CN103663958B - A kind of method for preparing preformod of optical fiber with low water peak - Google Patents

A kind of method for preparing preformod of optical fiber with low water peak Download PDF

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CN103663958B
CN103663958B CN201310437888.0A CN201310437888A CN103663958B CN 103663958 B CN103663958 B CN 103663958B CN 201310437888 A CN201310437888 A CN 201310437888A CN 103663958 B CN103663958 B CN 103663958B
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powder
optical fiber
preformod
preparing
low water
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CN103663958A (en
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沈小平
吴仪温
王强强
范修远
张亮
李震宇
蒋小强
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Tongding Interconnection Information Co Ltd
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Tongding Interconnection Information Co Ltd
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    • YGENERAL 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
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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Abstract

The present invention relates to a kind of method for preparing preformod of optical fiber with low water peak, this method is comprised the following steps:(a)Use vapor axial method(VAD)SiO is included in target rod deposition2, GeO2Deng powder;(b)After the completion for the treatment of that body of powder is deposited in target rod, target rod is detached from body of powder;(c)Handle sturcture is installed into tubulose body of powder one end, the other end installs plug, tubulose body of powder tubular glass body will be dehydrated and sintered into heating furnace of the body of powder feeding filled with dehydrated air and heat-conducting gas by handle sturcture;(d)Corroded in tubular glass body two ends welding extension tube after sintering, the liquid for being placed on hydrofluoric acid containing, cleaning treatment is carried out to its central bore region and outer surface, clear its is placed in clean environment and dried;(e)Dried tubular glass body is transferred in the electrothermal furnace containing oxygen and fluoro-gas and carries out melting contracting;(f)By the glass bar outsourcing covering after stretching or direct wire drawing into optical fiber.

Description

A kind of method for preparing preformod of optical fiber with low water peak
Technical field
The invention belongs to fiber optic communication field, it is related to a kind of manufacture method of preform, specifically a kind of gas Phase axial deposition method(VAD)Prepare the manufacture method of preformod of optical fiber with low water peak in large size.
Background technology
Preform manufacture typically uses two-step process, i.e., first manufacture plug, then in mandrel outer using different Technology manufactures surrounding layer.Typical plug manufacture method has following four:Modified chemical vapor deposition method(MCVD), plasma Strengthen chemical vapor deposition method(PCVD), pipe outside vapor deposition(OVD)With axial vapor deposition method(VAD).Surrounding layer is manufactured Technology has tiretube process and Direct precipitation outsourcing according to the classification of outer packet mode, has OVD according to the preparation technology of clad material classification, VAD and APVD methods.Surrounding layer to material purity require it is relatively low, index distribution section is single, according to its outsourcing side The difference or the difference of outsourcing material magazine content of formula, select the plug of suitable core bag proportioning.The manufacture of plug determines optical fiber The performance of product, is the key technology for preparing optical fiber.
Now common VAD method is described briefly.Figure 12 is the equipment schematic diagram of common double lamp VAD techniques.Such as Figure 12 institutes Show, the first blowtorch 13 and the second blowtorch 14 are used to spray such as hydrogen and oxygen but are not limited to hydrogen and oxygen fuel, such as argon Gas but be not limited to the protection gas such as argon gas and such as silicon tetrachloride, germanium tetrachloride but be not limited to the two be used for react generation two The reactive material of the powder such as silica and germanium dioxide.By taking silicon tetrachloride and oxyhydrogen flame as an example, the spray of the first and second blowtorch 13,14 When the hydrogen and oxygen fueled combustion penetrated, in the region close to the surface of the first and second blowtorch 13,14, from the first and second blowtorch The chemical substance SiCl of 13,14 injections4Temperature drastically raise, when described chemical substance reaches and more than the chemical reaction Temperature both about 1300 DEG C when, oxidation as described below and hydrolysis are proceeded by, so as to generate the oxide of silicon, particle The SiO of shape2
SiCl4+ O2→ SiO2+ 2Cl2(oxidation)
SiCl4+ 2H2O → SiO2+ 4HCl (hydrolysis)
The particle produced is moved together with the high-temperature gas from described deposition blowlamp injection, then existing by thermophoresis On surface around the prefabricated rods relatively low as being deposited on temperature, the thermograde around the circular prefabricated rods causes this Thermophoresis phenomenon.
In actual production process, different types of reactive material of the first and second blowtorch 13,14 is supplied to by control The refractive index of covering 22 can be more than by making the refractive index of plug 21, for example, add four chlorinations in the first blowtorch of deposition of core layer 21 Germanium, so as to realize that the sedimentary refractive index of sandwich layer 21 is more than covering 22.
In actual production process, by the angle and the week that adjust the particle beam that the first blowtorch and the second blowtorch are ejected Enclose Temperature Distribution, make powder sandwich layer 21 and covering 22 simultaneously toward axially and radially growing, by the laser in sandwich layer end or Photographic equipment 41 implements the growth pattern of tracking end, the lift end of feedback control prefabricated rods(It is not drawn into)Pull rate.
For low water peak single mode fiber preparation, relative to OVD techniques, traditional VAD techniques due in the absence of center target rod, It need not consider that centre bore interface is polluted by extraneous hydrogen containing foreign during sintering and collapsing, be adapted to prepare low water peak, zero water Peak fiber, but be due to the support without target rod, the blowtorch in bosom needed in deposition process and meanwhile take into account powder radially and Axial direction growth rate, substantially increase the difficulty of technology controlling and process, be similarly limited to the ratio of the radial and axial deposition of powder with And the equilibrium relation of collection efficiency, it greatly limit the sedimentation rate that VAD methods prepare plug.Specifically by taking Figure 12 as an example, powder After the port injection of blowtorch 13 comes out, direction and the regulation of temperature field surrounding by powder stream form the footpath of sandwich layer 21 To the growth with axial direction, the end of sandwich layer 21 is in hemispherical, and adjustment angle powder can shape towards radial and axial increase anyway Into an equalization point, radially faster axial direction also can be faster, due in the actual production process of preformod of optical fiber with low water peak plug, Covering and sandwich layer diameter than general control between 3 to 7, it is more in the case of 5 or so, that is to say, that the diameter of sandwich layer 21 reaches During 50mm, the diameter of covering 21 must reach 250mm, and diameter, which to reach be dehydrated after certain size and sinter, can all turn into problem, That is the growth rate of sandwich layer radial direction is restricted in actual applications, so the growth of axial direction can be also limited, so as to limit The sedimentation rate of prefabricated rods is made.
By taking the following two patent analyses on VAD techniques as an example:
Chinese patent(CN 1952848A)" vapor axial precipitation equipment and gas phase axial deposition method " reports one kind and adopted With two blowtorch, blowtorch one with deposited powder on the end of the straight soot preforms of axis, so as to grow sandwich layer;Blowtorch Two sandwich layer outside deposited powder, so as to grow covering.The soot preforms tail end detected by temperature detector Relativeness between first and second relative maximum temperatures, and relative minimum temperature therebetween, setting three, passes through Analysis and the difference of setup parameter, control unit is by adjusting blowtorch one, the gas flow and composition of blowtorch two, blowtorch position with And soot preforms lift speed to control the total quality of soot preforms.
United States Patent (USP)(US20120103023A1)" method of manufacture preform " discloses one kind and takes two sprays Lamp, blowtorch one with deposited powder on the end of the straight soot preforms of axis, so as to grow sandwich layer;Blowtorch two is in sandwich layer For deposited powder around, so as to grow covering.The shape of soot preforms is detected by CCD imagers.Pass through graphical analysis Software analysis detects the difference between shape and setting shape, and blowtorch gas flow and composition, blowtorch are adjusted using control system The lifting speed of position and soot preforms controls the total quality of soot preforms.
Such preparation method has following problem:
A) tail end of soot preforms both needs to control Temperature Distribution, needs to control shape again, process parameter control is multiple Miscellaneous, quantity-produced stability is not high;
According to soot rods profile feedback control pull rate and blowtorch powderject speed, powder density lack of homogeneity holds Easily because prefabricated rods weight and volume itself is continuously increased, Powder Rod is caused to ftracture, sedimentation rate is limited, production efficiency reduction.
The content of the invention
Complicated, the problem of efficiency is low and there is speed limit for above-mentioned control, the invention discloses a kind of new VAD deposition process, provides the target rod of sandwich layer deposition in whole deposition process, simplifies the density in Powder Rod growth course, several What size Control, improves deposition efficiency and speed, while providing a kind of reduction due to being present in center in dehydration and sintering process The method of the hydrogen containing foreign in hole, prepares the preform preparation method available for LWPF.
To reach above-mentioned purpose, the scheme that its technical problem of present invention solution is taken is:It is this to prepare LWPF The method of prefabricated rods, this method is comprised the following steps:
(a)Use vapor axial method(VAD)SiO is included in target rod deposition2, GeO2Deng powder.Joined by setting technique Number includes target rod lifting speed and the delivery rate of different blowtorch, feed gaseous species and feed gas content, to ensure doping And geometrical homogenization.
(b)After the completion for the treatment of that body of powder is deposited in target rod, target rod is detached from body of powder, in being centrally formed for body of powder Along the centre bore of axis.
(c)Handle sturcture is installed into tubulose body of powder one end, the other end installs plug, then by handle sturcture by powder Tubulose body of powder is dehydrated and sintered into tubular glass body by body feeding in the heating furnace filled with dehydrated air and heat-conducting gas.
(d)Tubular glass body two ends welding extension tube after sintering, the tubular glass body is placed in the liquid of hydrofluoric acid containing Corroded in vivo, then carry out cleaning treatment to tubular glass body central bore region and outer surface, then by the tubulose after cleaning Vitreum is placed in clean environment and dried;
(e)Dried tubular glass body is transferred in the electrothermal furnace containing oxygen and fluoro-gas and carries out melting contracting, is melted Need to vacuumize in one end of tubular glass body during contracting, make central area interior orientation stream of the gas after the condensation of tubular glass body It is dynamic.In compression process is melted, tubular glass body is kept rotating along axis, and tubular glass body can be carried out simultaneously in compression process is melted Stretching.
(f)By the glass bar outsourcing covering after stretching or direct wire drawing into optical fiber, the optical fiber is in 1383nm wavelength attenuations Less than 0.35dB/km.
By such scheme, the optical fiber that the preform of preparation is drawn is less than 0.31dB/ in the attenuation of 1383nm wavelength km
By such scheme, the OH mass contents of tubular glass body central area are less than 1ppb in the step e;
By such scheme, the prefabricated rods vapor axial method in the step a uses at least two deposition blowlamps.
By such scheme, the first blowtorch in the step is deposited in target rod, and the second blowtorch deposits powder in the first blowtorch Deposited on end, the 3rd blowtorch is deposited on the second blowtorch deposited powder, and so on.
By such scheme, the innermost layer for being used for deposited powder layer in the vapor axial method is deposited on pre- mounted in axis side To rotation target rod on, the target rod be glass or ceramic material.
By such scheme, plug is the column glass material that hydroxyl mass content is less than 10ppm in the step c.
By such scheme, the dehydration of tubulose body of powder is in one kind containing chlorine, helium and oxygen or many in the step c Carried out in the atmosphere for the mixed gas planted in heating furnace.
By such scheme, the step d includes the extension tube for keeping original deposition initiating terminal, and excision deposition terminates containing for end The glass of plug, terminates to weld extension tube at the glass containing plug at end in excision deposition.
By such scheme, tubular glass body is placed in the liquid of hydrofluoric acid containing and corroded in the step e, in centre bore The thickness that tubular glass body is corroded is not less than 50 μm.
By such scheme, the tubular glass body corrosion thickness is not less than 500 μm.
By such scheme, the cleaning liquid deionized water in the step e.
By such scheme, in the step e before condensation, atmosphere under heating environment to central area and in Heart bore region glass carries out chemical attack, dehydration using fluoro-gas.
By such scheme, the step of described chemical attack, dehydration in the fluoro-gas that uses for C2F6And O2Mixing Gas.
By such scheme, the hydroxyl matter mass content requirement of the gaseous mixture is less than 1ppm.
By such scheme, the temperature of the heating furnace in described step e is 1600 to 2200 degree, and heating furnace translational speed is 10~80mm/min, overpressure is -100 pa of pa to+100.
Compared with prior art, usefulness of the present invention is:This method for preparing preformod of optical fiber with low water peak is reasonable Sintering is assigned with, is dehydrated, the function of collapsing stretching possesses high deposition efficiency, sedimentation rate, control is simple, is adapted to prepare various Large-sized preformod of optical fiber with low water peak of core bag ratio, greatly reducing the manufacturing cost of optical fiber, there is provided band center target rod VAD deposition process, greatly reduce core bag deposition physical dimension proportioning, geometrical homogenization mixes the difficulty of uniformity, is adapted to In many lamp plane SH waves, the large size prefabricated rod of various core bag geometry and refractive index structures is prepared.
Brief description of the drawings:
The present invention is further described below in conjunction with the accompanying drawings.
Fig. 1 is the process chart for the method that the present invention prepares preformod of optical fiber with low water peak;
Fig. 2 is axial gas phase method of the invention(VAD)The deposition schematic diagram of double blowtorch;
Fig. 3 is axial gas phase method of the invention(VAD)The deposition schematic diagram of many blowtorch;
Fig. 4 is dehydration of the end in the present invention without the body of powder of plug, sinters schematic diagram;
Fig. 5 is the dehydration of body of powder of the end with plug in the present invention, sinters schematic diagram;
Fig. 6 is the vitreum sectional view of sintering rear center direct polycondensation in the present invention;
Fig. 7 is the vitreum sectional view that is not condensed of sintering rear center in the present invention;
The schematic diagram that Fig. 8 extends again after the two ends cutting for glass tube after being sintered in the present invention;
Fig. 9 corrodes schematic diagram to extend and corroding in the present invention in electrothermal furnace after hydrogen desiccation;
Figure 10 for the present invention in extend and corrode after hydrogen desiccation electrothermal furnace collapsing stretch schematic diagram;
Figure 11 is the attenuation spectrogram of pulling optical fiber preform in the present invention;
Figure 12 is the schematic diagram of common VAD equipment.
In figure:10th, centre bore;11st, axis;12nd, body of powder;13rd, the first blowtorch;14th, the second blowtorch; 15、16、 Blowtorch;18th, vitreum;19 tubular glass bodies;21st, sandwich layer;22nd, 23,24, sedimentary;31st, target rod;32nd, extension tube; 33rd, plug;34th, conveying mechanism;50th, heating furnace;51st, heating cavity;61st, electrothermal furnace;63rd, vavuum pump.
Embodiment
Below in conjunction with the accompanying drawings and embodiment the present invention will be described in detail:
A kind of method for preparing preformod of optical fiber with low water peak shown in Fig. 1, this method is comprised the following steps:
(a)Use vapor axial method(VAD)SiO is included in the deposition of target rod 312, GeO2Deng powder, wherein the first blowtorch 13 in the outside deposition of core layer 21 of target rod 31, and the grade blowtorch of the second blowtorch 13 is deposited in sandwich layer periphery, so as to grow covering.By setting Technological parameter such as target rod lifting speed and the delivery rate of different blowtorch, feed gaseous species and feed gas content are determined, to protect Card doping and geometrical homogenization;
(b)After the completion for the treatment of that body of powder 12 is deposited in target rod 31, target rod 31 is detached from body of powder 12, in body of powder 12 The centre bore 10 being centrally formed along axis 11;
(c)Handle sturcture is installed into the one end of tubulose body of powder 12, the other end installs plug 33, then will by handle sturcture Tubulose body of powder 12 is dehydrated and sintered into pipe by body of powder feeding in the heating furnace 50 filled with dehydrated air and heat-conducting gas Shape vitreum 19.
(d)The two ends of tubular glass body 19 welding extension tube 32 after sintering, hydrogeneous fluorine is placed in by the tubular glass body 19 Corroded in the liquid of acid, cleaning treatment is then carried out to the central bore region of tubular glass body 19 and outer surface, then will cleaning Tubular glass body 19 afterwards is placed in clean environment and dried;
(e)Dried tubular glass body 19 is transferred in the electrothermal furnace containing oxygen and fluoro-gas and carries out melting contracting, Need to vacuumize in one end of tubular glass body when melting contracting, make central area interior orientation of the gas after the condensation of tubular glass body 19 Flowing.In compression process is melted, tubular glass body 19 keeps rotating along axis 11, can be simultaneously to tubular glass in compression process is melted Body 19 is stretched;
(f)By the glass bar outsourcing covering after stretching or direct wire drawing into optical fiber, the optical fiber is in 1383nm wavelength attenuations Less than 0.35dB/km.
Different from common VAD methods depositing operation, in the VAD method depositing operations provided in the present invention to deposition of core layer the The deposition of one blowtorch 13 all 31 progress in the target rod of a rotation, Powder Rod is cutd open after first layer according to refractive index from inside to outside It is the second, the three or more blowtorch successively the need for face or sedimentation rate.
The schematic diagram for double lamp VAD deposition process that Fig. 2 provides for the present invention.As shown in Fig. 2 the first blowtorch 13 and the second spray Lamp 14 is used to spray such as hydrogen and oxygen but is not limited to hydrogen and oxygen fuel gas, such as argon gas but is not limited to argon gas Protect gas and such as silicon tetrachloride, germanium tetrachloride but be not limited to the two be used for react generation silica and germanium dioxide etc. The reactive material of the siliceous and germanium of powder.The fluid comprising silica and germanium dioxide particle of reaction generation is along flame direction It is ejected into the target rod 31 rotated along axis 11, due to the presence of target rod 31, collection efficiency of the powder in target rod 31 is carried significantly Height, relative to common VAD methods, the collection efficiency of powder is improved to 50~70% by 20~40%;As the common VAD methods of Figure 12 pass through The laser or photographic equipment that are placed near the Powder Rod tapering of sandwich layer 21 measure change or the temperature of the physical dimension in tapering in real time Sensing equipment measures the Temperature Distribution in tapering, the lifting speed of feedback control Powder Rod, so as to control the diameter of Powder Rod in real time Uniformity.The method that the present invention is provided can cancel the feedback control components, ensure to mix by setting corresponding technological parameter Miscellaneous and geometrical homogenization.The fluid of the silica containing particle ejected from the second blowtorch 14 is sunk with sandwich layer 21 for target Product and grow, due to the presence of center target rod 31, greatly improve the sedimentation rate of sandwich layer 21, in actual applications can be the Increase the second blowtorch the 14, the 3rd or more blowtorch outside one blowtorch 13 further to improve the overall sedimentation rate of plug.
The schematic diagram that such as Fig. 3 deposits for a kind of VAD methods of many lamps in the present invention, according to the silica of setting component, two The powder such as germanium oxide are by the first blowtorch 13, the second blowtorch 14, blowtorch 15 and 16 sprays and be deposited into corresponding sedimentary 22, 23rd, 24, wherein each sedimentary 22,23,24 is concentric with center target rod 31, in the number or single blowtorch by increasing blowtorch Reactant flow, can improve the sedimentation rate of body of powder 12, by harmonizing silicon tetrachloride in each lamp, germanium tetrachloride and other The content of dopant can obtain the prefabricated rods of more refractive index profiles.
After the completion for the treatment of that target size and the body of powder adulterated are deposited in target rod 31, target rod 31 is taken out from body of powder 12 From, as shown in figure 4, the axle center for removing the body of powder 12 of center target rod 31 occurs in that centre bore 10, and for holding body of powder 12 top extension tube 32. extension tube 32 is placed on be placed in the top of dehydrothermal stove 50 move up and down and rotate it is defeated Send in mechanism 34.Body of powder 12 is transported in heating furnace 50 by conveying mechanism 34, heating furnace 50 is risen to 1000 to 1200 Degree, while injecting the gas for dehydrating and removing impurities and heat conduction in heating cavity 51, the gas is preferably chlorine and helium Gaseous mixture, rotates and moves up and down body of powder 12, by wherein hydrogen containing foreign and other impurities in 1000 to 1200 temperature spent Under the conditions of removed by chemical method, the temperature in cavity is then promoted to 1500 degree or so, powder porous loosening body is burnt Form vitreum 18.
Such as Fig. 5 preferably in the end of body of powder 12, installs the plug 33 that can be engaged with centre bore 10 in the present invention, The glassy zone that the plug 33 is preferably near the vitreum that hydroxy radical content is less than 10 ppm, the centre bore 10 is that light guide is fine The position in bosom is tieed up, most of light influences the strongest in the regional spread, the purity in the region on the optical property of optical fiber, On the other hand, in the high-temperature process for being dehydrated and sintering, if not installing gas stream in plug 33, centre bore 10 in end Speed and flow are significantly greater than the situation for installing plug 33, are likely to result in the impurity attachment in cavity, more seriously, cross high temperature Degree and the chlorine gas environment of high concentration cause the volatilization and oxidation of the position germanium dioxide, influence refractive index profile distribution, after increase The difficulty of continuous processing.
In production application, exemplified by it there is the technique of centre bore 10 after this depositions of OVD and PCVD, main contains Hydrogen impurity is to be diffused into the region in the water before centre bore 10 is condensed and in condensation course in environment, such as will contain centre bore During 10 tubular glass body 19 is transferred to condensation stove, the gas diffusion containing moisture in environment to the area of centre bore 10 Domain, the optical fiber of made preform has big absworption peak in 1383nm wave bands, it is impossible to prepare LWPF.Study table Face:When central bore region is positioned over containing in hydrogen atmosphere, such as in air, the water of physical absorption(H2O)With the water of chemisorbed(- OH)It is bonded in central bore region on glass rapidly, moisture is higher, standing time, more long this absorption was more strong, and And no matter how short this standing time have, its hydrogen containing foreign spread causes optical fiber water peak exceeded enough.
In the present invention, as shown in fig. 6, be dehydrated and sintering function body of heater in, by the region of centre bore 10 Negative pressure slightly is provided, the tiny structure is preferably less than -100pa, body of powder 12 is directly burnt till into center condensation in the atmosphere Vitreum 18.Then target physical dimension is redrawn into as needed, and its optical fiber prepared meets low water peak light in 1383nm Fine requirement.
The scheme of prioritizing selection is in sintering furnace, to be sintered directly into such as the tubular glass body 19 in Fig. 7 in the present invention, should Scheme has taken into account the demand of large-size mandrel posterior drawing processing, and collapsing function is placed on into the step, is not increasing technique stream On the premise of journey, the method for the region of centre bore 10 reprocessing has been invented.Such as the method that Fig. 4 is provided, containing for center interval is solved The problem of hydroxyl impurity, but the region germanium dioxide volatilizees and aoxidized in the dehydration more than 1000 degree and sintering process, makes burning The centre line zone refractive index reduction of prefabricated rods, forms center lower limit, influences the optical property of optical fiber after knot.In the present invention, first Sinter tubular glass body 19 into, the increase hydrofluoric acid corrosion in subsequently docking cleaning process, increase contains fluorine gas in drawing process Body remove water and corrosion method, remove the relatively low containing water impurity and the region Ge content of centre bore 10 and inner boundary region Part.
As shown in figure 8, after body of powder 12 sinters tubular glass body 19 into, in its end on extension tube 32, the glass Glass pipe 32 is preferably that hydroxy radical content is less than 10ppm, and the tubular glass body 19 of two ends glass tube respectively is positioned over into hydrofluoric acid containing Corrosion cleaning is carried out in solution to barred body interface, the inner wall corrosion thickness of centre bore 10 is more than 50um, and optimal state is greater than 0.5mm, is cleaned tubular glass body 19 after corrosion, and optimum state is cleans with deionized water, then by the rod after cleaning Body is placed in the environment of dry gas and dried.
Such as tubular glass body 19 is placed in electrothermal furnace 61 by Fig. 9,10, is filled with one end of tubular glass body 19 containing fluorine gas Body, the gas is preferably the gaseous mixture of oxygen and fluoro-gas, and the fluoro-gas is preferably C2F6, by the tubulose glass filled with gas Glass body 19 is heated in electrothermal furnace, and heating-up temperature is more than 1500 degree, make the hydrous matter in environment and center in centre bore 10 The region of hole 10 includes water section and reacted away with freon, is vavuum pump 63 at other one section of tubular glass body 19, determines gas To flowing, while reaction product is detached into centre bore 10 by pump 63.
According to setting program to the region removal of impurities of centre bore 10 and corrosion after, as shown in Figure 10, by the temperature liter of electrothermal furnace 61 To 2000 degree or so, continue to be less than -100 pa slightly negative pressure in the end position of vavuum pump 63, progressively centre bore 10 is condensed, is Guarantee centre bore 10 region glass part has preferable axial symmetry, and whole collapsing process keeps tubular glass body 19 along axle Line 11 rotates.In the collapsing method of the present invention, solid can be stretched simultaneously, be drawn into the tubulose glass of target external diameter Glass body 19.
Collapsing will be appealed and be stretched to the glass bar of target external diameter, it is outer again according to the core bag diameter proportion of final glass optical fiber Corresponding covering is wrapped, the surrounding layer can also be outside the method Direct precipitation such as OVD, VAD or APVD by tiretube process Bag, by the preform after outsourcing into demand external diameter glass optical fiber, due to take the present invention provide dehydration sintering Scheme optimal in direct collapsing and the present invention in stove, i.e., increase dehydrogenation process before collapsing and during collapsing stretching, The center aperture layer of avoiding contains higher hydroxyl.The hydroxy radical content in the final region is less than 1ppb, and the optical fiber drawn is in 1383nm There is the absworption peak less than 0.31dB/km near wavelength.
Figure 11 is the attenuation spectrogram that prefabricated rods and the optical fiber being drawn into are prepared using the method for the bright offer of this law, wherein 91 are Using the VAD deposition process of the bright middle offer of this law but without the light prepared by chemical method dehydrogenation during follow-up sintering Fine attenuation spectrum, 92 be first to be cleaned and dried using what is provided in invention with hydrofluoric acid corrosion, then in air-flow environment containing freon The preform of middle condensation is drawn into the attenuation spectrogram of optical fiber, and 93 be using the VAD deposition process provided in invention and de- The attenuation spectrogram for the preform for being dehydrated and sintering in water sintering furnace.
The present invention is described in further detail below by specific embodiment;Following four embodiment is contained respectively is burning Direct polycondensation prepares G652 preforms in freezing of a furnace, and double lamps deposit and pass through hydrofluoric acid, freon corrosion and then collapsing stretching G652 preforms are prepared, three lamps deposit and pass through hydrofluoric acid, G657 optical fiber is prepared after freon corrosion and then collapsing stretching The embodiment of prefabricated rods.
Embodiment 1
Using the ceramic target rods of a diameter of 8mm in VAD methods deposition, deposition of core layer and covering powder are distinguished using two blowtorch Layer diameter is to 55mm and 200mm, and its center core layer is SiO2With GeO2Mixture, covering is SiO2Powder, body of powder averag density is 0.55gram/cm3, powder body length is 1000mm.Deposition removes ceramic target rod after terminating from body of powder, is installed in its end External diameter is 8.1mm, and length is 90mm solid glass rod, and the solid bar is the high purity quartz that hydroxyl mass content is less than 1ppm Rod.Then body of powder is transferred to the delivery platform of dehydration-sintering furnace, prefabricated rods are put in dehydration-sintering furnace from top to bottom, are Avoid the volatilization of center germanium dioxide doped layer from causing the center of section to be sunk, poise the big chi that sandwich layer sedimentation diameter reaches 55mm It is very little to design to dilute sagging influence, in order to avoid the too high glass caused in sintering furnace of furnace temp when centre bore is condensed Inner bag softening transform, without using glass inner bag in the sintering furnace, uses graphite inner container near hot-zone.
Hot zone temperature is risen to 1100 DEG C, 40SLPM helium is filled with the bottom of sintering furnace, 5SLPM chlorine, body of powder with 400mm/min speed passes through the hot-zone of sintering furnace from top to bottom, completes after above-mentioned dehydration procedure, and sintering furnace temperature is increased to 1500 DEG C, maintenance chlorine and helium atmosphere flow are constant, and body of powder enters overheated zone from bottom to top with 7mm/min speed, realize The sintering of body of powder, sintering circuit provides centre bore 100pa negative pressure in body of powder top extension rod after terminating, by hot zone temperature 1900 DEG C are increased to, helium gas flow 10SLPM is reduced to, chlorine gas flow is reduced to 2SLPM, by sintered body with 5mm/min Speed is from top to bottom through overheated zone, condensation center hole.Solid bar after condensation is stretched to external diameter 41mm, using OVD method outsourcings To 150mm solid bars, wire drawing optical fiber result such as table 1:
Cladding diameter 1310nm attenuations 1383nm attenuations 1550nm attenuations
125µm 0.338dB/km 0.291dB/km 0.196dB/km
Embodiment 2
Using the ceramic target rods of a diameter of 8mm in VAD methods deposition, deposition of core layer and covering powder are distinguished using two blowtorch Layer diameter is to 18mm and 220mm, and its center core layer is SiO2With GeO2Mixture, covering is SiO2Powder, body of powder averag density is 0.55gram/cm3, powder body length is 1000mm.Deposition removes ceramic target rod after terminating from body of powder, is installed in its end External diameter is 8.1mm, and length is 90mm solid glass rod, and the solid bar is the high purity quartz that hydroxyl mass content is less than 1ppm Rod.Then body of powder is transferred to the delivery platform of dehydration-sintering furnace, prefabricated rods are put in cavity liner from top to bottom for glass In the dehydration-sintering furnace of pipe.
Hot zone temperature is risen to 1100 DEG C, 40SLPM helium is filled with the bottom of sintering furnace, 5SLPM chlorine, body of powder with 400mm/min speed passes through the hot-zone of sintering furnace from top to bottom, completes after above-mentioned dehydration procedure, and sintering furnace temperature is increased to 1500 DEG C, maintenance chlorine and helium atmosphere flow are constant, and body of powder enters overheated zone from bottom to top with 7mm/min speed, realize The sintering of body of powder;Then the glass tube end after sintering is docked into extension tube, the assembly after docking is corroded with hydrofluoric acid To centre bore aperture increases 1mm, dried 12 hours in the gas that drying nitrogen is purged, then first with 1700 in electrothermal furnace DEG C temperature, at center, internal control is filled with 1SLPM oxygen and 0.5SLPM freon(C2F6), body of heater is with 30mm/min speed edge Axially past vitreum 18, apply 100pa negative pressure after etching at one end through vavuum pump, while furnace temperature is risen into 2000 Degree, is condensed with 15mm/min translational speed to glass tube.The prefabricated rods of condensation are drawn into optical fiber, light in fiber drawing furnace Fine result such as table 2:
Cladding diameter 1310nm attenuations 1383nm attenuations 1550nm attenuations
125µm 0.333dB/km 0.308dB/km 0.192dB/km
Embodiment 3
Using the ceramic target rods of a diameter of 8mm in VAD methods deposition, deposition of core layer, the first covering are distinguished using three blowtorch With the second covering powder bed diameter to 65mm, 160mm and 280mm, its center core layer is SiO2With GeO2Mixture, covering is SiO2 Powder, body of powder averag density is 0.55gram/cm3, powder body length is 800mm.Deposition is removed after terminating from body of powder Ceramic target rod, it is 8.1mm that external diameter is installed in its end, and length is 90mm solid glass rod, and the solid bar contains for hydroxyl quality High purity quartz rod of the amount less than 1ppm.Then body of powder is transferred to the delivery platform of dehydration-sintering furnace, by prefabricated rods from upper and Under put in cavity liner be glass tube dehydration-sintering furnace in.
Hot zone temperature is risen to 1100 DEG C, 40SLPM helium is filled with the bottom of sintering furnace, 5SLPM chlorine, body of powder with 400mm/min speed passes through the hot-zone of sintering furnace from top to bottom, completes after above-mentioned dehydration procedure, and sintering furnace temperature is increased to 1500 DEG C, maintenance chlorine and helium atmosphere flow are constant, and body of powder enters overheated zone from bottom to top with 7mm/min speed, realize The sintering of body of powder;Then the glass tube end after sintering is docked into extension tube, the assembly after docking is corroded with hydrofluoric acid To centre bore aperture increases 1mm, the light internal drying purged in drying nitrogen 12 hours, then first with 1700 DEG C in electrothermal furnace Temperature, at center, internal control is filled with 1SLPM oxygen and 0.5SLPM freon(C2F6), body of heater is with 30mm/min speed along axle To vitreum 18 is passed through, apply 100pa negative pressure after etching at one end through vavuum pump, while furnace temperature is risen into 2000 DEG C, glass tube is condensed and stretched with 12mm/min translational speed.It is 43mm by preform bar stretching external diameter, by outside 43mm It is that 46mm external diameters are that 150mm hydroxyls mass content is less than in 1ppm sleeve pipe that footpath plug, which is placed in internal diameter, is directly melted on wire-drawer-tower Contracting wire drawing is to 125um external diameters.Its optical fiber result such as table 3:
Cladding diameter 1310nm attenuations 1383nm attenuations 1550nm attenuations
125µm 0.332dB/km 0.295dB/km 0.189dB/km
Embodiment 4
The embodiment is the preparation method of the bend insensitive fiber prefabricated rods using three blowtorch.
Using the ceramic target rods of a diameter of 8mm in VAD methods deposition, deposition of core layer, the first covering are distinguished using three blowtorch With the second covering powder bed diameter to 45mm, 62mm and 180mm, its center core layer is SiO2With GeO2Mixture, the first covering is SiO2Powder, the second covering is fluorine-containing SiO2Powder, body of powder averag density is 0.5gram/cm3, powder body length is 800mm. Deposition removes ceramic target rod after terminating from body of powder, and it is 8.1mm that external diameter is installed in its end, and length is 90mm solid glass Rod, the solid bar is the high purity quartz rod that hydroxyl mass content is less than 1ppm.Then body of powder is transferred to dehydration-sintering furnace Delivery platform, prefabricated rods is put in from top to bottom in the dehydration-sintering furnace that cavity liner is glass tube.
Hot zone temperature is risen to 1100 DEG C, 40SLPM helium is filled with the bottom of sintering furnace, 5SLPM chlorine, body of powder with 400mm/min speed passes through the hot-zone of sintering furnace from top to bottom, completes after above-mentioned dehydration procedure, and sintering furnace temperature is increased to 1450 DEG C, maintenance chlorine and helium atmosphere flow are constant, and body of powder enters overheated zone from bottom to top with 8mm/min speed, realize The sintering of body of powder;Then the glass tube end after sintering is docked into extension tube, the assembly after docking is corroded with hydrofluoric acid To centre bore aperture increases 1mm, dried 12 hours in the cavity that drying nitrogen is purged, then first with 1700 DEG C in electrothermal furnace Temperature, at center, internal control is filled with 1SLPM oxygen and 0.5SLPM freon(C2F6), body of heater is with 30mm/min speed along axle To vitreum 18 is passed through, apply 100pa negative pressure after etching at one end through vavuum pump, while furnace temperature is risen into 2000 DEG C, glass tube is condensed and stretched with 20mm/min translational speed.By preform bar stretching external diameter to 41mm, then will 41mm external diameters plug is using OVD methods outsourcing to 150mm solid bars, wire drawing optical fiber result such as table 4:
This method reasonable distribution for preparing preformod of optical fiber with low water peak sintering, dehydration, the function of collapsing stretching possesses High deposition efficiency, sedimentation rate, control is simple, is adapted to the large-sized preformod of optical fiber with low water peak for preparing various core bag ratios, The manufacturing cost of optical fiber is greatly reduced there is provided the VAD deposition process with center target rod, core bag deposition geometry is greatly reduced Size is matched, and geometrical homogenization mixes the difficulty of uniformity, is suitable for many lamp plane SH waves, prepares various core bag geometry and folding Penetrate the large size prefabricated rod of rate structure.
It is emphasized that:It the above is only presently preferred embodiments of the present invention, not make any formal to the present invention Limitation, any simple modification that every technical spirit according to the present invention is made to above example, equivalent variations and modification, In the range of still falling within technical solution of the present invention.

Claims (12)

1. a kind of method for preparing preformod of optical fiber with low water peak, this method is comprised the following steps:
(a) using vapor axial method (VAD), deposition includes SiO in target rod (31)2And GeO2Powder, by set technique join Number includes target rod (31) lifting speed and the delivery rate of different blowtorch, feed gaseous species and feed gas content, to ensure Doping and geometric proportion and uniformity;
(b) after the completion for the treatment of that body of powder (12) is deposited in target rod (31), target rod (31) is detached from body of powder (12), in powder The centre bore (10) being centrally formed along axis (11) of body (12);
(c) handle sturcture is installed into tubulose body of powder (12) one end, the other end installs the plug that hydroxy radical content is less than 10ppm (33), then body of powder is sent into tubulose powder in the heating furnace (50) filled with dehydrated air and heat-conducting gas by handle sturcture Opisthosoma (12) is dehydrated and sintered into tubular glass body (19);
(d) tubular glass body (19) two ends welding extension tube (32) after sintering, the tubular glass body (19) is placed in hydrogeneous Corroded in the liquid of fluoric acid, the interior tubulose vitreum (19) of centre bore (10) is corroded thickness not less than 50 μm, then to pipe Shape vitreum (19) centre bore (10) region and outer surface carry out cleaning treatment, then the tubular glass body (19) after cleaning is placed in Dried in clean environment;
(e) dried tubular glass body (19) is transferred to containing oxygen and C of the hydroxyl mass content requirement less than 1ppm2F6 Carry out melting contracting in the electrothermal furnace of gas, need to vacuumize in one end of tubular glass body when melting contracting, make gas in tubular glass body (19) the central area interior orientation flowing after being condensed, in compression process is melted, tubular glass body (19) keeps rotating along axis (11), Tubular glass body (19) is stretched simultaneously in compression process is melted;Before condensation, to the gas of central area under heating environment Atmosphere and centre bore (10) region glass use C2F6And O2Gaseous mixture carry out chemical attack, dehydration;
(f) by the glass bar outsourcing covering after stretching or direct wire drawing into optical fiber, the optical fiber is less than in 1383nm wavelength attenuations 0.35dB/km。
2. the method according to claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:The light of the step f The fine attenuation in 1383nm wavelength is further below 0.31dB/km.
3. the method as claimed in claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:Tubulose in the step e The hydroxyl mass content of vitreum (19) central area is less than 1ppb.
4. the method according to claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:In the step a Prefabricated rods vapor axial method uses at least two deposition blowlamps.
5. the method according to claim 4 for preparing preformod of optical fiber with low water peak, it is characterised in that:First blowtorch during deposition (13) deposited in target rod, the second blowtorch (14) is deposited on the first blowtorch (13) deposited powder, and the 3rd blowtorch is in the second blowtorch Deposited on deposited powder, and so on.
6. the method according to claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:The vapor axial method In the innermost layer for being used for deposited powder layer be deposited on the target rod (31) of the pre- rotation mounted in axis (11) direction, the target rod (31) it is glass or ceramic material.
7. the method according to claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:Blocked up in the step c Head (33) is the column glass material that hydroxyl mass content is less than 10ppm.
8. the method according to claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:Managed in the step c The dehydration of sprills body (12) one or more mixed gas containing chlorine, helium and oxygen atmosphere in heating furnace Carry out.
9. the method according to claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:The step d is included The extension tube (32) of original deposition initiating terminal is kept, excision deposition terminates the glass containing plug (33) at end, in excision deposition knot Extension tube (32) is welded at the Shu Duan glass containing plug (33).
10. the method for preparing preformod of optical fiber with low water peak according to claim 1, it is characterised in that:The tubulose glass Glass body (19) corrosion thickness is not less than 500 μm.
11. the method according to claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:In the step d Tubular glass body (19) is cleaned using deionized water.
12. the method according to claim 1 for preparing preformod of optical fiber with low water peak, it is characterised in that:In described step e Heating furnace temperature for 1600 to 2200 degree, heating furnace translational speed be 10~80mm/min, overpressure be -100pa to+ 100pa。
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USRE50249E1 (en) 2017-03-29 2024-12-31 Prysmian S.P.A. Method and apparatus for drying and consolidating a preform for optical fibres
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