CN1159242C - Process for preparing high-strength antifatigue optical fibre - Google Patents
Process for preparing high-strength antifatigue optical fibre Download PDFInfo
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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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- 239000013307 optical fiber Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 230000002929 anti-fatigue Effects 0.000 title claims description 18
- 239000010936 titanium Substances 0.000 claims abstract description 68
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 67
- 238000000034 method Methods 0.000 claims abstract description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000010453 quartz Substances 0.000 claims abstract description 12
- 238000005491 wire drawing Methods 0.000 claims abstract description 10
- 238000003980 solgel method Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000011521 glass Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 15
- 239000003595 mist Substances 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 239000000084 colloidal system Substances 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
- 230000004927 fusion Effects 0.000 claims description 4
- 238000009775 high-speed stirring Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000001879 gelation Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 10
- 239000000835 fiber Substances 0.000 abstract description 10
- 230000003287 optical effect Effects 0.000 abstract description 8
- 230000008021 deposition Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract 2
- 239000011247 coating layer Substances 0.000 abstract 1
- 238000001947 vapour-phase growth Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- 239000010410 layer Substances 0.000 description 11
- 238000006460 hydrolysis reaction Methods 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 230000007062 hydrolysis Effects 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 239000003929 acidic solution Substances 0.000 description 5
- 239000003637 basic solution Substances 0.000 description 5
- 238000007654 immersion Methods 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000013459 approach Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000001117 sulphuric acid Substances 0.000 description 4
- 235000011149 sulphuric acid Nutrition 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 3
- 150000003608 titanium Chemical class 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 241001300078 Vitrea Species 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000006121 base glass Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- -1 germanium ion Chemical class 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Images
Classifications
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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
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.
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CNB011335459A CN1159242C (en) | 2001-10-10 | 2001-10-10 | Process for preparing high-strength antifatigue optical fibre |
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CNB011335459A CN1159242C (en) | 2001-10-10 | 2001-10-10 | Process for preparing high-strength antifatigue optical fibre |
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CN1159242C true CN1159242C (en) | 2004-07-28 |
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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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2001
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