• 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:
    An improved method of producing an optical fiber with a low transmission loss for use in an optical communication system. The method comprises a chemical vapor deposition process wherein starting materials in gas phase are oxidized to form a soot on a glass substrate, and the soot which deposits on the substrate is vitrified in an atmosphere of an inert gas which is easily dissolved in the vitrified glass. A preferable soot contains silicon dioxide, a first dopant for effecting an increase of the refraction index of the silicon dioxide and a second dopant for effecting a reduction of the vitrification temperature of the soot.
    公开号:SU1194266A3
    申请号:SU772499558
    申请日:1977-07-04
    公开日:1985-11-23
    发明作者:Акамацу Такеси；Окамура Кодзи
    申请人:Фудзицу Лимитед (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to a method for producing a low loss optical fiber for use in an optical communication system.
    The aim of the invention is to improve the quality of the fiber produced by increasing the thickness of the sediment of the doped layer.
    The drawing shows a scheme for carrying out the method of chemical wasp extraction from the gas phase.
    The gas generator 1 contains the first
    raw material in the form of liquid tetrachloride silicon chloride (SiCl). In generator 1, a carrier gas is blown with argon to carry gas from the liquid. The amount of entrained gas is determined by the vapor pressure of the liquid at the temperature of the liquid and the flow rate of the carrier gas. Argon carrying the gaseous source material is piped to tubular reactor 2. The reactor is a quartz glass tube that is used as a layer of glass coating in a preformed bar stock. The preformed bar stock consists of silicon dioxide and at least one of the additives for adjusting the refractive index of silicon glass. The second raw material in the gas phase, which varies in the additive, for example germanium tetrachloride, is fed together with the first raw material in the gas phase from a separate gas generator containing the second material in the liquid phase (not shown). This is carried out by blowing a carrier gas, argon, as in generator 1. In addition, oxygen gas is supplied to gaseous reactant 2 in the reactor 2 (island. In some parts of the beam, also gaseous raw materials can be produced in the gas generator, which contains a liquid mixture raw materials, carrier gas purge.
    The reactor 2 is mounted on a machine used in the manufacture of glass products to rotate at a given speed. When the reactor is rotated, its outer surface is partially heated by the burner 3, for example, hydrogen-hydrogen, which moves axially along the tubular reactor. Thus, the local zone of heating of the reactor surface moves in a spiral along the circumference of the reactor and along its length.
    The raw materials fed to the tubular reactor interact with the oxygen supplied to form the smallest glass particles consisting of the main SiO glass material and GeOg additive when the reactor is heated in the manner described. Particles of the resulting glass are then deposited on the inner wall of the reactor. The carbon layer per unit area of the inner surface mainly depends on the total flow rate of gases passing through the reactor per unit cross section of the passage channel in the reactor, and on the total flow rate of gaseous raw materials and carrier gases per unit cross section area channel in the reactor. That is, if the flow rate increases while maintaining the flow rate at a constant value, the number of oxides formed in the form of glass also increases, and consequently, the thickness of the layer increases. If the flow rate increases with increasing oxygen supply, but while maintaining the flow rate at a constant value, the deposition zone of the resulting glass spreads forward, so that the thickness of the layer decreases. The deposited layer is heated to 1900-2000C. With a burner flame, which moves to the place where the carbon is deposited and then melts to form glass. The resulting glass layer has a reduced thickness compared with a layer of soot. The degree of heating of the moving flame depends on the pressure of the gas (oxygen — hydrogen) and the speed of movement of the flame. If the velocity of the displacement increases at a constant pressure of the gas, then the heat energy transmitted by the local, reactor zone decreases. If the gas pressure increases at a constant rate of movement, then the heat energy transmitted by the local zone of the reactor increases.
    If the heat energy reported by the local zone of the reactor is excessively high, then the glass of the reactor,
    directly exposed to the flame, is softened before the melting of the glass in the reactor is completed. This results in a deformation of the reactor and / or the ingress of gases contained in the flame into the glass of the reactor, which is undesirable for a tubular reactor which is used as a layer of glass coating on a preformed bar stock.
    If the thermal energy is only slightly higher than the required one, but sufficient to oxidize the initial ra-type materials, then complete glassing does not occur. nagara Therefore, the gas pressure of the flame and the speed of movement of the burner must be set in such a way that the thermal energy imparted to the quartz glass reactor is sufficient to effect a complete vitrification of the deposited layer, in case of complete oxidation, without any damage to the reactor.
    The proposed method consists in blowing the carrier gas through the refined materials in the liquid phase to transfer the raw materials to the gas phase, supplying the raw materials in the gas phase with the carrier gas to the tubular reactor of quartz stele, supplying oxygen as a reactant gas to the reactor, heating the reactor in the local zone, and this zone is displaced towards the output end of the reactor along the length of the reactor, due to which the raw materials in the gas phase interact with oxygen to form a deposit deposited in the form e layer on the inner surface of the reactor, and vitrification of the resulting layer of carbon by melting the carbon. An inert gas that readily dissolves in the molten glass, regardless of the carrier gas, is fed to the reactor.
    In tab. 1 summarizes the reaction conditions used in chemical vapor deposition according to known (reference examples 1 and 3) and proposed (example 2) methods. Table I
    Consumption of gaseous raw materials, SiCla
    cm / min
    The flow rate of the mixture of gaseous raw materials containing the source material and the carrier gas Ar, cm / min
    Consumption of reagent gas 0 „,
    cm / min
    Consumption of rare gas Not,
    cm / min
    Burner flame speed, cm / min
    The thickness of the glass core layer obtained with each movement of the flames, al ON
    The quality of the glass core layer
    300
    300
    200 2000
    About 5
    50
    50
    High High Low (without start-up (without (with voids) voids)) In control example 1, a tube of quartz glass 40 cm long and 20 cm in outer diameter is used as a reactor, and a glass core layer is formed on the inner surface of the reactor high quality. In example 2, a tubular reactor of the same type and size is used, and on the inner surface of the reactor by moving the flame at the same speed as in control example 1, a layer of high quality glass core is obtained. In control example 3, a tubular reactor of the same type and the same dimensions as in console 1 was used, and a layer of glass core of lower quality but of the same thickness was obtained on the inner surface of the reactor with each flame moving at a similar rate movement. In example 2, helium is injected into reactor 2 as shown in the figure by the dashed line. The reaction conditions in Reference Example 1 are such that the thick layer of the glass core is as thick as possible, provided that the resulting layer is of high quality. However, the thickness of the glass core layer produced by each movement of the flame in Control Example 1 is only 10 W m. The reaction conditions in Example 2 are such that each layer of the glass core is as thick as possible, provided that the resulting layer is of high quality. The glass core layer obtained with each flame movement is five times thicker than in the console example 1. As can be seen from a comparison of the control example 1 with example 2, the control one, example 1 provides for obtaining a high quality glass core Ton's gift that the flow rate of a mixture of gaseous raw materials containing SiCl, GeCl4 and carrier gas A and the flow rate of all gases is limited to 1100 cm / min. In this case, the deposited carbon, consisting of SiOx and GeOj oxides, has only one fifth thickness, according to Example I, therefore, each layer of the glass core has a small thickness. When implementing the control example 3, the efforts are aimed at ensuring that the deposited carbon deposits are the same thickness as the example I. In the control example 1, a mixture of raw materials in the gas phase containing SiCl4, GeCl4 and carrier gas AG is used, with the same flow rate as and in example 2, while the flow rate of all gases is maintained at 2500 cm / min in example 2. In control example 3, the glass core layer obtained by vitrifying a deposited carbon deposit has so many voids that ... the glass core is unsuitable for use in effective optical communication. The superiority of the invention over a known method becomes apparent from a comparison of control example 1 with example 2. However, to understand the features of the invention, it is reasonable to compare with control example 3. In example 2 and control example 3, the speed of movement of the flame, the thickness of the layers of carbon deposited cores are the same. However, the glass core of Example 2 does not have voids, while the glass core of Test Case 3 has many voids. Such a difference is caused by the following. In control example 3, oxygen is supplied at a flow rate of 2000 cm / min, whereas in example 2, a flow rate of 2000 cm / min consists of oxygen supplied in an amount of 500 cm / min and gels supplied in an amount of 1500. The supply of oxygen and hydrogen in an amount of 500 cm / min is stoichiometrically sufficient to interact with the mixture of raw materials in the gas phase containing a gas carrier at a flow rate of 500 cm / min. However, in the control example 3, the oxygen consumption exceeds 500 cm / min by 1500. This excess oxygen supply is used to prevent an increase in the thickness of the deposited carbon deposit. According to Example 2, instead of an abundant supply of oxygen, the supply of gels is used at the same flow rate. This means that in the case of the control example 3, the internal spaces in the deposited carbon layer are occupied with oxygen and oxidation gases such as chlorine and CO: while in example 2 such spaces are mainly occupied with helium. Helium easily spreads in the glass without any interaction with it, when the carbon is melted for vitrification, and the dissolution of the helium in the glass does not improve the optical characteristics of the glass. In this connection, it becomes clear that helium, which occupies most of the interior spaces in the deposited carbon layer, dissolves and, therefore, disappears during the glass transition of the deposited carbon. As a result, the internal spaces that would pass into the voids in the molten glass with a known method, are reduced. The reduced internal spaces of the deposited carbon layer are not filled with a small amount of non-expanding reagent gases, but are filled mainly with helium until the internal spaces are closed. Therefore, during the vitrification, the gaseous reagents are displaced from the inner space of the deposited carbon layer and, therefore, the deposited carbon layer passes into the layer of molten steel without voids. In the implementation of the proposed method, instead of gels, other rare gases can be used, which easily dissolve in the molten glass and do not interact with it, for example argon. Argon is commonly used as a carrier gas for entraining gaseous raw materials such as SiCl. and GeCl. Using argon instead of gels to form the atmosphere is incorrect. In addition, the indicated supply of gels does not seem necessary if the supply of gels is used as the supply of carrier gas. The carrier gas is consumed only in the amount necessary for the formation of gaseous starting materials before they are fed to the reactor. Therefore, to ensure that the atmosphere in the reactor, which is formed mainly by helium or argon, resulting in a decrease in the proportion of gas reactants such as oxygen or chlorine, in the inner spaces of the deposited carbon layer, it is necessary to use a separate supply of helium or argon, regardless of the supply carrier gas. In Example 4, according to the intended method, a mixture of reactant gases containing source materials with carrier gases and oxygen is introduced together with helium into a quartz glass reactor having an outer diameter of 20 mm and a length of 40 cm, the day the reaction takes place in the gas. phase and otstelovl the obtained product, as in example 2. In table. 2 shows the injected gases and their flow costs. Tab.ca2 Each source material in the gas phase is generated in a separate gas generator by blowing gas carrier Ar through a generator containing the source material in the liquid phase. After the reactor is loaded with gas, this reactor is heated with an oxygen-hydrogen burner at a burner flame speed of 5 cm / min, as in example 2. As a result, the thickness of each glass layer obtained with each flame move is about 40 / mm. Moving the flame is repeated 50 times, and then the tubular reactor with a layer of glass core in it is flattened to obtain a solid
    up to preformed bar stock. In this bar stock, a solid glass core has a diameter of 10 mm. The bar stock is heated and stretched to produce an optical fiber. The resulting fiber has a length of about 10 km, an outer diameter of 125 | am and a core diameter of 62.5 | and "1. Numerical fiber aperture is 0.20.
    The glass core of the fiber consists of about 10% GeOj, formed from SESC, about 1% PjOj, formed from RJC, and 89% Si02, formed from SiCl4. During flame movement, no deformation of the quartz glass tubular reactor occurs. In addition, there is no void in the resulting glass core. In Example 4, CeOg is the first additive that is added to SiO to increase the refractive index of SiOg, while it is the second additive that is added to SiOg to reduce the temperature of vitrification of SiOg.
    Compared with the control example 1 (Table 1), the thickness of the obtained glass core layer without voids in Example 4 is four times as large. This advantage of the invention is the result of the combined use of a second additive designed to reduce the vitrification temperature of silica and to create an atmosphere of gels in which chemical vapor deposition is carried out.
    In example 4, the vitrification temperature of the deposited carbon layer was reduced to about 1400 ° C, which enhances the effect of the gels due to the fact that the reduced flow rate of the gels (500 cm / min) and the increased flow rate of oxygen (lOO) are applied compared with example 2.
    The carbon layer of the proposed method has a significantly increased thickness, compared with the known method. Therefore, the proposed method can be applied instead of the known one, in which the process of formation of a deposit and the process of formation of glass occur with each movement of the flame. With the proposed method, in the first stage only the formation process is carried out; burning by re-moving the flame to obtain a plurality of carbon layers, and in the second stage, the carbon layer brought to a predetermined thickness, for example 1-1.5 mm, is heated so that glazing occurs. vyvyv this nagara. Thus, the production cost is reduced in comparison with the known method. The exemplary examples of the invention relate only to the method of forming a glass core layer on the inner surface of a tubular reactor, used as a glass coating after flattening. Odin; However, the invention can be used to produce a glass coating that encloses the rod of a solid glass core so as to obtain a preformed bar stock without any kind of flattening.
    权利要求:
    Claims (2)
    [1]
    1. METHOD OF OBTAINING A PREPARATION FOR EXTENSION OF AN OPTICAL FIBER by depositing a layer of doped SiOg on the inner surface of a quartz tube from the gas phase by oxidation with oxygen S2.CI4 with the addition of at least one compound from the GeCl 4 PCl 3 group using Ar as a carrier gas and subsequent heating for the vitrification of the deposited layer, characterized in that ,. in order to improve the quality of the obtained fiber by increasing the thickness of the deposited layer, vitrification is carried out while passing through the helium tube at a speed of 500-1500 cm / min
    [2]
    2. The method of pop. ^ characterized in that the deposition is carried out at the following feed rates
    reagents see / min: SiCl 4 + Ag . 300 GeCl 4 + Ag 200 0 g 500 Not1500 3. The method according to p. 1 1, about t and h and
    The fact that precipitation is carried out at the following feed rates
    reagents, cm ^ / min: SiCl ^ + Ar 300 GeCl ^ + Ar 350 PC1 + Ar thirty o z.1000 Not 500 Priority on points: 07/05/76 on pp. 1 and 2;
    11/01/76 under item 3.
    0 2
    Lg
    about.
    "P
    1 1194266 2
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    同族专利:
    公开号 | 公开日
    DE2730346A1|1978-01-12|
    FR2357496B1|1982-05-14|
    CA1107576A|1981-08-25|
    FR2357496A1|1978-02-03|
    US4149867A|1979-04-17|
    DE2730346B2|1979-07-19|
    DE2730346C3|1985-02-07|
    GB1586119A|1981-03-18|
    NL7707370A|1978-01-09|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    GB1391177A|1971-08-09|1975-04-16|Thermal Syndicate Ltd|Vitreous siliceous material|
    CA1050833A|1974-02-22|1979-03-20|John B. Macchesney|Optical fiber fabrication involving homogeneous reaction within a moving hot zone|
    US3933454A|1974-04-22|1976-01-20|Corning Glass Works|Method of making optical waveguides|US4230744A|1979-02-21|1980-10-28|Corning Glass Works|System for delivering materials to deposition site on optical waveguide blank|
    US4191545A|1979-03-02|1980-03-04|Bell Telephone Laboratories, Incorporated|Optical fiber fabrication process|
    JPS6232140B2|1983-02-18|1987-07-13|Hoya Corp|
    DE3735532A1|1987-10-21|1989-05-03|Rheydt Kabelwerk Ag|Process for the production of a preform for optical waveguides|
    JPH0478568B2|1988-06-28|1992-12-11|Sumitomo Electric Industries|
    KR100408230B1|2001-05-02|2003-12-03|엘지전선 주식회사|Method of manufacturing free form of optical fiber|
    US20040065119A1|2002-10-02|2004-04-08|Fitel U.S.A. Corporation|Apparatus and method for reducing end effect of an optical fiber preform|
    JP4552599B2|2004-10-29|2010-09-29|住友電気工業株式会社|Optical fiber preform manufacturing method|
    WO2007022641A1|2005-08-25|2007-03-01|Institut National D'optique|Flow cytometry analysis across optical fiber|
    WO2009151489A2|2008-02-25|2009-12-17|Corning Incorporated|Nanomaterial and method for generating nanomaterial|
    WO2011085465A1|2010-01-18|2011-07-21|Institut National D'optique|Flow cytometry analysis across optical fiber|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP51078866A|JPS5945613B2|1976-07-05|1976-07-05|
    JP13217076A|JPS5710051B2|1976-11-01|1976-11-01|
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