rate of 30SLPM for about 15 minutes to pre-purge the porous preform core rod, and then blowing heavy water (D) after purging2O) gas for 60-180 min, heavy water (D)2O) gas is generated by a heavy water bubbler, carrier gas He passes through the bubbler at the flow rate of 3-4L/min, the temperature of the bubbler is kept at 75-85 ℃, and meanwhile, the He gas flow of 20SLPM passes through a sintering furnace.
9. The method of claim 7 wherein the step ofdrying the loose core rod by D-H exchange comprises introducing D into a sintering furnace2Gas for 60-360 min, D2The partial pressure of (A) is 1333 Pa-4000 Pa.
10. The method of claim 7, wherein the core rod bulk isotope D-H exchange drying is performed by purging a sintering furnace with He at a flow rate of 30SLPM for 15 minutes, and then flowing 3-4L (He) of the (He) gas through D2An O bubbler (the temperature of the bubbler is kept between 75 and 85 ℃), a mixed gas of heavy water gas and helium gas flowing out of the bubbler, and 0.4SLPM deuterium gas (D)2) And simultaneously introducing the core rod loose body into a sintering furnace, and purging the core rod loose body for 60-360 minutes together with the He gas flow of 20 SLPM.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100340508C (en) * | 2004-11-29 | 2007-10-03 | 长飞光纤光缆有限公司 | Method for manufacturing optical fiber unsensitive to hydrogen |
| CN101912968A (en) * | 2010-08-20 | 2010-12-15 | 西北有色金属研究院 | Suspension sintering method of slender powder metallurgy tube/bar blank |
| CN102149648A (en) * | 2008-09-09 | 2011-08-10 | 信越化学工业株式会社 | Process for producing optical-fiber base material |
| CN112805252A (en) * | 2018-08-08 | 2021-05-14 | 康宁股份有限公司 | Method for manufacturing halogen-doped silica preform for optical fiber |
| CN112939443A (en) * | 2021-01-29 | 2021-06-11 | 华南理工大学 | High borosilicate glass cladding cesium iodide single crystal core optical fiber and preparation method and application thereof |
-
2003
- 2003-05-23 CN CN 03128870 patent/CN1234633C/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100340508C (en) * | 2004-11-29 | 2007-10-03 | 长飞光纤光缆有限公司 | Method for manufacturing optical fiber unsensitive to hydrogen |
| CN102149648A (en) * | 2008-09-09 | 2011-08-10 | 信越化学工业株式会社 | Process for producing optical-fiber base material |
| CN101912968A (en) * | 2010-08-20 | 2010-12-15 | 西北有色金属研究院 | Suspension sintering method of slender powder metallurgy tube/bar blank |
| CN112805252A (en) * | 2018-08-08 | 2021-05-14 | 康宁股份有限公司 | Method for manufacturing halogen-doped silica preform for optical fiber |
| CN112805252B (en) * | 2018-08-08 | 2023-04-04 | 康宁股份有限公司 | Method for manufacturing halogen-doped silica preform for optical fiber |
| CN112939443A (en) * | 2021-01-29 | 2021-06-11 | 华南理工大学 | High borosilicate glass cladding cesium iodide single crystal core optical fiber and preparation method and application thereof |
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|---|---|
| CN1234633C (en) | 2006-01-04 |
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