CN1159242C - Process for preparing high-strength antifatigue optical fibre - Google Patents

Process for preparing high-strength antifatigue optical fibre Download PDF

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CN1159242C
CN1159242C CNB011335459A CN01133545A CN1159242C CN 1159242 C CN1159242 C CN 1159242C CN B011335459 A CNB011335459 A CN B011335459A CN 01133545 A CN01133545 A CN 01133545A CN 1159242 C CN1159242 C CN 1159242C
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titanium
mix
mixture
temperature range
optical fibre
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CN1356277A (en
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童维军
王铁军
曹宇青
谢康
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Yangtze Optical Fibre and Cable Co Ltd
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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
    • C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
    • 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
    • C03B37/0128—Manufacture of preforms for drawing fibres or filaments starting from pulverulent glass
    • C03B37/01291—Manufacture of preforms for drawing fibres or filaments starting from pulverulent glass by progressive melting, e.g. melting glass powder during delivery to and adhering the so-formed melt to a target or preform, e.g. the Plasma Oxidation Deposition [POD] process
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
    • C03B2201/40—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
    • C03B2201/42—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn doped with titanium

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The present invention discloses technology for manufacturing a high-strength fatigue resistance optical waveguide fiber by using an outer coating layer mixing titanium. The present invention is composed of the following steps: 1. a sol-gel method is used for synthesizing quartz micro powder mixing titanium; 2. the quartz micro powder mixing titanium is made into a quartz glass pipe mixing titanium; 3. the plasma chemical vapor phase deposition technology is used for preparing a core rod; 4. a sleeve pipe method is used for synthesizing an optical fiber prefabricated rod; 5. the optical fiber prefabricated rod is withdrawn by adopting the wiredrawing technology of the sleeve pipe method. Then, the high-strength fatigue resistance optical waveguide fiber is obtained. The present invention solves the problems that a titanium mixing process and a rod making process are carried out on the same device in the prior art, which has the disadvantages of greatly improved original device, large investment and low deposition efficiency of titanium. When the technology is adopted, the tensile strength and the fatigue resistance performance of the optical fiber can be increased.

Description

Make the production technique of high-strength antifatigue optical fibre
Technical field
The present invention relates to a kind of production technique of optical guided wave fibre, the production technique that the titanium surrounding layer is made high-strength antifatigue optical fibre is mixed in specifically a kind of employing.
Background technology
As typical ceramic, silica glass inherent intensity is very high.In theory, because the bond energy of ionic linkage or covalent bonds oxide material is much larger than metallic bond bonded metallic substance, the tensile strength of silica fiber is than the high several magnitude of steel fiber (as copper wire, aluminium wire etc.) of same geometrical dimension.But in actual applications, because the surface easily contaminated (mainly being the contaminant particles of introducing in the drawing process) or the corrosion (mainly being water vapour, ammonia or other corrosive gases) of the SiO2 that opticfiber communication is used base glass bare fibre, form defective or center of stress, under the effect of tensile stress, form the tiny crack (process of the random growth of this tiny crack is referred to as fatigue) of random growth, make its tensile strength be exponential decline.
In order to reduce or stop the formation of glass optical fiber surface imperfection, thereby the mechanical property of improving optical fiber increases the work-ing life of optical fiber, many investigators did the work of this respect, mainly contain two kinds of effective solution routes at present: a kind of is to be coated with in the pulling process of glass optical fiber its surface to enclose plastic protective layer, avoid glass surface directly contact with extraneous, at present in the drawing process generally employing be that the resene organism of thermoset, gas-solid or ultra-violet curing is coated; Another kind of approach is that various processing are carried out on the glass optical fiber surface.People know that already adding the low glass of one deck thermal expansivity in advance on Vitrea surface can make its tensile strength increase, because this mixture is chilled to the process of room temperature from high temperature, can form stress on the surface of glass, it can stop the formation and the expansion of glass surface tiny crack.The relevant technical literature of this solution route some, as the GlassFibers:I of people such as Giffen application, Cladding,, Journal of the American Ceramic Society, Vol.52, No.12, pp661-4, Dec.1969.At present, preceding a kind of technological approaches comparative maturity, extensively by domestic and international optical fiber manufacturer usefulness, then a kind of technological approaches is the direction that this technical field is mainly studied.
In order to prepare the enhancing optical fiber that this outside surface has stress, done many trials both at home and abroad, the research of wherein doped titanium quartzy surrounding layer optical fiber is main direction.The document primary study of announcing be the influence of the doped titanium concentration of surrounding layer and cladding thickness to the optical fiber mechanical property.It is generally acknowledged TiO 2-SiO 2Glass is according to TiO 2Doping content can be divided into three zones: stabilized zone (0-10wt%), metastable zone (10-18wt%) and unstable region (＞18wt%) wherein the doping content about 10wt% can reach more excellent performance.In addition, document is thought the tiny crack degree of depth of optical fiber surface generally at 0.5-1.5um, and therefore, suitable surrounding layer thickness is comparatively suitable about 3um.
United States Patent (USP) (patent No. U.S.Pat.No.5067975,5140665,5180411,6189340) has been introduced in more detail and has been adopted the outer vapour deposition process of pipe (OVD technology) manufacturing to mix the production technique and the waveguiding structure of titanium surrounding layer optical waveguides, and has introduced a kind of thin covering enhancing optical waveguides.Adopt the outer gas-phase deposition manufacturing of pipe to mix titanium surrounding layer optical guided wave fibre, it mixes the titanium process and the system rod motion carries out on same equipment, needs original equipment is carried out bigger improvement, and investment is big, and adopts the sedimentation effect of this method titanium low.
Summary of the invention
Goal of the invention of the present invention is exactly the defective at the outer vapour deposition process manufacturing process of aforementioned tube, the synthetic in advance titanium quartz glass sleeve of mixing of a kind of employing sol-gel method is proposed, the glass plug of using plasma chemical vapor deposition method (PCVD technology) preparation design waveguiding structure, the two assembles preform, carry out wire drawing then, thereby make the production technique of high-strength antifatigue optical fibre, to remedy the deficiency of existing production technique.
In order to realize the foregoing invention purpose, the present invention has adopted following technical scheme:
The present invention selects high-purity Ti Cl for use 4TiCl 3Or Ti (SO 4) 2, silicon sol or SiO 2Micro mist, the vitriol oil, hydrochloric acid, ammoniacal liquor and deionized water, organic solvent are as chemical feedstocks, and pure quartz glass tube is as the vapour deposition starting material.
Technical scheme of the present invention is made up of five parts:
1) the synthetic titanium quartz micropowder (see figure 3) of mixing of sol-gel method
A, adopt that sol-gel method is synthetic mixes the titanium quartz micropowder three kinds of technological approaches are arranged:
One, at first prepare titanium colloidal sol, then quartz micropowder is evenly spread among the above-mentioned titanium colloidal sol, the surface that makes colloid be wrapping to micro mist by the pH value (＞3.5 scopes) that adds ammonia soln adjusting mixture forms gel mixture, remove solution, collect gel mixture, use deionized water rinsing again, in 70-500 ℃ temperature range, carry out drying then, then dried powder is washed again, in 70-500 ℃ temperature range, carry out drying again, obtain ionic TiO free from foreign meter 2-SiO 2Powder.
They are two years old, prepare silicon sol and titanium colloidal sol respectively, then in the process of mixing two kinds of colloidal sols, add the pH value (scope of 1-5) that dilute sulphuric acid or dilute hydrochloric acid solution are regulated colloid mixture on one side, one side high-speed stirring, make the mixture uniform mixing but do not flocculate, pH value (＞3.5 scopes) to the colloid that adds ammonia soln adjustment colloid mixture again forms gel, remove solution, collect gel mixture, use deionized water rinsing again, in 70-500 ℃ temperature range, carry out drying then, dry intact back is washed dried powder, carries out drying again and obtain ionic TiO free from foreign meter in 70-500 ℃ temperature range 2-SiO 2Powder.
Its three, with highly purified silicon sol and TiCl 3Mix, stirred for several hour obtains the mixture of partial gel at normal temperatures, add dilute sulphuric acid and dilute hydrochloric acid again and make the mixture flocculation, remove solution, collect gel mixture, use deionized water rinsing again, in 70-500 ℃ temperature range, carry out drying then, then dried powder is washed, in 70-500 ℃ temperature range, carry out drying again, obtain ionic TiO free from foreign meter 2-SiO 2Powder.
B, sol-gel technology control:
Form in the process of sol-gel in the titanium salt hydrolysis, follow general saline hydrolysis rule, that is:
A, solution are thin more, and hydrolysis degree is big more; Otherwise solution is dense more, and hydrolysis degree is more little.
B, no matter be titanium tetrachloride or titanous chloride, titanium sulfate, all belong to strong acid weak base salt, it is acid that solution is.
C, hydrolysis reaction are thermo-negative reaction, add the hydrolysis that heat energy promotes titanium solution.Especially when titanium tetrachloride and titanous chloride hydrolysis, hydrolysate HCl has volatility, adds heat energy and promotes that HCl constantly breaks away from solution, thereby promote that hydrolysis reaction is more violent.
Therefore, in the process of the sol-gel for preparing titanium salt, principle according to the titanium salt hydrolysis, control entire reaction course by strictness control strength of solution, regulator solution pH value and control reaction temperature (20-120 ℃), comprise and mix titanium concentration (0-15% weight ratio) and homogeneity, gel particle size and density etc.
2) vitrifying of micro mist
Adopt the sol-gel method synthetic mix titanium micro powder granule granularity below 1mm, chemisorption water-content height, mainly be to make its degassing, dehydration in vitrified process.The present invention can adopt two kinds of glassification process: one, and will mix the titanium micro mist and place the fusion in the temperature range more than 1800 ℃ of high frequency graphite electric furnace, select for use graphite jig to be drawn into and mix the titanium quartz glass tube; Its two, adopt gas smelting mixing the outside surface that the titanium micro mist is deposited on purity quartz glass pipe for high, again the gained Glass tubing is placed the logical chlorine of annealing furnace in 900-1200 ℃ of temperature range, to handle to carry out processed in 10-30 hour and eliminates stress.
3) preparation of plug
As everyone knows, PCVD technology is to realize the more excellent chemical vapor deposition method of complex index of refraction section, and the thickness that at every turn deposits glass coating can be controlled at several microns the order of magnitude.According to different waveguiding structures, the doping content of germanium ion and fluorion can accurately realize the refractive index profile of required plug in the adjusting deposition process.
4) preparation of preform
Gained is mixed the titanium quartz glass tube and plug polishes with oxyhydrogen flame respectively, carry out the immersion of basic solution and acidic solution more respectively, use deionized water rinsing then, remove planar water with volatile organic solvent again, the plug after the glass processing is inserted in the doped titanium quartz glass sleeve obtain preform at last.
5) drawing optical fiber
The gained preform adopts the tiretube process drawing process to carry out wire drawing on conventional wire-drawer-tower, and its drawing process should be controlled the geometry of wire-drawing temperature (1800-2000 ℃ temperature range) and optical fiber.In theory, the cross section of each interfacial layer of prefabricated rods is scaled in the drawing optical fiber.According to the design requirements of fiber geometric, need accurately control during the structure of prefabricated rods, the geometry of general emphasis control optical waveguides, again the geometrical dimension of the external diameter of the adjusting wire-drawing temperature control optical fiber by among a small circle and surrounding layer (≤10um).TiO for independent drawing 2-SiO 2The synthetic glass pipe can reduce TiO according to the plug of the big geometric proportion of capacity of equipment deposition 2-SiO 2The control difficulty of synthetic glass pipe cross-sectional area.
The present invention has following beneficial effect:
1, the tensile strength and the anti-fatigue performance of optical fiber have been increased
By doping treatment, added stress in advance at the optical fiber outside surface, can stop the formation and the expansion of optical fiber tiny crack under action of pulling stress, reach the performance of high-strength anti-fatigue.
2, reduced cost
The present invention breaks away from synthesis technique and the optical fiber production equipment of mixing the titanium quartz glass tube, and the optical fiber producing apparatus huge to original investment do not have any transformation, do not influence the ordinary production technology of conventional fiber yet.In addition, the synthetic preform production unit of titanium quartz glass tube facility investment of mixing of sol-gel method of the present invention much smaller than issued patents special use.
Description of drawings
Fig. 1 is a process route chart of the present invention;
Fig. 2 is the synthetic TiO of the present invention 2-SiO 2The micro mist process route chart;
Fig. 3 mixes titanium surrounding layer optical guided wave fibre structural representation for the inventive method system.
1 sandwich layer, 2 inner claddings 3 are mixed the titanium surrounding layer
Embodiment
Below enumerate part embodiment, the inventive method be described further:
Embodiment one:
At first prepare titanium colloidal sol, then quartz micropowder is evenly spread among the above-mentioned titanium colloidal sol, the pH value of regulating mixture by the adding ammonia soln is 5, and the surface that makes colloid be wrapping to micro mist forms gel mixture, removes solution, collect gel mixture, use deionized water rinsing again, carry out drying 200 ℃ temperature then, then dried powder is washed again, in 200 ℃ temperature range, carry out drying again, obtain ionic free from foreign meter and mix titanium micro mist TiO 2-SiO 2Powder.To mix the titanium micro mist and place the fusion in the temperature range more than 1800 ℃ of high frequency graphite electric furnace, and select for use graphite jig to be drawn into and mix the titanium quartz glass tube; To mix titanium quartz glass tube using plasma chemical vapor deposition method and make plug; To mix titanium quartz glass tube and plug polishes with oxyhydrogen flame respectively, carry out the immersion of basic solution and acidic solution more respectively, use deionized water rinsing then, increase except that planar water with volatile organic solvent again, the plug after the glass processing is inserted in the doped titanium quartz glass sleeve obtain preform at last; Adopt the tiretube process drawing process on conventional wire-drawer-tower the gained preform, carry out wire drawing, promptly make high-strength antifatigue optical fibre 1800 ℃ temperature.
Embodiment two:
Prepare silicon sol and titanium colloidal sol respectively, then in the process of mixing two kinds of colloidal sols, the pH value that adds dilute acid soln adjusting colloid mixture on one side is 1, one side high-speed stirring, make the mixture uniform mixing but do not flocculate, adding ammonia soln again, to adjust the pH value of colloid mixture be 4 to form gel to colloid, remove solution, collect gel mixture, use deionized water rinsing again, carry out drying 70 ℃ of temperature then, dry intact back is washed dried powder, carries out drying 70 ℃ temperature again and obtains ionic TiO free from foreign meter 2-SiO 2Powder.Adopt gas smelting mixing the outside surface that the titanium micro mist is deposited on purity quartz glass pipe for high, again the gained Glass tubing is placed the logical chlorine of annealing furnace to dewater in 30 hours and eliminate stress 900 ℃ of Temperature Treatment.To mix titanium quartz glass tube using plasma chemical vapor deposition method and make plug; To mix titanium quartz glass tube and plug polishes with oxyhydrogen flame respectively, carry out the immersion of basic solution and acidic solution more respectively, use deionized water rinsing then, increase except that planar water with volatile organic solvent again, the plug after the glass processing is inserted in the doped titanium quartz glass sleeve obtain preform at last; Adopt the tiretube process drawing process on conventional wire-drawer-tower the gained preform, carry out wire drawing, promptly make high-strength antifatigue optical fibre 1800 ℃ temperature.
Embodiment three:
With highly purified silicon sol and TiCl 3Mix, stir the mixture that obtained partial gel in 3 hours at normal temperatures, add dilute sulphuric acid and dilute hydrochloric acid again and make the mixture flocculation, remove solution, collect gel mixture, use deionized water rinsing again, in 500 ℃ temperature range, carry out drying then, then dried powder is washed, in 500 ℃ temperature range, carry out drying again, obtain ionic TiO free from foreign meter 2-SiO 2Powder.Adopt gas smelting mixing the outside surface that the titanium micro mist is deposited on purity quartz glass pipe for high, again the gained Glass tubing is placed the logical chlorine of annealing furnace to dewater in 20 hours and eliminate stress 1200 ℃ of Temperature Treatment.To mix titanium quartz glass tube using plasma chemical vapor deposition method and make plug; To mix titanium quartz glass tube and plug polishes with oxyhydrogen flame respectively, carry out the immersion of basic solution and acidic solution more respectively, use deionized water rinsing then, increase except that planar water with volatile organic solvent again, the plug after the glass processing is inserted in the doped titanium quartz glass sleeve obtain preform at last; Adopt the tiretube process drawing process on conventional wire-drawer-tower the gained preform, carry out wire drawing, promptly make high-strength antifatigue optical fibre 1800 ℃ temperature.
Embodiment four:
With highly purified silicon sol and TiCl 3Mix, stir the mixture that obtained partial gel in 3 hours at normal temperatures, add dilute sulphuric acid and dilute hydrochloric acid again and make the mixture flocculation, remove solution, collect gel mixture, use deionized water rinsing again, in 300 ℃ temperature range, carry out drying then, then dried powder is washed, in 300 ℃ temperature range, carry out drying again, obtain ionic TiO free from foreign meter 2-SiO 2Powder.To mix the titanium micro mist and place the fusion in the temperature range more than 1800 ℃ of high frequency graphite electric furnace, and select for use graphite jig to be drawn into and mix the titanium quartz glass tube; To mix titanium quartz glass tube using plasma chemical vapor deposition method and make plug; To mix titanium quartz glass tube and plug polishes with oxyhydrogen flame respectively, carry out the immersion of basic solution and acidic solution more respectively, use deionized water rinsing then, increase except that planar water with volatile organic solvent again, the plug after the glass processing is inserted in the doped titanium quartz glass sleeve obtain preform at last; Adopt the tiretube process drawing process on conventional wire-drawer-tower the gained preform, carry out wire drawing, promptly make high-strength antifatigue optical fibre 2200 ℃ temperature.

Claims (7)

1, a kind of production technique of making high-strength antifatigue optical fibre, it is made up of following steps:
1) adopts the synthetic titanium quartz micropowder of mixing of sol-gel method;
2) will mix the titanium quartz micropowder makes and mixes the titanium quartz glass tube;
3) the using plasma chemical vapor deposition method is made plug;
4) adopt tiretube process synthetic fibre-optical prefabricated rods;
5) preform is adopted the tiretube process drawing process carry out wire drawing, promptly get high-strength antifatigue optical fibre.
2, a kind of production technique of making high-strength antifatigue optical fibre of claim 1, wherein mix the titanium quartz micropowder and adopt following method preparation: at first prepare titanium colloidal sol, then quartz micropowder is evenly spread among the titanium colloidal sol, the pH value that adds ammonia soln adjusting mixture makes colloid be wrapping to the surface formation gel mixture of micro mist, remove solution, collect gel mixture, use deionized water rinsing again, in 70-500 ℃ temperature range, carry out drying then, then dried powder is washed again, in 70-500 ℃ temperature range, carry out drying again, obtain ionic TiO free from foreign meter 2-SiO 2Powder.
3, a kind of production technique of making high-strength antifatigue optical fibre of claim 1, wherein mix the titanium quartz micropowder and adopt following method preparation: prepare silicon sol and titanium colloidal sol respectively, then two kinds of colloidal sols are mixed, add the pH value that dilute acid soln is regulated colloid mixture on one side, one side high-speed stirring, make the mixture uniform mixing but do not flocculate, pH value to the colloid that adds ammonia soln adjustment colloid mixture again forms gel, remove solution, collect gel mixture, use deionized water rinsing again, in 70-500 ℃ temperature range, carry out drying then, dry intact back is washed dried powder, carries out drying again and obtain ionic TiO free from foreign meter in 70-500 ℃ temperature range 2-SiO 2Powder.
4, a kind of production technique of making high-strength antifatigue optical fibre of claim 1 is wherein mixed the titanium quartz micropowder and is adopted following method preparation: with highly purified silicon sol and TiCl 3Mix, stirred for several hour obtains the mixture of partial gel at normal temperatures, add diluted acid again and make the mixture flocculation, remove solution, collect gel mixture, use deionized water rinsing again, in 70-500 ℃ temperature range, carry out drying then, then dried powder is washed, in 70-500 ℃ temperature range, carry out drying again, obtain ionic TiO free from foreign meter 2-SiO 2Powder.
5, claim 2, a kind of production technique of making high-strength antifatigue optical fibre of 3 or 4, wherein the temperature in colloidal sol and the gelation process is 20-120 ℃.
6, a kind of production technique of making high-strength antifatigue optical fibre of claim 1, wherein mix the titanium quartz glass tube and adopt following method preparation: will mix the titanium micro mist and place the fusion in the temperature range more than 1800 ℃ of high frequency graphite electric furnace, and select for use graphite jig to be drawn into and mix the titanium quartz glass tube.
7, a kind of production technique of making high-strength antifatigue optical fibre of claim 1, wherein mix the titanium quartz glass tube and adopt following method preparation: adopt gas smelting mixing the outside surface that the titanium micro mist is deposited on purity quartz glass pipe for high, again the gained Glass tubing is placed the logical chlorine of annealing furnace in 900-1200 ℃ of temperature range, to handle and carried out processed in 10-30 hour and eliminate stress.
CNB011335459A 2001-10-10 2001-10-10 Process for preparing high-strength antifatigue optical fibre Expired - Lifetime CN1159242C (en)

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Publication number Priority date Publication date Assignee Title
CN100406401C (en) * 2005-09-15 2008-07-30 长飞光纤光缆有限公司 Method for making low water peak optical fiber preformrod adopting plasm outward spraying method
CN113568092B (en) * 2021-07-27 2022-10-25 中国建筑材料科学研究总院有限公司 Multilayer quartz optical fiber and preparation method and application thereof

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