CN102320732A - Method for preparing optical fiber preform rod - Google Patents
Method for preparing optical fiber preform rod Download PDFInfo
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- CN102320732A CN102320732A CN201110245353A CN201110245353A CN102320732A CN 102320732 A CN102320732 A CN 102320732A CN 201110245353 A CN201110245353 A CN 201110245353A CN 201110245353 A CN201110245353 A CN 201110245353A CN 102320732 A CN102320732 A CN 102320732A
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- prefabricated rods
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- 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]
- C03B37/01413—Reactant delivery systems
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- 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/10—Internal structure or shape details
- C03B2203/22—Radial profile of refractive index, composition or softening point
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/10—Internal structure or shape details
- C03B2203/22—Radial profile of refractive index, composition or softening point
- C03B2203/26—Parabolic or graded index [GRIN] core profile
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
- C03B2207/32—Non-halide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The invention relates to a method for preparing optical fiber preform rod, which comprises the following steps: directly coating a uniform quartz loose body on an external surface of a core rod by using silane or siloxane as a raw material through an external vapor deposition method so as to form a loose-body preform rod, slowing heating the loose-body preform rod at a high temperature for dehydration, and sintering the loose-body preform rod to obtain a transparent optical fiber preform rod. The invention adopts clean silane or siloxane as a raw material for forming the quartz coating, does not generate a lot of harmful hydrogen chloride, overcomes the disadvantage that chlorine-containing raw material introduces single bonds which can block atomic bonds into the coating, increases the purity and strength of the preform rod material, and improves the mechanical strength of optical fibers.
Description
Technical field
The present invention relates to a kind of method for preparing preform; This method comprises uses outside vapour deposition process directly to coat quartzy uniformly loose body at the outside surface of plug with silane or siloxanes as raw material; Form loose body prefabricated rods, the slow heat of the body prefabricated rods of will loosening is again dewatered and is sintered transparent preform into.
Background technology
Over more than 30 year, optic fibre manufacture process is always in continuous development.The preform manufacturing technology is the core technology of optical fiber industry.The ME of " two-step approach " is generally adopted in the production of present commercial prefabricated rods, i.e. the first step, the manufacturing of plug; Second step, the manufacturing of outer packet portion with becomes excellent.Wherein the ME of plug typically has method gas-phase deposition in the pipe; Improve chemical vapor deposition method and plasma activated chemical vapour deposition (plasma chemical vapor deposition) plasma exciatiaon chemical Vapor deposition process like MCVD (modified chemical vapor deposition), and manage outer method gas-phase deposition such as OVD (outside vapor deposition) outside vapor deposition process and VAD (vapor axial deposition) external shaft to depositing operation.The at present typical technology of outer packet technology comprises RIT (rod in tube) and RIC (rod in cylinder) tiretube process, the direct epiboly of Soot, APVD plasma spraying process and sol-gel method.Wherein the direct epiboly of tiretube process and Soot mainly adopts the preparation of the realization clad material of similar plug outside vapor deposition process characteristics; The key distinction is relative plug ME; What tiretube process adopted is the off-line preparation method, and what the direct epiboly of Soot adopted is online preparation method.When producing plug,, not only make the also covering of essential fabrication portion of plug in order to ensure the optical quality of optical fiber.Can become a lot of little plugs to the plug drawing-down subsequently, also can not drawing-down, this depends on the size of plug.Next, additional surrounding layer (packet technology overcladding outside being commonly called as) is processed prefabricated rods on plug.Before the wire drawing, can also can not stretch the preform bar stretching diameter reduction, this depends on the size of prefabricated rods and fiber drawing furnace.The optical characteristics of preform depends primarily on the plug manufacturing technology; The cost of preform depends primarily on outer packet technology, so the plug manufacturing technology becomes the core technology that preform is made the field with outer packet technology.
The method of existing immediate preform is a tiretube process, like US005837334A, US007089765B2.Tiretube process is to produce plug earlier at present, this plug is inserted the quartz glass tube of size match again, and making plug and sleeve pipe melt the fusion prolongation synchronously through heat becomes photoconductive fiber.Tiretube process is to be used for conventional that produce and one of immediate technology of the present invention.But there is following weak point in this tiretube process: the geometric accuracy that large-sized sleeve pipe requires is high, and ME is complicated, and the material unaccounted-for (MUF) in the sleeve pipe course of processing causes cost to increase.Plug and telescopic interface have increased the complexity of drawing optical fibers technology; It is strict more that the cleaning at interface and drying become; And the interface has increased the probability that mechanical fiber optic strength weak link produces; Increased the possibility of unit length fibercuts, the interface also has a negative impact to optical fiber water peak (being called the water peak owing to hydroxyl absorption peak in 1360nm～1460nm scope in the fiber-optic transfer), avoids the additional technical process in interface to increase the production cost of prefabricated rods.
Managing the direct epiboly of outer method+Soot is to be thought to make the first-selected operational path of low-cost large scale prefabricated rod by industry at present, like US005917109A.Especially along with VAD and OVD organize the technical development of shaking depositing operation to many modulated structures more, the direct epiboly of Soot has significantly reduced the manufacturing cost of preform.Because outside vapour deposition process VAD and OVD characteristics are that sedimentation rate is high, starting material obtain easily; The direct outer packet technology of the outer method+Soot of pipe provides most commercial prefabricated rods at present, and typical two-step process route is VAD+OVD, OVD+OVD, VAD+VAD.But be the large scale prefabricated rod in the low water peak of preparation; Also there is following deficiency in the technological line of managing the direct epiboly of outer method+Soot: well-known; Manage outer method owing to have Soot preparation and vitrified separation process; Realizing that complex index of refraction section and Ge/F mix aspect such as the technology obvious deficiency of method in the pipe relatively altogether, therefore, the technology stability aspect faces huge challenge.
Another kind of and the approaching technology of the present invention is plasma activated chemical vapour deposition+APVD technology.This technology is to be the target rod with the plug that chemical vapor deposition method in managing becomes, and at it outside, adopts APVD technology that silica powder is sprayed on the quartzy target and processes the compound surrounding layer of cheapness.Synthetic quartz target rod has been guaranteed the quality of optical fiber, and outer spray technique silica powder has higher deposition efficiency, is a kind of conventional technology cheaply of producing that has been used for.But this technology has following problem; Because the silica powder that the sedimentation effect of APVD is high and employing is cheap; The purity of this silica powder and consistence are influenced by starting material and fluctuate bigger; Some impurity that wherein contains has disadvantageous effect to the wire drawing intensity of optical fiber, and this starting material can not be purified and the non-renewable popularization that has limited the large size prefabricated rod technology of its production.In addition, the large scale prefabricated rod of this technological line preparation is owing to the consistence remarkably influenced mechanical fiber optic performance of material, and typical breakpoint rate is more than the twice of the large scale prefabricated rod of Soot outsourcing prepared in the drawing process process.
The characteristics of plasma activated chemical vapour deposition technology are the very thin thickness of settled layer, can be through the accurate controls of charging, and the waveguiding structure design of optical fiber is formed and structure design reaches the unification of harmony with material.At material The Nomenclature Composition and Structure of Complexes design aspect; Introduce the design of FGM, promptly, make the footpath of plug or cross section of optic fibre upwards have successive The Nomenclature Composition and Structure of Complexes graded through setting proper formula; Therefore and make the character gradual change of material, make no tangible interface in the prefabricated rods.When making each layer viscosity coupling, thermal stresses obtains relaxing, thus in the subsequent technique that optical fiber is made, just can residual thermal stress in the optical fiber with produce scission of link, thereby reduced optical fiber decay, optimized characteristics such as PMD, warpage, welding and anti-hydrogen are aging.Plasma activated chemical vapour deposition technology sandwich layer and optics covering are all mixed GeO
2And F, utilize the two difference can be easy to realize sandwich layer and the covering coupling on viscosity to viscosity influence, thereby even plasma activated chemical vapour deposition optical fiber without D
2Handle and also have good anti-hydrogen loss performance.Plasma activated chemical vapour deposition technology is introduced F except the effect of landing low-refraction, can reduce significantly also that hydroxyl reaches the effect that reduces the water peak to the rate of diffusion in core district under the condition of high temperature.In addition, an amount of F also can effectively reduce the defective in the optical fiber.In drawing process, optical fiber is prone to form defectives such as Si, Ge, SiO and GeO, and these defectives not only can cause strong uv-absorbing, and its hangover influence is until the decay of 1550nm, and these defectives very easily combine with H simultaneously, form strong absorption peak.Fluorine can combine with these defectives, and defective is played a good healing effect, not only makes optical fiber have low decay, has also guaranteed the anti-hydrogen loss characteristic that optical fiber is good.Plasma activated chemical vapour deposition process using gas ions effect deposition silica glass, fluorine has higher deposition efficiency, and for OVD and VAD technology, the sedimentation effect of fluorine is extremely low in the deposition process, great majority are mixed F and in sintering process, are carried out (as feeding SiF
4).But receive the restriction of deposit thickness, need to adopt repeatedly deposition-agglomerating method, thereby mixing aspect the fluorine, plasma activated chemical vapour deposition technology has clear superiority.Plasma activated chemical vapour deposition with its refractive index profile control accurately advantage especially be fit to make G652D, G.657, G.655, type fiber such as DCF.
Vapour deposition process of the prior art all is with SiCl
4Be raw material, SiCl
4Vapour deposition process can produce strong corrosion property and toxic chlorine and hydrogenchloride, and purifying treatment is of a high price, and has neither part nor lot in the remaining SiCl of reaction
4Be difficult to hydrogenation and reclaim, will produce baneful influence in case get into environment, contaminated ground can become barren land.
With SiCl
4Be raw material deposition silica glass; Can in silica glass material, introduce the Si-Cl key, destroy original Si-O spacial framework, cause Si-O atom chain break; Show as the viscosity that reduced quartzy melt and the physical strength of optical fiber on the macroscopic view, make the fibercuts probability increase.Above-mentioned technological deficiency is the technical problem that those skilled in the art needs to be resolved hurrily always.
Being defined as of terms more of the present invention:
Bushing pipe: the purity quartz glass pipe for high that vapour deposition is used in the pipe, reactant are deposited on Glass tubing behind inner reaction tube inwall forms thin layer of glass.
Plug: contain sandwich layer and the solid prefab that partly deposits covering.
Silane: comprise general formula Si
nH
2n+2One type hydrogenate and this hydrogenate on Wasserstoffatoms by the substituted verivate of one or more other groups, n is the integer more than or equal to 1.
Siloxanes: be chain, ring-type or the netted macromolecular compound that contains siliconoxygen bond.
Refractive index profile: the relation curve between prefabricated rods/plug/optical fiber glass refraction and its radius.
A value: the diameter of optical fiber center core layer.
The c value: the plug conversion that is defined as method preparation in the pipe is the diameter in the optical fiber.
D value: be defined as the prefabricated rods conversion and be the diameter in the optical fiber.
Refractive index contrast Δ i%:
Relative refractive index Δ i%:
Wherein ni is the specific refractory power of i layer fiber optic materials, n
0Specific refractory power for pure silica glass.
Loose body prefabricated rods: be the loose body prefabricated rods that comprises PCVD plug and Soot outsourcing.
Summary of the invention
Technical problem to be solved by this invention is to provide to the deficiency of above-mentioned prior art existence a kind of preparation method of preform.Major advantage of the present invention is to adopt silane or the siloxanes of cleaning as forming the quartzy raw material of covering; And can not produce a large amount of deleterious hydrogenchloride; Overcome chloride raw material and in covering, introduced the single bonded shortcoming of blocking-up atomic bond, improved the consistence and the intensity of prefabricated rod cladding material.
The objective of the invention is to be realized by following method: it is to use outside vapour deposition process directly to coat quartzy uniformly loose body at the outside surface of plug with silane or siloxanes as raw material; Form loose body prefabricated rods; Calculate the quality of the surrounding layer deposition material of needs according to the waveguiding structure of plug, on this mandrel surface, deposit outsourcing layer with outside method.After perhaps earlier this plug being carried out extension elongation, remaking is that the target rod deposits outsourcing layer.The slow heat of the body prefabricated rods of will loosening again, dewatering sinters transparent preform into.
The general formula of described silane is Si
nH
2n+2, n is the integer of 1-10, can be that Wasserstoffatoms on hydrogenate or this hydrogenate is by substituted verivate of one or more other groups and cyclosilane; Siloxanes is chain, ring-type or the netted macromolecular compound that contains siliconoxygen bond.Described silane preferable methyl silane.Preferred octamethylcyclotetrasiloxane of described siloxanes or methyltrimethoxy silane.
The present invention's technical scheme preferably is: described plug is that chemical vapor deposition method is equipped with in the plasmatron; And bushing pipe is high purity, low-hydroxy-group squartz glass bushing pipe; Its relative refractive index is 0 to-0.3%; Its hydroxy radical content is generally 100ppb smaller or equal to 1000ppb, preferably less than 10ppb.The optical fiber parameter of described prefabricated rods meets the following conditions: 1.2≤c/a≤4.35, and 2.1≤d/c≤3.4.
The better technical scheme of the present invention is: the body prefabricated rods of will loosening is under 800 ℃～1200 ℃ temperature condition; Under the mixed atmosphere of oxygen, chlorine and helium, dewater; Progressively driving away organism, moisture and metallic impurity in the loose body, is being that heat sinters the transparent large prefabricated optical fiber bar of no bubble under the mixed atmosphere in oxygen, argon gas and chlorine under 1400-1600 ℃ the temperature condition then.This prefabricated rods can directly be used for wire drawing or with follow-up optical fiber preparation technologies such as preform bar stretching shapings.
The present invention's technical scheme more specifically is: will melt contract or stretch after plug be installed on the external sediment lathe around the rotation of plug axis, with unstripped gases such as silane or siloxanes and fuel gas with different pipelines towards blowtorch, it is excellent to make the flame of blowtorch spray to this target.The relative translation of paralleling to the axis takes place in plug and flame, makes the glass granules that generates in the torch flame be deposited on from level to level on the target rod, has formed the loose body prefabricated rods with enough cladding glass microparticle materials.Depositing operation need be according to dust density, and the external diameter of control dust rod makes it to satisfy how much requirements of final optical fiber.For realizing large size prefabricated rod and reduce the optical fiber manufacturing cost that preferred single rod group lamp equivalence sedimentation rate is not less than the direct outsourcing technology of 60g/min, also can adopt many rows to organize the synchronous sedimentary technology mode of lamp.Can the article on plasma body chemical vapor phase growing directly deposition or the molten plug that contracts of secondary carry out preliminary draft, when optimizing technical process, also make plasma activated chemical vapour deposition plug primary depositing joint length be able to break through 1200mm.
With respect to SiCl
4Be the vapour deposition process of raw material, the method for the invention has the sedimentation effect height, the advantage that tail gas clean environment load is little.Silane and siloxanes are purified easily, silicon content high (wherein silicomethane is up to 87.5%), and decomposition rate is fast, and decomposition temperature is lower, and rate of decomposition is high, and the sedimentation effect of outside method silane or siloxanes compares SiCl
4High by 10%～20%.SiCl
4Vapour deposition process can produce strong corrosion property and toxic chlorine and hydrogenchloride, and purifying treatment is of a high price, and has neither part nor lot in the remaining SiCl of reaction
4Be difficult to hydrogenation and reclaim, will produce baneful influence in case get into environment, contaminated ground can become barren land.And silane and siloxanes oxidation after product are nontoxic silicon-dioxide, water, carbonic acid gas etc., and environment is not had influence.
The positively effect of characteristics of the present invention and generation is:
1, use silane or siloxanes to prepare the loose body of prefabricated rods and have sedimentation effect height and the high advantage of transformation efficiency, and product is clean, non-environmental-pollution as main raw material.
2, the operational path selected for use of the present invention comprises and dewaters in the dehydration/sintering oven of the loose body of prefabricated rods and melt the process that contracts; Removed the inner fine structure defective of impurity atom and prefabricated rods; Thereby overcome chloride raw material is introduced singly-bound blocking-up silicon-oxy tetrahedron network in covering shortcoming; Improve the purity and the intensity of prefabricated rods material, can improve the physical strength of optical fiber.
3, the present invention directly deposits surrounding layer with respect to tiretube process on plug, has saved series of processes such as the necessary grinding of manufacturing sleeve pipe, polishing, stretching, has reduced manufacturing cost.Current domestic large scale prefabricated excellent sleeve pipe dependence on import, expensive not only, and also under one's control on the material specification.Plug manufacturing and outside legal system are equipped with two kinds of technologies of clad material to be combined; Combine the advantage of two kinds of technologies; The composition structure of both having optimized fibre-optical mandrel has guaranteed the optical fiber property of fiber products; Combine the cost that sedimentation effect is high, outside vapour deposition process that be convenient to maximize has reduced prefabricated rods again, met high-performance, industrialization trend cheaply.
4, the method for the invention both can obtain high-precision optical waveguide structure, had obtained high production efficiency again, was fit to make high-quality large prefabricated optical fiber bar.The prefabricated rods diameter of this method preparation reaches 200mm, but the optical fiber of continuous drawing reaches 3000 kilometers, can reduce the loss end to end of many prefabricated rods, reduces inessential productions such as technology transportation and installation man-hour, increases the continuous production time, the raising utilization rate of raw materials.
Description of drawings
Fig. 1 is the fibre profile synoptic diagram of the embodiment of the invention 1 preform and drawing thereof.
Fig. 2 is the fibre profile synoptic diagram of the embodiment of the invention 2 preforms and drawing thereof.
Fig. 3 is the fibre profile synoptic diagram of the embodiment of the invention 3 preforms and drawing thereof.
Among the figure: the part of the sedimentary corresponding fiber core of 1 expression prefabricated rods, 2 expression prefabricated rod mandrel parts, 3 represent to be deposited on outside method the silica glass member of mandrel surface, R=0 representes the part that refractive index contrast equals 0.
Embodiment
Embodiment 1:
In high purity, low-hydroxy-group squartz glass bushing pipe, deposit sandwich layer and the part inner cladding material that Ge/F mixes altogether with chemical Vapor deposition process in the plasmatron; The hydroxy radical content of bushing pipe requires smaller or equal to 1000ppb; Further require less than 100ppb, requirement further is less than 10ppb.Adopt the bushing pipe of external diameter 36mm; From the mixed airflow of one of which end feeding ratio follow procedure changes in pipe silicon tetrachloride steam, germanium tetrachloride steam and high purity oxygen gas, using the low pressure plasma initiating chamical reaction to form thousands of layer thicknesses at the bushing pipe inwall is micron-sized silica glass thin layer.Place following the melting of high temperature under 1900 ℃-2200 ℃ to shorten solid glass stick into the above-mentioned bushing pipe that contains settled layer, be plug.Settled layer has constituted core segment corresponding in the prefabricated rods and has mixed the fluorine covering, even has also constituted a part of clad section, and this plug has the necessary core/cladding structure of fiber-optic transfer.Diameter of mandrel is 28mm.The type of heating that adopts during molten contracting can be hydrogen-oxygen flame, graphite furnace, high frequency plasma torch etc.The molten back that finishes of contracting is carried out surface finish with 2100 ℃-2200 ℃ high temperature oxyhydrogen flame to the solid plug.
Again this plug is installed on the external sediment lathe as the target rod, methyl-monosilane and oxygen through different pipeline input blowtorch, and mixed firing is taken place at the nozzle place of blowtorch form silicon dioxide powder and form the loose body of prefabricated rods on attached to the target rod.The density of the loose body of this prefabricated rods is 50%～55% of silica glass density, prefabricated rods should vertically be inserted in dehydration/sintering oven by loose body aerating oxygen 1500sccm and chlorine 150sccm in the stove; Temperature rise rate with 5 ℃/min makes furnace temperature rise to 1150 ℃; And constant temperature 90min with this understanding, remove moisture and other impurity, then; To dewater/sintering oven top local heating to 1650 ℃-1700 ℃; Simultaneously around the loose body of prefabricated rods axis rotation, upwards promote prefabricated rods with the speed of 5mm/min, make the whole prefabricated rods body that loosens be sintered to the preform of homogeneous transparent.Through test, this prefabricated rods c/a=1.2 and d/c=2.1.Utilize plasma activated chemical vapour deposition technology be easy to dark doping, composite mixed, accurately control the meliority of plug refractive index profile structure, thereby preparation fluorine doping sandwich layer obtains low the decay with covering.
Embodiment 2:
Using vapour deposition process is the fluorine-doped quartz pipe inside deposition silica glass of-0.30% external diameter as 50mm in relative refractive index.Its center core layer fluorine doping specific refractory power contribution amount is-0.08%, and the sagging covering F doping specific refractory power contribution amount of method preparation is-0.15% in the pipe.For improving the plug production capacity, preferred large size bushing pipe and high rate deposition technology, plug length 1200mm.The hydroxy radical content of bushing pipe is less than 100ppb.From the mixed airflow of an end of bushing pipe silicon tetrachloride steam, germanium tetrachloride steam and the high purity oxygen gas of the variation of feeding ratio follow procedure in pipe, forming thousands of layer thicknesses at the bushing pipe inwall is micron-sized silica glass thin layer.Place following the melting of high temperature under 2000 ℃-2200 ℃ to shorten solid glass stick into the above-mentioned bushing pipe that contains settled layer, obtain the plug of diameter 46mm.Adopt the high frequency plasma torch with plug molten contract finish after, settled layer has constituted core segment corresponding in the prefabricated rods and has mixed the fluorine covering, bushing pipe has constituted a part and has mixed the fluorine clad section, this plug has the necessary core/cladding structure of fiber-optic transfer.
Again this plug is installed on the external sediment lathe as the target rod, octamethylcyclotetrasiloxane and oxygen through different pipeline input blowtorch, and mixed firing is taken place at the nozzle place of blowtorch form silicon dioxide powder and form the loose body of prefabricated rods on attached to the target rod.The density of the loose body of this prefabricated rods is 50%～55% of silica glass density, prefabricated rods should vertically be inserted in dehydration/sintering oven by loose body aerating oxygen 1500sccm and chlorine 200sccm in the stove; Temperature rise rate with 4 ℃/min makes furnace temperature rise to 1150 ℃; And constant temperature 100min with this understanding, remove moisture and other impurity, then; To dewater/sintering oven top local heating to 1650 ℃-1700 ℃; Simultaneously around the loose body of prefabricated rods axis rotation, upwards promote prefabricated rods with the speed of 5mm/min, make the whole prefabricated rods body that loosens be sintered to the preform of homogeneous transparent.Through test, this prefabricated rods c/a=4.35 and d/c=3.4.This prefabricated rods diameter reaches 200mm, but continuous drawing 3000 kilometers of optical fiber G.657 can reduce the loss end to end of many prefabricated rods, reduces inessential productions such as technology transportation and installation man-hour, increases the continuous production time, the raising utilization rate of raw materials.
Embodiment 3:
Using vapour deposition process is the fluorine-doped quartz pipe inside deposition silica glass of-0.30% external diameter as 50mm in relative refractive index.Its center core layer fluorine doping specific refractory power contribution amount is-0.10%, and the inner cladding F doping specific refractory power contribution amount of method preparation is-0.11% in the pipe.For improving the plug production capacity, preferred large size bushing pipe and high rate deposition technology, plug length 1200mm.The hydroxy radical content of bushing pipe is less than 100ppb.From the mixed airflow of an end of bushing pipe silicon tetrachloride steam, germanium tetrachloride steam and the high purity oxygen gas of the variation of feeding ratio follow procedure in pipe, forming thousands of layer thicknesses at the bushing pipe inwall is micron-sized silica glass thin layer.Place following the melting of high temperature under 2000 ℃-2200 ℃ to shorten solid glass stick into the above-mentioned bushing pipe that contains settled layer, obtain the plug of diameter 46mm.Adopt the high frequency plasma torch with plug molten contract finish after, settled layer has constituted core segment corresponding in the prefabricated rods and has mixed the fluorine covering, bushing pipe has constituted a part and has mixed the fluorine clad section, this plug has the necessary core/cladding structure of fiber-optic transfer.
Again this plug is installed on the external sediment lathe as the target rod, methyltrimethoxy silane and oxygen through different pipeline input blowtorch, and mixed firing is taken place at the nozzle place of blowtorch form silicon dioxide powder and form the loose body of prefabricated rods on attached to the target rod.The density of the loose body of this prefabricated rods is 50%～55% of silica glass density, prefabricated rods should vertically be inserted in dehydration/sintering oven by loose body aerating oxygen 1500sccm and chlorine 200sccm in the stove; Temperature rise rate with 4 ℃/min makes furnace temperature rise to 1150 ℃; And constant temperature 100min with this understanding, remove moisture and other impurity, then; To dewater/sintering oven top local heating to 1650 ℃-1700 ℃; Simultaneously around the loose body of prefabricated rods axis rotation, upwards promote prefabricated rods with the speed of 5mm/min, make the whole prefabricated rods body that loosens be sintered to the preform of homogeneous transparent.Through test, this prefabricated rods c/a=4.35 and d/c=3.4.This prefabricated rods diameter reaches 200mm, but continuous drawing 3000 kilometers of optical fiber G.652 can reduce the loss end to end of many prefabricated rods, reduces inessential productions such as technology transportation and installation man-hour, increases the continuous production time, the raising utilization rate of raw materials.
Embodiment 4:
The present invention uses outside vapour deposition process directly to coat quartzy uniformly loose body at the outside surface of plug with trimethyl silane as raw material; Form loose body prefabricated rods; Calculate the quality of the surrounding layer deposition material of needs according to the waveguiding structure of plug, on this mandrel surface, deposit outsourcing layer with outside method.After perhaps earlier this plug being carried out extension elongation, remaking is that the target rod deposits outsourcing layer.The slow heat of the body prefabricated rods of will loosening again, dewatering sinters transparent preform into.Described plug is that chemical vapor deposition method is equipped with in the plasmatron, and bushing pipe is high purity, low-hydroxy-group squartz glass bushing pipe, and its relative refractive index is-0.1%, and its hydroxy radical content is smaller or equal to being generally 100ppb.The optical fiber parameter of described prefabricated rods meets the following conditions: c/a=2.35 and d/c=2.6.
Concrete technical scheme is: will melt contract or stretch after plug be installed on the external sediment lathe around the rotation of plug axis, with unstripped gases such as silane or siloxanes and fuel gas with different pipelines towards blowtorch, it is excellent to make the flame of blowtorch spray to this target.The relative translation of paralleling to the axis takes place in plug and flame, makes the glass granules that generates in the torch flame be deposited on from level to level on the target rod, has formed the loose body prefabricated rods with enough cladding glass microparticle materials.With loose body prefabricated rods under 1000 ℃ temperature condition; Under the mixed atmosphere of oxygen, chlorine and helium, dewater; Progressively driving away organism, moisture and metallic impurity in the loose body, is being that heat sinters the transparent large prefabricated optical fiber bar of no bubble under the mixed atmosphere in oxygen, argon gas and chlorine under 1500 ℃ the temperature condition then.For realizing large size prefabricated rod and reduce the optical fiber manufacturing cost that preferred single rod group lamp equivalence sedimentation rate is not less than the direct outsourcing technology of 60g/min, also can adopt many rows to organize the synchronous sedimentary technology mode of lamp.Can the article on plasma body chemical vapor phase growing directly deposition or the molten plug that contracts of secondary carry out preliminary draft, when optimizing technical process, also make plasma activated chemical vapour deposition plug primary depositing joint length be able to break through 1200mm.
Claims (7)
1. method for preparing preform; It is to use outside vapour deposition process directly to coat quartzy uniformly loose body at the outside surface of plug with silane or siloxanes as raw material; Form loose body prefabricated rods; The slow heat of the body prefabricated rods of will loosening again, dewatering sinters transparent preform into.
2. a kind of method for preparing preform as claimed in claim 1, the general formula of described silane is Si
nH
2n+2, n is the integer of 1-10; Siloxanes is chain, ring-type or the netted macromolecular compound that contains siliconoxygen bond.
3. according to claim 1 or claim 2 a kind of method for preparing preform, wherein said silane is methyl-monosilane, dimethylsilane or trimethyl silane.
4. according to claim 1 or claim 2 a kind of method for preparing preform, wherein said siloxanes is octamethylcyclotetrasiloxane or methyltrimethoxy silane.
5. a kind of method for preparing preform as claimed in claim 1; Wherein said plug is that chemical vapor deposition method is equipped with in the plasmatron; And bushing pipe is high purity, low-hydroxy-group squartz glass bushing pipe, and its relative refractive index is 0 to-0.3%, and its hydroxy radical content is smaller or equal to 1000ppb.
6. a kind of method for preparing preform as claimed in claim 1, the optical fiber parameter of wherein said prefabricated rods meets the following conditions: 1.2≤c/a≤4.35, and 2.1≤d/c≤3.4.
7. a kind of method for preparing preform as claimed in claim 1; It is with loose body prefabricated rods under 800 ℃～1200 ℃ temperature condition; Under the mixed atmosphere of oxygen, chlorine and helium, dewater; Progressively driving away organism, moisture and metallic impurity in the loose body, is being that heat sinters the transparent large prefabricated optical fiber bar of no bubble under the mixed atmosphere in oxygen, argon gas and chlorine under 1400-1600 ℃ the temperature condition then.
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| CN201110245353A CN102320732A (en) | 2011-08-25 | 2011-08-25 | Method for preparing optical fiber preform rod |
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| CN105330140A (en) * | 2015-11-30 | 2016-02-17 | 中天科技精密材料有限公司 | Preparing method of high purity quartz sleeve for large-size optical fiber preform |
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| CN108947231A (en) * | 2018-08-27 | 2018-12-07 | 江苏亨通光导新材料有限公司 | The preparation method and device of optical fiber preform core |
| CN109987860A (en) * | 2019-04-11 | 2019-07-09 | 陈国龙 | A kind of low temperature preparation method of the compound silica fibre of Cu-30Zn-5Al base of micro- radial strain |
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| WO2020177352A1 (en) * | 2019-03-01 | 2020-09-10 | 江苏永鼎光纤科技有限公司 | Optical fiber preform based on continuous fused quartz bushing, and manufacturing method therefor |
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| CN109987860B (en) * | 2019-04-11 | 2021-10-29 | 王黎明 | Low-temperature preparation method of micro-radial strain Cu-30Zn-5 Al-based composite quartz optical fiber |
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| CN110204190B (en) * | 2019-07-12 | 2023-11-24 | 杭州金星通光纤科技有限公司 | Manufacturing method and device of ultra-low loss single mode fiber |
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