• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    THE METHOD OF MANUFACTURING THE OPTICAL FIBER PREPARATION by inserting a rod of quartz glass into a tube of quartz glass with subsequent heating of the set to the fusing temperature, which in order to improve the quality of the fiber, oxygen and the surface treatment agent are fed into the gap between the rod and the tube glass in a gaseous state, formed in the presence of an acid; 1) a substance having a boiling point and sublimation not more than the fusion temperature of the kit, and containing at least ONE element An ent from the group: boron, phosphorus, halogen, sulfur, mouse, fluorine, SP, and the hydrogen content in it does not exceed 1%.
    公开号:SU1145923A3
    申请号:SU792852304
    申请日:1979-11-26
    公开日:1985-03-15
    发明作者:Синтани Такеси；Юцуми Ацуси；Сукава Тадааки；Кобаяси Рийюдзи
    申请人:Мицубиси Метал Корпорейшн (Фирма)；Дайнити-Ниппон Кейблз,Лтд (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to methods for manufacturing precursors of optical fibers I9 silicate glass. The closest to the proposed technical essence and the achieved result is a method of manufacturing optical fiber preforms by inserting a quartz glass rod into a quartz glass tube with subsequent heating of the kit to fusion temperature 1. However, blanks produced in a known manner have voids and foreign matter. These defects, especially voids, cause optical losses due to the scattering of light in the resulting optical fiber. The aim of the invention is to improve the quality of the fiber. This goal is achieved in that according to the method of manufacturing an optical fiber preform, by introducing a quartz glass rod into a quartz glass tube, followed by heating the kit to the fusion temperature, oxygen is supplied to the gap between the rod and the tube and forming a gaseous state in the gaseous state. in the presence of oxygen, a substance having a boiling point or sublimation temperature of no more than the temperature of fusion of the complex, and containing at least one element from the group: boron, fo sor, halogen, sulfur, mouse, fluorine, and the content of hydrogen in it does not exceed 1%. In order to manufacture optical fibers with significantly reduced dispersion losses, the rods and tubes are preferably cleaned before they are treated, for example, hydrofluoric acid, followed by washing with clean water. Such processing and washing can be performed in combination with ultrasonic. The rod is inserted into the tube ii. A means is applied to treat the glass and oxygen through the gap between the rod and the tube, which is heated as an assembly, at a high temperature, resulting in surface treatment of the rod and the tube (at low temperature the surfaces will not satisfactorily processed). Surface treatment of the product at a temperature of about, presumably, oKQjjio 1; 000 С, and more preferably about 1200С. Temperature The surface treatments are expressed as the temperature of the outer surface of the tube. Processing can also be carried out at a higher temperature, provided the rod and the tube are not softened or deformed, but temperatures are preferably up to about 1900 ° C, since higher temperatures can significantly change the amount and distribution of the dopant (if there is ) in a rod or tube. A set of a rod and a tube set of a molset can be heated in any way, for example, by slowly reciprocating or re-moving a heat source, such as an oxygen-hydrogen flame, parallel to the center axis of the rod while simultaneously rotating the kit around an axis. This method of heating is especially preferable when implementing the proposed method. The heat source is preferably moved at a speed of about 10-500 mm / min, and more preferably 50-300 mm / min, while simultaneously rotating the set at a speed of about 10-100 rpm, as a result of a human tube and rod. can be completely heated to a predetermined temperature evenly around the circumference at the place where they are heated by the heat source. The means used to process the surface of the glass must satisfy the requirements of the requirements: they must not contain more than 1% hydrogen by weight, the substances formed from them in the presence of oxygen at high temperature must have a heat {) degree or sublimation not higher than the temperature required to compress the pipe. When using surface treatment agents, glass with a hydrogen content of more than 1% by weight of the OH group during processing is inserted into the opposite surfaces of the rod and tube, causing increased absorption losses and, therefore, making optical fibers with low losses difficult. The lower the hydrogen content of the agent for treating the surface of the glass, the lower the absorption loss due to the presence of OH Groups.
    Therefore, the agents used to treat the surface of the glass used according to the proposed method preferably have a hydrogen content of not more than 0.1% by weight.
    The agents for treating the surface of the glass when heated to a high temperature in the presence of oxygen should not form a substance with a boiling point or sublimation higher than the temperature necessary to compress the tube, because otherwise the product and / tube that has settled on opposite surfaces of the rod and / tube at the interface between them after squeezing the tube and increasing the number of defects and spots with a 1-normal refractive index at the interface, increased scattering losses cause. Thus, the product should be almost completely evaporated, at least until the tube is compressed by applying heat.
    The temperature required to press the tube is the temperature at which the tube is compressed to ensure thermal coupling between the rod and the tube with each other (approximately 1900-2300 ° C for a syringe glass).
    For complete evaporation of the product, such agents are used to treat the surface of the glass, which give a product having a boiling or sublimation point lower than the compression temperature, for example, at least. Studies have shown. that the absence of defects at the interface between the rod and the tube after processing their surfaces by the proposed method is due to the following reasons. . By passing the surface treatment agent of the glass in the form of gas and oxygen through the gap between the rod and the tube, heated at high temperature, the substance that just formed in the presence of oxygen at-high temperature is uniformly embedded in the opposite surface layers of the rod and tube due to diffusion, dissolution, chemical reaction with glass, etc.,. as a result, the thin surface layer of the rod and the tube is modified into a layer of glass containing this substance (product). Consequently,
    the modified surface layers of the rod and tube acquire a close chemical affinity with each other or reduced viscosity, and when the tube is compressed after surface treatment, a satisfactory interface is free of defects such as voids causing scattering losses.
    In addition, some surface treatment agents oppositely clean the surface layers of the rod and tube in accordance with a different mechanism of action.
    In the case of a mechanism of action, a DiecTBO action, formed from an agent for surface treatment in the heated area of the kit, heated by a moving heat source, does not deposit on the heated area, but passes further to the low-temperature section, where it is deposited on the surfaces of the rod and tube. In this case, the nocropine substance, if any, on the surface, is precipitated. By moving a heat source to a low-temperature area, the product on the surface evaporates under the influence of high temperature, as a result of which the foreign substance also separates from the surface under the influence of pressure when the product evaporates and is carried away along with the steam downwards in the direction of the propelled engine. so that the agents used to treat the surface of the glass have this pressure. Together with the movement of the heat source, this phenomenon is repeated and the extraneous material gradually moves in the direction of downward movement, as a result of which it ultimately leaves the surfaces of the rod and tube. . Some other types of surface treatment agents clean the opposite surface layers of the rod and tube, providing a herbal effect on them, resulting in clean surface layers that acquire chemical affinity with each other due to the incorporation of substances. Since the surface treatment is carried out in accordance with the inventive method by passing a gaseous agent for treating the surface of the glass in combination with oxygen, in which they can flow in the form of gas, i.e. blend at surface treatment temperature with oxygen. In addition, if the treatment agents can be transported in a mixture with oxygen at low temperatures, the gas mixture pipeline can be easily insulated to prevent fogging. From this point of view, it is preferable to use surface treatment agents that have sufficient vapor pressure at low temperatures. .a, and more specifically, at least 10 mm Hg. at. Since the substance formed from the surface treatment agent is incorporated into the core and the tube during surface treatment in accordance with the inventive method, it is undesirable that the surface treatment agent contain an element that exhibits a characteristic absorption property at a wavelength (or close to thereto) of light to be transmitted through the resulting optical fiber. If the agents used to process the surface of the glass satisfy the above requirements, toso their elemental composition and chemical structure are not particularly limited. It is preferable to use such glass surface treatment agents that provide products that are capable of stably located in glass and glass rods, such as glass-modifying oxides. Which do not have the ability to glass formation, but can stably stay in the glass frame, where they are introduced to modify the characteristics of the glass. Specific examples of agents for glass surface treatment. are BFj, BCt ,, BBr, BJj, BHF, BHClj, B (CH} 0), and similar boron compounds, PCti, PBHg, PJi, PFj, PCfj, PBrj, PJj,. PFjj-, Pcfs, PBrj, PJs and similar phosphorus halide compounds P0c and | sub-humid phosphorus oxide chlorine; ) (PNGfj) ,, (PNGfj) s ;,, (PNCli) “, (PNei,), -. -. and the like fosfonitrnlhloridy AsF, AsClj, AsBrj, AsFj and similar halides arsenic SbiFj SbCf SbBrj, SbPjr, SbGl h halide such nye soednieki SjFjt antimony,, SjBrz, SFa, iSeii, 3F,, SFe and. similar to sulfur halide compounds SQji and similar sulfur compounds, SOFj,, SOCI (i, SOBra, SOaFg, SOiCtij 80g (OH) P, SzOfCTf, 50g (OH) C1, SO (OH) F and similar oxyhalide compounds, SeFi ", SeFff , SeCfj, SeCt,, SejEr, SeBr., And similar halide compounds of selenium, CClzFz, CGljF, CClFj, and similar carbon chlorofluoride compounds. SG (, CC11 (, SBGl, and similar carbon tetrahalide compounds; ctiOr .Ccs); oxygen compounds J GIF, GIF,., BrF, BrFii and similar halogen compounds j, Fj, Brj and similar halogens, etc. These compounds can be used alone or as a mixture, at least two of them. Substances having a hydrogen content higher than 1% by weight should be mixed with other substances.However, the hydrogen content in the mixture should not exceed 1% by weight.It is preferable to use bC1 as a means for surface treatment of glass, BFj, VVgz, PF3, POCtz, CcSiF}, CGiFf, F, SFj, etc. The agent for treating the surface of the glass is supplied as a gas to the gap between the rod and the tube mixed with oxygen in a ratio of preferably 0.1- 200 hours (here and below by volume) more preferably 0.5-100 hours. Particularly preferably 1- 50 hours of treatment for 100 hours of oxygen. Satisfactory results can be obtained by processing thin surface layers of the rod and tube. The time required for surface treatment varies depending on the total pressure and flow rate of the gas mixture of the processing agent with oxygen, the concentration of the treatment agent in the mixture, etc., and the total pressure and flow rate and total concentration of the mixture Theme.The shorter the processing time. When using a gas mixture containing “colo 0.1–1000 hours of treating agent per 100 hours of oxygen, at a total pressure of about 100–5000 mm Hg. and approximately 20–5000 ml / min in combination with a moving heat source, the heat source is repositioned or reciprocally required a number of times (usually 1–100 times) 7 11 at a speed in the previously mentioned limits. When using other heating means, such as a fixed type, such as an electric furnace, in which the assembled set is heated completely, the surfaces are treated for a time equivalent to the total time, during which the assembled set is heated by the above-mentioned moving source heat at a temperature sufficient to treat surfaces. In the implementation of the proposed method, it is preferable to use a gas mixture containing about 0.5-200 hours, and more preferably about 0.5-100 parts of the activating agent per 100 hours, oxygen, at a total pressure of about 500-1000 mm Hg and about 50-2000 ml / min in combination with a mobile heat source, the heat source being moved at a speed in the wound range of 1–20 times. The rod and tube with the treated surfaces are then connected to each other in the usual way, for example , scoop up the tube at about 1900-2300 o odorodnym flame or similar sources of heat while rotating ;; rod and tubes located concentrically relative to each other in order to compress the tube, apply heat and flame to it, and ensure thermal adhesion of the tube to the rod. Thus, a preform can be made to produce an optical fiber. From the blanks made by the proposed Method, optical fibers can be obtained in the usual way, for example, by pulling the blanks at a speed of about 10,100 m / min to an outer diameter of about 100-200 microns while simultaneously heating for: cooking in an electrical circuit. The rod and tube subjected to surface treatment in accordance with the proposed method can be satisfactorily connected to one another, as a result of which an optical blank is obtained that has significantly fewer defects on the interface than the blank obtained by the lime method. Example 1. A 80 cm long tube with an inner diameter of 15.4 mm is prepared, consisting of a silicate glass support tube with Pr 1.4585, having an outer diameter of 20 mm and a thickness of 1.5 mm. The cladding layer with a thickness of 0.8 mm is formed on the inner surface of the carrier tube and consists of silicate glass with front ° 1,4485 doped with boron and fluorine. The tube is used immediately after preparation. A rod with an outer diameter of 8 mm, made of high-purity silicate glass (1.4585), was washed over the surface with 30% (by weight) hydrofluoric acid, then thoroughly washed in clean water using ultrasound and inserted concentrically into the tube. A mixture of oxygen with gas ZS12upri Og / BC e 800/20 (here and below is a volume ratio) and a total pressure of 760 mm Hg are continuously fed into the gap between the core and the tube with a flow rate of 800 ml / min. at room temperature with simultaneous rotation of the rod and tube around the central axis at a speed of 60 rpm. At the same time, in order to heat the assembled set in order to treat surfaces parallel to the tube, the oxygen-hydrogen flame is moved back and forth 10 times at a speed of 100 mm / min. The outer surface of the tube at the site where it is heated by a flame has a temperature of about 1500 ° C, which is measured with an infrared thermometer. - tt With continuous simultaneous rotation of the rod and tube around the axis at a speed of 60 rpm after surface treatment, the tube is heated with an oxygen-hydrogen flame to, which ensures its compression, resulting in an intermediate billet with an outer diameter of 17 mm. To adjust the outer diameter, a tube of silicate glass with a diameter of 25 mm and a thickness of 1.5 mm is cut into the intermediate billet, after which the tube is compressed as described above and an optical fiber preform is obtained having an outer diameter of 2 O, 5 mm. The billet is then fused with an oxygen-hydrogen flame to a corrected and external diameter of 20 mm. 9 . 1145 After that, the billet is pulled at a speed of 30 m / min. S / while heating it while in a resistance furnace, as a result an optical fiber with a core diameter of 60 µm, a cladding layer thickness of 15 µm and an outer diameter of 150 µm is formed. The fiber is pre-coated with urethane resin, and then over the pre-layer is coated with a protective layer of nylon. In this way, the outer diameter of the optical fiber is adjusted to 0.9 mm. The resulting optical fiber has a very low loss (tcM table). The scattering losses are determined from the characteristic loss curve in accordance with the X display method, in which the value inverse of the fourth power of the wavelength L is laid on the abscissa axis, and the total loss (dB / km) in the fiber is on the ordinate axis, and As a scattering loss, the total loss (dB / km) at an infinitely long wavelength, which is determined by extrapolating the linear portion of the curve in the wavelength range from 0.650, 85 microns to an infinitely long wavelength. Such a loss value does not depend on the wavelength, and it is usually taken: as an indicator of scattering loss. Examples 2-8 and comparative examples 1-3. The operations for the manufacture of blanks and optical fibers as described in example 1 are repeated, however, the means for processing the surface of the glass are mixed with oxygen in other ratios (see table) and, moreover, in the comparative example they do not treat the surfaces. Rods and carrier tubes, having a cladding layer, are anapogic in size and refractive index used in example 1. 3 of comparative example 2, the substance formed during surface treatment remains at the interface between the rod and the tube (does not evaporate when the tube is compressed). The loss characteristics of the manufactured optical cyclocons are given in the table. Examples 9-14 and Wed 4-4. The steps for manufacturing blanks and optical fibers described in Example 1 are repeated, however, the cladding layer is made of boron-doped silicate glass c, 4510, and the means for processing the surface of the glass are mixed with oxygen in other ratios (see table). In comparative example 5, as in comparative example 2, the substance formed during the surface treatment remains at the interface between the rod and the tube. In addition, in Comparative Example 6, there is an unsatisfactory thermal adhesion of the tube to the rod during compression due to the deposition of SnOg. The loss characteristics of fabricated optical fibers are given in table. As can be seen from the table, optical fibers made according to examples 114 have lower scattering losses than optical fibers produced by comparative examples 1-6, i.e. When using the proposed method, a satisfactory connection of the rod and the tube is achieved.
    Oj / BCf 3 800/20 Oi / BFj 800/20 Oj / BFj 80U / 200 Oa / VVgz 800/50
    0.4 0.6 0.5 0.7
    Table continuation
    权利要求:
    Claims (1)
    [1]
    METHOD FOR MANUFACTURING AN OPTICAL FIBER PREPARATION by introducing a quartz glass rod into a quartz glass tube and then heating the kit to a fusion temperature, characterized in that, in order to improve the quality of the fiber, oxygen and an agent for processing the glass surface are fed into the gap between the rod and the tube gaseous state, forming in the presence of oxygen a substance having a boiling or sublimation temperature no higher than the fusion temperature of the kit and containing at least one element from nN: boron, phosphorus, a halogen, sulfur, arsenic, fluorine, and hydrogen content of not more than 1%.
    1145923 2
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    同族专利:
    公开号 | 公开日
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    CA1131029A|1982-09-07|
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    DE2947074C2|1990-02-01|
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    DE2947074A1|1980-07-17|
    AU5323479A|1980-07-03|
    SE7909684L|1980-06-30|
    US4264347A|1981-04-28|
    FR2445301B1|1985-07-12|
    IT7927477D0|1979-11-22|
    GB2038311A|1980-07-23|
    IT1126375B|1986-05-21|
    NL182308C|1988-02-16|
    SE438311B|1985-04-15|
    NL182308B|1987-09-16|
    BR7907675A|1980-09-09|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP53165302A|JPS5924092B2|1978-12-29|1978-12-29|
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