WO2017181649A1 - 光纤预制棒的制造装置及其制造方法 - Google Patents

光纤预制棒的制造装置及其制造方法 Download PDF

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WO2017181649A1
WO2017181649A1 PCT/CN2016/104312 CN2016104312W WO2017181649A1 WO 2017181649 A1 WO2017181649 A1 WO 2017181649A1 CN 2016104312 W CN2016104312 W CN 2016104312W WO 2017181649 A1 WO2017181649 A1 WO 2017181649A1
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pressure
sio
preset
optical fiber
fiber preform
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PCT/CN2016/104312
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English (en)
French (fr)
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赵奉阔
田国才
屠建宾
钮晓平
钱亮
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江苏亨通光导新材料有限公司
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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]
    • C03B37/018—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] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • 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]
    • C03B37/018—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] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • C03B37/01853—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering

Definitions

  • the invention belongs to the field of optical communication technology, and in particular relates to a device for manufacturing an optical fiber preform and a manufacturing method thereof.
  • organic raw materials siloxanes
  • carbon-containing gases CH4, CF4, Freon, etc.
  • the carbon remaining in the preform of the optical fiber preform When the carbon remaining in the preform of the optical fiber preform is sintered at a high temperature, it reacts with SiO 2 (silica) to break the silicon-oxygen bond (Si-O) in the vitreous; the CO/CO2 formed by the reaction is easily formed in the vitreous body. bubble. Silicon-oxygen bond (Si-O) cleavage bonds and bubbles in the vitreous will directly affect the strength of the fiber and the attenuation of the optical signal.
  • SiO 2 silicon-oxygen bond
  • the deposition process of optical fiber preform manufacturing should be carried out in the presence of excess oxygen.
  • the sintering of large-sized optical fiber preforms is generally carried out by vacuum sintering. If an oxidizing gas (such as Cl 2 and O 2 ) is introduced into the sintering furnace during sintering, the interior of the sintering equipment will be oxidized and corroded. This not only reduces the service life of the equipment but also causes contamination of the optical fiber preform during the sintering process.
  • an oxidizing gas such as Cl 2 and O 2
  • Chinese patent CN103771697A discloses that a stoichiometric oxygen can result in a lower deposition rate than excess oxygen during the deposition process.
  • Cl 2 is used for dehydration.
  • a good way of dehydration As the density of the bulk of the optical fiber preform increases, it is difficult for the gas molecules outside the loose body to enter the loose body, and the dehydration effect will also decrease. At the same time, the gas molecules inside the loose body are difficult to be discharged, and it is easy to remain inside the optical fiber preform. The formation of bubbles affects the quality of the optical fiber preform.
  • the invention provides an apparatus for manufacturing an optical fiber preform, comprising: an oxidative dehydration sintering furnace, a central tube located in the sintering furnace, at least one heating element located in the sintering furnace and located outside the central tube, and located in the central tube a SiO 2 body, a sealing cover for sealing the center tube, a cavity in the center tube called an inner cavity, located outside the center tube, and located in the sintering furnace, called an outer cavity, connected to the outer cavity a vacuum exhaust pipe and a first gas pipe, a second vacuum exhaust pipe connected to the sintering furnace, and a second gas pipe, wherein the heat generating body, the SiO 2 body, and the sealing cover are both located in the sintering furnace.
  • the invention further provides a method for manufacturing an optical fiber preform, comprising the steps of:
  • the first step vacuum processing the SiO 2 body located in the central tube;
  • the second step in a vacuum state, He gas is introduced into the outer cavity, O 2 gas, Cl 2 gas, and He gas are introduced into the inner cavity to fully adsorb the SiO 2 body;
  • the third step heating the heater to heat the temperature of the SiO 2 body to a first preset temperature, and the C in the SiO 2 body is fully reacted with O 2 ;
  • the fourth step continuing to heat the heater so that the temperature of the SiO 2 body is heated to a second preset temperature, and the OH in the SiO 2 body is sufficiently reacted with Cl 2 ;
  • the fifth step stopping the heater heating, vacuum processing the SiO 2 body
  • Step 6 continue to heat the heater so that the temperature of the SiO 2 body is heated to a third preset temperature, and the SiO 2 body is vitrified to obtain a low C, low OH optical fiber preform.
  • Step F4 to be increased when the pressure to the interior cavity of 101 kPa, after the SiO 2 glass body is removed, to obtain a low C, low OH optical fiber preform.
  • the method of the invention solves the problems of carbon removal and dehydration by the methods of deoxidation and removal of SiO2 and the oxidative dehydration sintering furnace to obtain low C and low OH optical fiber preforms; the invention has simple and reliable structure.
  • FIG. 1 is a schematic structural view of an apparatus for manufacturing an optical fiber preform according to the present invention
  • FIG. 2 is a schematic flow chart showing a method of manufacturing an optical fiber preform of the present invention.
  • the apparatus for manufacturing an optical fiber preform body includes an oxidative dehydration sintering furnace 11 and a center made of transparent quartz glass in the oxidative dehydration sintering furnace 11.
  • a tube 12 a heating element 5 located on both sides of the central tube 12, an SiO2 body (silica body) 10 in the center tube 12, a sealing cover 14 for sealing the center tube 12, and a central tube 12 is referred to as an inner cavity 12, located outside the central tube 12 and located in the sintering furnace 11, referred to as an outer cavity 15, a first vacuum exhaust pipe 2 connected to the outer cavity 15, and a first gas pipe 9, connected a first vacuum pump 1 on the first vacuum exhaust pipe 2 and outside the outer cavity 15, a first pressure sensor 8 connected to the first gas pipe 9 and located outside the outer cavity 15, and connected to the sintering furnace a second vacuum exhaust pipe 7 and a second air pipe 4, a second vacuum pump 6 connected to the second vacuum exhaust pipe 7 and located outside the outer cavity 15, and connected to the second air pipe 4 and located A second pressure sensor 3 outside the outer chamber 15.
  • the heating element 5, the SiO2 body (silica body) 10, and the sealing cover 14 are all located in the sintering furnace 11.
  • the central tube 12 can isolate the corrosive oxidizing gas from the graphite member, the metal, and the like which are easily oxidized in the oxidative dehydration sintering furnace 11; the heating element 5 is used to heat the inner cavity 13 of the oxidative dehydration sintering furnace 11;
  • the first vacuum exhaust pipe 2 is used for vacuum evacuation of the outer cavity 15, the first vacuum pump 1 is used for vacuuming the outer cavity 15, and the second vacuum exhaust pipe 7 is used for vacuum evacuation of the inner cavity 13, the second vacuum pump 6 is used for evacuating the inner cavity 13;
  • the first air pipe 9 is for supplying air into the outer cavity 15, the first pressure sensor 8 is used for pressure monitoring of the outer cavity 15, and the second air pipe 4 is used for the inner cavity 13
  • the inner pressure is supplied, and the second pressure sensor 3 is used for pressure monitoring of the inner chamber 13.
  • the first pressure sensor 8 for monitoring the pressure of the outer cavity 15 and the second pressure sensor 3 for monitoring the pressure of the inner cavity 13 are used to monitor the pressure difference between the inside and the outside of the central tube 12 to This controls the evacuation speed of the first vacuum pump 1 for evacuating the outer chamber 15 and the second vacuum pump 6 for evacuating the inner chamber 13; controlling the first air tube 9 for venting the outer chamber 15 And the flow rate of the gas in the second air pipe 4 for ventilating the inner cavity 13 to control the pressure in the central pipe 12 to always be lower than the pressure outside the central pipe 12, and the pressure outside the central pipe 12 and the inner pipe 12
  • the pressure difference is 0-350pa, preferably 50-100pa, to avoid overflow of Cl 2 and O 2 from the sintering furnace 11, thereby avoiding oxidative corrosion of graphite parts and metals by oxidative corrosive gases such as Cl 2 , HCl and O 2 .
  • the method for manufacturing an optical fiber preform of the present invention has the following steps:
  • the first pressure sensor 8 and the second pressure sensor 3 are monitored, and the pressure difference between the inside and the outside of the center tube 12 is monitored to obtain the evacuation speeds of the first vacuum pump 1 and the second vacuum pump 6.
  • the flow rate of the gas passing through the first gas pipe 9 to the outer cavity 15 is controlled, and the flow rate of the gas from the second gas pipe 4 to the inner cavity 13 is controlled to keep the pressure in the central pipe 12 always lower than the pressure outside the central pipe 12.
  • the manufacturing method of the optical fiber preform of the present invention comprises the following steps:
  • First step Vacuum treatment of the SiO 2 body 10 located in the central tube 12: Specifically, the gas in the SiO 2 body 10 is evacuated.
  • the second step in the vacuum state, He gas is introduced into the outer cavity 15, and O 2 gas, Cl 2 gas, and He gas are introduced into the inner cavity 13, so that the SiO 2 body 10 is sufficiently adsorbed.
  • the third step heating the heater 5 such that the temperature of the SiO 2 body 10 is heated to a first predetermined temperature, and C in the SiO 2 body 10 is sufficiently reacted with O 2 .
  • the fourth step heating the heater 5 is continued to heat the temperature of the SiO 2 body 10 to a second predetermined temperature, and the OH in the SiO 2 body 10 is sufficiently reacted with Cl 2 .
  • the fifth step the heating of the heater is stopped, the SiO 2 body 10 is vacuum-treated, and the gas in the SiO 2 body 10 is discharged through the second gas pipe 4.
  • Step 6 Continue to heat the heater 5 so that the temperature of the SiO 2 body 10 is heated to a third predetermined temperature, and the SiO 2 body is vitrified to obtain a transparent low C, low OH optical fiber preform.
  • the first preset temperature is 800 ° C; the second preset temperature is 1200 ° C; and the third preset temperature is 1500 ° C.
  • the manufacturing method of the optical fiber preform of the present invention is compared with the manufacturing method of the existing optical fiber preform, and the added technical solution includes: the second step: respectively, the He gas is introduced into the outer cavity, and the O2 is introduced into the inner cavity 13 , Cl2, and He gas; the third step described above: sufficient reaction of OH and Cl2 in the SiO2 body.
  • a low C, low OH optical fiber preform is produced by the manufacturing method of the inventive optical fiber preform.
  • the method for producing the SiO 2 body 10 of the present invention has the following three embodiments:
  • a SiO 2 body 10 having a density of 0.4 to 0.8 g/cm 3 was obtained by a deposition method using CH 4 and O 2 as reaction gases and SiCl 4 as a raw material.
  • a SiO 2 body 10 having a density of 0.4 to 0.8 g/cm 3 was obtained by a deposition method using H 2 and O 2 as reaction gases and OMCTS as a raw material.
  • a SiO2 body 10 having a density of 0.4 to 0.8 g/cm 3 was obtained by a deposition method using CH4 and O2 as reaction gases and OMCTS as a raw material.
  • the SiO2 body 10 obtained by the above three deposition methods is placed in the oxidative dehydration sintering furnace 11 of the present invention, and is covered with a sealing cover 14, and the manufacturing method of the optical fiber preform of the present invention also has three embodiments.
  • a first embodiment of the method for producing an optical fiber preform of the present invention the SiO 2 body 10 is produced by the manufacturing method of the first embodiment of the SiO2 body 10, and the first and third steps of the method for manufacturing the optical fiber preform of the present invention are The specific content of the sixth step is as follows:
  • Step A1 The SiO2 body 10 is placed in the sintering furnace 11 and covered with a sealing cover 14.
  • Step A2 synchronously reducing the pressure of the inner cavity 13 and the outer cavity 15, so that the inner cavity 13 and the outer cavity 15 are in a vacuum state, that is, the pressure outside the central tube 12 and the pressure in the central tube 12 are both 5 pa.
  • 5pa is an absolute pressure, converted to a degree of vacuum, 5pa is less than 0.1MPa, which is equivalent to an absolute pressure of 0), and maintains the first preset time.
  • the first preset time is 30 min.
  • Step B1 In the vacuum state, the first gas pipe 9 is supplied with He gas to the outer cavity 15, and the second gas pipe 4 is supplied with 3 slm of O 2 gas, 2 slm of Cl 2 gas, and 3 slm of He to the inner cavity 13 .
  • the gas causes the SiO 2 body 10 to be sufficiently adsorbed.
  • Step B2 The first pressure sensor 8 monitors the pressure in the outer chamber 15 outside the center tube 12, while the second pressure sensor 3 monitors the pressure in the inner chamber 12 in the center tube 12, always maintaining the pressure of the outer chamber 15. The pressure difference from the pressure of the inner chamber 13 is greater than the first predetermined pressure.
  • the first preset pressure is 5-250 pa.
  • Step B3 When the pressure of the inner cavity 13 reaches the first preset pressure value, the ventilation to the inner cavity 13 and the outer cavity 15 is stopped, and the second predetermined time is maintained to sufficiently adsorb the SiO 2 body 10.
  • the first preset pressure value is 10 4 pa; the second preset time is 90 min.
  • the specific content of the third step is: heating the heater 5, heating the temperature of the SiO2 blank 10 to a first preset temperature at a first preset heating rate, and maintaining the third predetermined time to make the SiO 2 blank 10
  • the inside C is fully reacted with O 2 .
  • the first preset heating rate is 3.5 ° C / min; the first preset temperature is 800 ° C; the third preset time is 120 min.
  • the specific content of the above fourth step is: continue to heat the heater 5, and heat the temperature of the SiO 2 body 10 to a second preset temperature at a second preset heating rate to make OH and Cl 2 in the SiO 2 body 10. Full response.
  • the second preset heating rate is 10 ° C / min; the second preset temperature is 1200 ° C.
  • Step E1 synchronously starting the first vacuum pump 1 and the second vacuum pump 6, so that the pressure of the outer cavity 15 outside the central tube 12 is greater than the pressure of the inner cavity 13 in the central tube 12, and the pressure of the outer cavity 15 is always maintained.
  • the pressure difference of the pressure of the inner cavity 13 is greater than the second preset pressure.
  • the second preset pressure is 50-100 pa.
  • Step E2 synchronously reducing the pressure of the inner cavity 13 and the outer cavity 15, so that the inner cavity 13 and the outer cavity 15 are in a vacuum state, that is, the pressure outside the central tube 12 and the pressure in the central tube 12 are both 5 pa.
  • 5pa is an absolute pressure, converted to a vacuum, 5pa is less than 0.1MPa, which is equivalent to an absolute pressure of 0), and maintains a third preset time.
  • the third preset time is 120 min.
  • Step F1 heating the heater 5 is continued, and the temperature of the SiO 2 body 10 is heated to a third preset temperature at a third predetermined heating rate for a fourth predetermined time to sufficiently vitrify the SiO 2 body 10.
  • the third preset temperature is 1500 ° C; the third preset heating speed is 5 ° C / min; the fourth preset time is 20 min.
  • Step F2 The SiO 2 blank 10 is lowered to a fourth preset temperature at a fourth preset temperature drop rate.
  • the fourth preset cooling rate is 5 ° C / min; the fourth preset temperature is 400 ° C.
  • Step F3 the first air pipe 9 opens into the outer cavity 15 with N 2 , and the second air pipe 4 opens into the inner cavity 13 to pass N 2 , so that the pressure in the central pipe 12 is always lower than that outside the central pipe 12 .
  • the pressure, and the pressure difference between the pressure outside the center tube 12 and the pressure in the center tube 12 is within a third preset pressure.
  • the third preset pressure is 250 pa.
  • Step F4 When the pressure in the inner cavity 13 was increased to 101 kPa, the vitrified SiO 2 body 10 was removed to obtain an optical fiber preform having an OH content of 0.6 ppm and a C content of 5 ppm.
  • a second embodiment of the manufacturing method of the optical fiber preform of the present invention the SiO2 blank 10 is produced by the manufacturing method of the second embodiment of the SiO2 blank 10, and the second embodiment of the manufacturing method of the optical fiber preform of the present invention and the first
  • the differences between the embodiments are as follows:
  • Step B2 The first pressure sensor 8 monitors the pressure in the outer chamber 15 outside the center tube 12, while the second pressure sensor 3 monitors the pressure in the inner chamber 12 in the center tube 12, always maintaining the pressure of the outer chamber 15.
  • the pressure difference from the pressure of the inner chamber 13 is greater than the second predetermined pressure. That is, the pressure difference between the pressure of the outer cavity 15 and the pressure of the inner cavity 13 is different.
  • the second preset pressure is 50-100 pa.
  • Step F4 When the pressure in the inner cavity 13 was increased to 101 kPa, the vitrified SiO2 body 10 was removed to obtain an optical fiber preform having an OH content of 1 ppm and a C content of 3 ppm. That is, the OH content and the C content of the optical fiber preform are different.
  • the third embodiment of a method of manufacturing an optical fiber preform according to the present invention is made of SiO2 SiO 2 green body blank 10, the third embodiment of the present invention is a method for producing an optical fiber preform and the first
  • the difference between an embodiment is as follows:
  • Step F4 When the pressure in the inner cavity 13 is increased to the fourth predetermined pressure, the vitrified SiO 2 body 10 is removed to obtain an optical fiber preform having an OH content of 0.7 ppm and a C content of 8 ppm. That is, the content of OH and the content of C in the optical fiber preform are different.
  • the fourth preset pressure is 101 kPa.
  • the optical fiber preform of the third embodiment was used to obtain an optical fiber preform having an OH content of 169 ppm (high content) and a C content of 261 ppm (high content).
  • the method of the invention solves the problems of carbon removal and dehydration by the methods of deoxidation and removal of SiO2 and the oxidative dehydration sintering furnace to obtain low C and low OH optical fiber preforms; the invention has simple and reliable structure.

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Abstract

一种光纤预制棒的制造装置及其制造方法，其制造装置包括：氧化脱水烧结炉（11）、位于该烧结炉（11）内的中心管（12）、位于该烧结炉（11）内且位于该中心管（12）外的至少一发热体（5）、位于该中心管内的SiO2坯体（10）、用于密封该中心管（12）的密封罩（14）、位于该中心管（12）内称为内腔体（12）、位于该中心管（12）外且位于烧结炉内称为外腔体（15）、连接至该外腔体（15）的第一真空排气管（2）和第一气管（9）、连接至该烧结炉的第二真空排气管（7）和第二气管（4），其中，所述发热体、SiO2坯体、以及密封罩均位于所述烧结炉内。

Description

光纤预制棒的制造装置及其制造方法 技术领域
本发明属于光通信技术，尤其涉及一种光纤预制棒的制造装置及其制造方法。
背景技术
在光纤预制棒的制造工艺过程中，经常使用有机原料(硅氧烷类)或者含碳气体(CH4、CF4、氟利昂等)反应制得光纤预制棒坯体，含碳原料或含碳的气体分子量越大越不容易充分燃烧，因此燃烧不尽的碳容易残留在光纤预制棒坯体中。
光纤预制棒坯体中残留的碳在高温烧结时，与SiO2(二氧化硅)反应，使得玻璃体内的硅氧键(Si-O)发生断裂；反应生成的CO/CO2容易在玻璃体内形成气泡。硅氧键(Si-O)断裂键及玻璃体内的气泡将直接影响光纤的强度和光信号的衰减。
为了避免上述存在的问题，光纤预制棒制造的沉积工艺应当在过量氧存在下进行。
大尺寸光纤预制棒的烧结一般采用真空烧结的方法，烧结过程中如果向烧结炉内通入氧化性气体(比如Cl2和O2)，烧结设备内部将会因此而氧化腐蚀。这样不仅降低了设备的使用寿命而且烧结过程中也会造成光纤预制棒的污染。
中国专利CN1076430A和CN1213650A均揭示在真空烧结装置，其加热和保温件均使用石墨材料，无法使用O2对SiO2坯体进行除碳处理；同时，Cl2以及Cl2与OH反应生成的HCl也会加速石墨和金属材料的腐蚀降低设备的使用寿命。
中国专利CN103771697A揭示一种化学计量的氧相比在沉积工艺过程中过量的氧会导致较低的沉积速率，本专利采用的一种常压烧结的方式中使用Cl2进行脱水不失，为一种较好的脱水方式。但是随着光纤预制棒松散体的密度的提高，松散体外部的气体分子难以进入松散体内部，脱水的效果也将下降；同时，松散体内部的气体分子难以排出，容易留在光纤预制棒内部形成气泡，影响光纤预制棒的质量。
发明内容
本发明的目的在于提供一种解决除碳和脱水问题、以获得低C和低OH光纤预制棒的光纤预制棒的制造装置及其制造方法。
本发明提供一种光纤预制棒的制造装置，其包括：氧化脱水烧结炉、位于该烧结炉 内的中心管、位于该烧结炉内且位于该中心管外的至少一发热体、位于该中心管内的SiO2坯体、用于密封该中心管的密封罩、位于该中心管内称为内腔体、位于该中心管外且位于烧结炉内称为外腔体、连接至该外腔体的第一真空排气管和第一气管、连接至该烧结炉的第二真空排气管和第二气管，其中，所述发热体、SiO2坯体、以及密封罩均位于所述烧结炉内。
本发明又提供一种光纤预制棒的制造方法，其包括如下步骤：
第一步：对位于中心管内的SiO2坯体进行真空处理；
第二步：在真空状态下，外腔体内通入He气体、内腔体内通入O2气体、Cl2气体、和He气体，使SiO2坯体充分吸附；
第三步：加热加热器，使得SiO2坯体的温度加热至第一预设温度，SiO2坯体内的C与O2充分反应；
第四步：继续加热加热器，使得SiO2坯体的温度加热至第二预设温度，SiO2坯体内的OH与Cl2充分反应；
第五步：停止加热器加热，对SiO2坯体进行真空处理；
第六步：继续加热加热器，使得SiO2坯体温度加热至第三预设温度，对SiO2坯体进行玻璃化处理，获得低C、低OH的光纤预制棒。
步骤F4：待内腔体内的压力增加至101kpa时，将玻璃化之后的SiO2坯体去除，获得低C、低OH的光纤预制棒。
本发明方法，通过SiO2坯体的脱OH和除C的方法和氧化脱水烧结炉,解决除碳和脱水问题，以获得低C和低OH光纤预制棒；本发明结构简单、可靠。
附图说明
图1所示为本发明光纤预制棒的制造装置的结构示意图；
图2所示为本发明光纤预制棒的制造方法的流程示意图。
图号说明：
1-第一真空泵、2-第一真空排气管、3-第二压力传感器、4-第二气管、5-发热体、6-第二真空泵、7-第二真空排气管、8-第一压力传感器、9-第一气管、10-SiO2坯体、11-氧化脱水烧结炉、12-中心管、13-内腔体、14-密封罩、15-外腔体。
具体实施方式
如图1所示为本发明光纤预制棒的制造装置的结构示意图，本光纤预制棒坯体的制造装置包括氧化脱水烧结炉11、位于该氧化脱水烧结炉11内的透明石英玻璃制成的中心管12、位于该中心管12两侧的发热体5、位于该中心管12内的SiO2坯体(二氧化硅胚体)10、用于密封该中心管12的密封罩14、位于该中心管12内称为内腔体12、位于该中心管12外且位于烧结炉11内称为外腔体15、连接至该外腔体15的第一真空排气管2和第一气管9、连接在该第一真空排气管2上且位于外腔体15外的第一真空泵1、连接在该第一气管9上且位于外腔体15外的第一压力传感器8、连接至该烧结炉11的第二真空排气管7和第二气管4、连接在该第二真空排气管7上且位于外腔体15外的第二真空泵6、以及连接在该第二气管4上且位于外腔体15外的第二压力传感器3。其中，发热体5、SiO2坯体(二氧化硅胚体)10、以及密封罩14均位于烧结炉11内。
其中，中心管12可以将腐蚀氧化性气体与氧化脱水烧结炉11内的石墨件、金属等易于氧化的部件隔离开；发热体5用于对氧化脱水烧结炉11的内腔体13进行加热；第一真空排气管2用于外腔体15真空排气，第一真空泵1用于外腔体15抽真空；第二真空排气管7用于内腔体13真空排气，第二真空泵6用于内腔体13抽真空；第一气管9用于向外腔体15内供气，第一压力传感器8用于外腔体15压力监视，第二气管4用于向内腔体13内供气，第二压力传感器3用于内腔体13压力监视。
在光纤预制棒坯体的氧化脱水过程中，使用监视外腔体15压力的第一压力传感器8和监视内腔体13压力的第二压力传感器3，达到监视中心管12内外的压差，以此来控制用于由于对外腔体15抽真空的第一真空泵1和用于内腔体13抽真空的第二真空泵6的抽真空速度；控制用于向外腔体15通气的第一气管9和用于向内腔体13通气的第二气管4内气体的流量，来控制中心管12内的压力始终低于该中心管12外的压力，且中心管12外的压力与中心管12内的压力差为0-350pa,优选50-100pa，以避免Cl2和O2从烧结炉11内溢出，从而避免Cl2、HCl以及O2等氧化腐蚀性气体对石墨件和金属的氧化腐蚀。
本发明光纤预制棒的制造方法，具有如下步骤：
在光纤预制棒坯体的氧化脱水过程中，监视第一压力传感器8和第二压力传感器3，监视中心管12内外的压力差，得到第一真空泵1和第二真空泵6的抽真空速度。
控制第一气管9向外腔体15通气体的流量、控制第二气管4向内腔体13通气体的流量，保持中心管12内的压力始终低于该中心管12外的压力。
如图2所示，本发明光纤预制棒的制造方法，其包括如下步骤：
第一步：对位于中心管12内的SiO2坯体10进行真空处理：具体的是，将SiO2坯体10内的气体排空。
第二步：在真空状态下，外腔体15内通入He气体、内腔体13内通入O2气体、Cl2气体、和He气体，使SiO2坯体10充分吸附。
第三步：加热加热器5，使得SiO2坯体10的温度加热至第一预设温度，SiO2坯体10内的C与O2充分反应。
第四步：继续加热加热器5，使得SiO2坯体10的温度加热至第二预设温度，SiO2坯体10内的OH与Cl2充分反应。
第五步：停止加热器加热，对SiO2坯体10进行真空处理，通过第二气管4使SiO2坯体10内的气体被排出。
第六步：继续加热加热器5，使得SiO2坯体10温度加热至第三预设温度，对SiO2坯体进行玻璃化处理，获得透明的低C、低OH的光纤预制棒。
其中，第一预设温度为800℃；第二预设温度为1200℃；第三预设温度为1500℃。
本发明光纤预制棒的制造方法与现有光纤预制棒的制造方法相比，由于增加的技术方案包括：上述第二步：分别向外腔体通入He气体、内腔体13内通入O2、Cl2、和He气体；上述第三四步：使SiO2坯体内的OH和Cl2充分的反应。
通过这样的改变，采用发明光纤预制棒的制造方法制得低C、低OH的光纤预制棒。
本发明SiO2坯体10的制造方法，具有如下三个实施例：
第一实施例：以CH4和O2为反应气体、以及以SiCl4为原料，通过沉积方法获得密度0.4～0.8g/cm3的SiO2坯体10。
第二实施例：以H2和O2为反应气体、以及以OMCTS为原料，通过沉积方法获得密度0.4～0.8g/cm3的SiO2坯体10。
第三实施例：以CH4和O2为反应气体、以及以OMCTS为原料，通过沉积方法获得密度0.4～0.8g/cm3的SiO2坯体10。
通过上述三种沉积方法制得的SiO2坯体10置于本发明中的氧化脱水烧结炉11之中，并盖上密封罩14，本发明光纤预制棒的制造方法也具有三个实施例。
本发明光纤预制棒的制造方法的第一实施例：采用SiO2坯体10第一实施例的制造方法制成SiO2坯体10，本发明光纤预制棒的制造方法的第一、第三步至第六步的具体内容 如下：
上述第一步的具体步骤为：
步骤A1：SiO2坯体10置于烧结炉11之中，并盖上密封罩14。
步骤A2：同步降低内腔体13和外腔体15的压力，使得内腔体13和外腔体15处于真空状态，即：中心管12外的压力与该中心管12内的压力均为5pa(5pa是一个绝对压力，换算成真空度，5pa小于0.1MPa，即相当于绝对压力为0)，并保持第一预设时间。
该第一预设时间为30min。
上述第二步的具体步骤为：
步骤B1：在真空状态下，第一气管9向外腔体15通入He气体，同时第二气管4向内腔体13通入3slm的O2气体、2slm的Cl2气体、以及3slm的He气体，使SiO2坯体10充分吸附。
步骤B2：第一压力传感器8监视中心管12外的外腔体15内的压力，同时第二压力传感器3监视中心管12内的内腔体12内的压力，始终保持外腔体15的压力与内腔体13的压力的压力差大于第一预设压力。
该第一预设压力为5-250pa。
步骤B3：当内腔体13的压力达到第一预设压力值时，停止向内腔体13和外腔体15通气，保持第二预设时间，使SiO2坯体10充分吸附。该第一预设压力值为104pa；第二预设时间为90min。
上述第三步的具体内容为：加热加热器5，以第一预设加热速度将SiO2坯体10的温度加热至第一预设温度，并保持第三预设时间，使SiO2坯体10内的C与O2充分反应。
该第一预设加热速度为3.5℃/min；该第一预设温度为800℃；该第三预设时间为120min。
上述第四步的具体内容为：继续加热加热器5，以第二预设加热速度将SiO2坯体10的温度加热至第二预设温度，使SiO2坯体10内的OH和Cl2充分的反应。
该第二预设加热速度为10℃/min；该第二预设温度为1200℃。
上述第五步的具体内容为：
步骤E1:同步启动第一真空泵1和第二真空泵6，使中心管12外的外腔体15的压力大于中心管12内的内腔体13的压力，并始终保持外腔体15的压力与内腔体13的压力的压力差大于第二预设压力。
该第二预设压力为50-100pa。
步骤E2：同步降低内腔体13和外腔体15的压力，使得内腔体13和外腔体15处于真空状态，即：中心管12外的压力与该中心管12内的压力均为5pa(5pa是一个绝对压力，换算成真空度，5pa小于0.1MPa，即相当于绝对压力为0)，并保持第三预设时间。
第三预设时间为120min。
上述第六步的具体内容为：
步骤F1：继续加热加热器5，以第三预设加热速度将SiO2坯体10的温度加热至第三预设温度，保持第四预设时间，使SiO2坯体10充分玻璃化。
该第三预设温度为1500℃；第三预设加热速度为5℃/min；该第四预设时间为20min。
步骤F2：SiO2坯体10以第四预设降温速度降至第四预设温度。
该第四预设降温速度为5℃/min；该第四预设温度为400℃。
步骤F3：第一气管9向外腔体15内通入N2，同时第二气管4向内腔体13内通入N2，保持中心管12内的压力始终低于该中心管12外的压力，且该中心管12外的压力与中心管12内的压力的压力差为第三预设压力以内。
该第三预设压力为250pa。
步骤F4：待内腔体13内的压力增加至101kpa时，将玻璃化之后的SiO2坯体10去除，获得OH含量为0.6ppm和C含量为5ppm的光纤预制棒。
现有技术采用本第一实施例光纤预制棒的制造方法，获得OH含量为143ppm(高含量)和C含量为92ppm(高含量)的光纤预制棒。
本发明光纤预制棒的制造方法的第二实施例：采用SiO2坯体10第二实施例的制造方法制成SiO2坯体10，本发明光纤预制棒的制造方法的第二实施例与上述第一实施例的区别如下：
步骤B2：第一压力传感器8监视中心管12外的外腔体15内的压力，同时第二压力传感器3监视中心管12内的内腔体12内的压力，始终保持外腔体15的压力与内腔体13的压力的压力差大于第二预设压力。即：外腔体15的压力与内腔体13的压力的压力差不同。
该第二预设压力为50-100pa。
步骤F4：待内腔体13内的压力增加至101kpa时，将玻璃化之后的SiO2坯体10去除，获得OH含量为1ppm和C含量为3ppm的光纤预制棒。即：光纤预制棒的OH含量和C含量不同。
现有技术采用本第二实施例光纤预制棒的制造方法，获得OH含量为164ppm(高含量)和C含量为227ppm(高含量)的光纤预制棒。
本发明光纤预制棒的制造方法的第三实施例：采用SiO2坯体10第三实施例的制造方法制成SiO2坯体10，本发明光纤预制棒的制造方法的第三实施例与上述第一实施例的区别如下：
步骤F4：内腔体13内的压力增加至第四预设压力时，将玻璃化之后的SiO2坯体10去除，获得OH含量为0.7ppm和C含量为8ppm的光纤预制棒。即：光纤预制棒的OH的含量和C的含量不同。
该第四预设压力为101kpa。
现有技术采用本第三实施例光纤预制棒的制造方法，获得OH含量为169ppm(高含量)和C含量为261ppm(高含量)的光纤预制棒。
本发明方法，通过SiO2坯体的脱OH和除C的方法和氧化脱水烧结炉,解决除碳和脱水问题，以获得低C和低OH光纤预制棒；本发明结构简单、可靠。
以上参照附图说明了本发明的优选实施例，本领域技术人员不脱离本发明的范围和实质，可以有多种变型方案实现本发明。举例而言，作为一个实施例的部分示出或描述的特征可用于另一实施例以得到又一实施例。以上仅为本发明较佳可行的实施例而已，并非因此局限本发明的权利范围，凡运用本发明说明书及附图内容所作的等效变化，均包含于本发明的权利范围之内。
以上详细描述了本发明的优选实施方式，但是本发明并不限于上述实施方式中的具体细节，在本发明的技术构思范围内，可以对本发明的技术方案进行多种等同变换，这些等同变换均属于本发明的保护范围。

Claims (15)

  1. 一种光纤预制棒的制造装置，其特征在于，其包括：氧化脱水烧结炉、位于该烧结炉内的中心管、位于该烧结炉内且位于该中心管外的至少一发热体、位于该中心管内的SiO2坯体、用于密封该中心管的密封罩、位于该中心管内称为内腔体、位于该中心管外且位于烧结炉内称为外腔体、连接至该外腔体的第一真空排气管和第一气管、连接至该烧结炉的第二真空排气管和第二气管，其中，所述发热体、SiO2坯体、以及密封罩均位于所述烧结炉内。
  2. 根据权利要求1所述的光纤预制棒的制造装置，其特征在于：还包括连接在该第一真空排气管上且位于外腔体外的第一真空泵、以及连接在该第二真空排气管上且位于外腔体外的第二真空泵。
  3. 根据权利要求1所述的光纤预制棒的制造装置，其特征在于：还包括连接在该第一气管上且位于外腔体外的第一压力传感器、以及连接在该第二气管上且位于外腔体外的第二压力传感器。
  4. 采用权利要求1-3任一所述的制造装置的光纤预制棒的制造方法，其特征在于，其包括如下步骤：
    第一步：对位于中心管内的SiO2坯体进行真空处理；
    第二步：在真空状态下，外腔体内通入He气体、内腔体内通入O2气体、Cl2气体、和He气体，使SiO2坯体充分吸附；
    第三步：加热加热器，使得SiO2坯体的温度加热至第一预设温度，SiO2坯体内的C与O2充分反应；
    第四步：继续加热加热器，使得SiO2坯体的温度加热至第二预设温度，SiO2坯体内的OH与Cl2充分反应；
    第五步：停止加热器加热，对SiO2坯体进行真空处理；
    第六步：继续加热加热器，使得SiO2坯体温度加热至第三预设温度，对SiO2坯体进行玻璃化处理，获得低C、低OH的光纤预制棒。
  5. 根据权利要求4所述的光纤预制棒的制造方法，其特征在于：所述SiO2坯体的制造方法为：以CH4和O2为反应气体、以及以SiCl4为原料，通过沉积方法获得SiO2坯体。
  6. 根据权利要求4所述的光纤预制棒的制造方法，其特征在于：所述SiO2坯体的制造方法为：以H2和O2为反应气体、以及以OMCTS为原料，通过沉积方法获得SiO2坯 体。
  7. 根据权利要求4所述的光纤预制棒的制造方法，其特征在于：所述SiO2坯体的制造方法为：以CH4和O2为反应气体、以及以OMCTS为原料，通过沉积方法获得SiO2坯体。
  8. 根据权利要求5-7任一所述的光纤预制棒的制造方法，其特征在于：所述第一步包括如下步骤：
    步骤A1：SiO2坯体置于烧结炉之中，并盖上密封罩；
    步骤A2：同步降低内腔体和外腔体的压力，使得内腔体和外腔体处于真空状态，并保持第一预设时间。
  9. 根据权利要求8所述的光纤预制棒的制造方法，其特征在于：所述第二步包括如下步骤：
    步骤B1：在真空状态下，第一气管向外腔体通入He气体，同时第二气管向内腔体通入O2气体、Cl2气体、以及He气体，使SiO2坯体充分吸附；
    步骤B2：监视中心管外的外腔体内的压力，同时监视中心管内的内腔体内的压力，始终保持外腔体的压力大于内腔体的压力；
    步骤B3：当内腔体的压力达到第一预设压力值时，停止向内腔体和外腔体通气，保持第二预设时间，使SiO2坯体10充分吸附。
  10. 根据权利要求9所述的光纤预制棒的制造方法，其特征在于：所述步骤B2，外腔体的压力与内腔体的压力的压力差大于第一预设压力5-250pa、或者外腔体的压力与内腔体的压力的压力差大于第二预设压力。
  11. 根据权利要求9所述的光纤预制棒的制造方法，其特征在于：所述第三步的具体内容为：加热加热器，以第一预设加热速度将SiO2坯体的温度加热至第一预设温度，并保持第三预设时间，使SiO2坯体内的C与O2充分反应。
  12. 根据权利要求11所述的光纤预制棒的制造方法，其特征在于：所述第四步的具体内容为：继续加热加热器，以第二预设加热速度将SiO2坯体的温度加热至第二预设温度，使SiO2坯体内的OH和Cl2充分的反应。
  13. 根据权利要求12所述的光纤预制棒的制造方法，其特征在于：所述第五步包括如下步骤：
    步骤E1:同步启动第一真空泵和第二真空泵，使中心管外的外腔体的压力大于中心 管内的内腔体的压力，并始终保持外腔体的压力与内腔体的压力的压力差大于第二预设压力；
    步骤E2：同步降低内腔体和外腔的压力，使得内腔体和外腔体处于真空状态，并保持第三预设时间。
  14. 根据权利要求13所述的光纤预制棒的制造方法，其特征在于：所述第五步包括如下步骤：
    步骤F1：继续加热加热器，以第三预设加热速度将SiO2坯体的温度加热至第三预设温度，保持第四预设时间，使SiO2坯体充分玻璃化；
    步骤F2：SiO2坯体以第四预设降温速度降至第四预设温度；
    步骤F3：第一气管向外腔体内通入N2，同时第二气管向内腔体内通入N2，保持中心管内的压力始终低于该中心管外的压力，且该中心管外的压力与中心管内的压力的压力差为第三预设压力以内；
    步骤F4：内腔体内的压力增加至第四预设压力时，将玻璃化之后的SiO2坯体去除，获得低C、低OH的光纤预制棒。
  15. 根据权利要求14所述的光纤预制棒的制造方法，其特征在于：第一预设温度为800℃；第二预设温度为1200℃；第三预设温度为1500℃；该第四预设温度为400℃；第一预设时间为30min；第二预设时间为90min；第三预设时间为120min；该第四预设时间为20min；该第一预设压力值104pa；该第一预设加热速度为3.5℃/min；该第二预设加热速度为10℃/min；第三预设加热速度为5℃/min；该第四预设降温速度为5℃/min；该第一预设压力为5-250pa；该第二预设压力为50-100pa；该第三预设压力为250pa；该第四预设压力为101kpa。
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