CN102976608A - Method and device for producing diboron trioxide-doped stress rod - Google Patents
Method and device for producing diboron trioxide-doped stress rod Download PDFInfo
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- CN102976608A CN102976608A CN2012105543058A CN201210554305A CN102976608A CN 102976608 A CN102976608 A CN 102976608A CN 2012105543058 A CN2012105543058 A CN 2012105543058A CN 201210554305 A CN201210554305 A CN 201210554305A CN 102976608 A CN102976608 A CN 102976608A
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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]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/30—Polarisation maintaining [PM], i.e. birefringent products, e.g. with elliptical core, by use of stress rods, "PANDA" type fibres
- C03B2203/31—Polarisation maintaining [PM], i.e. birefringent products, e.g. with elliptical core, by use of stress rods, "PANDA" type fibres by use of stress-imparting rods, e.g. by insertion
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Abstract
The invention relates to a method and a device for producing a diboron trioxide-doped stress rod. The method comprises the following steps of: preparing diboron trioxide (B2O3)-doped glass particle preformed rod by a VAD method; putting the B2O3-doped glass particle preformed rod into a sintering furnace, and controlling the sintering temperature to be 1200-1500 DEG C and the sintering speed to be 3-7mm/min; when the starting end is sintered, controlling the heat preservation time to be not shorter than 30 minutes; lifting the B2O3-doped preformed rod to the upper end of a muffle tube, cooling for two or more hours, then taking out the B2O3-doped preformed rod and putting the B2O3-doped preformed rod into an annealing furnace; putting the B2O3-doped preformed rod into a maintaining furnace, slowly heating up to 800-1000 DEG C, annealing for five or more hours, slowly cooling to the room temperature, and then taking out the B2O3-doped preformed rod; welding the B2O3-doped preformed rod and then installing the B2O3-doped preformed rod into an extension device; slowly heating the B2O3-doped preformed rod up to 1350-1450 DEG C in a high temperature furnace, and setting the extension speed to be 5-8mm/min; and after extension, slowly cooling.
Description
Technical field
The present invention relates to the polarization-preserving fiber preform field, especially relate to a kind of production and mix boron trioxide (B
2O
3) method and apparatus of stress rods.
Background technology
Polarization maintaining optical fibre is a kind of special optical fiber, and it has a type optical fiber of the linear polarization that keeps institute's transmission ray.Polarization maintaining optical fibre can be applicable to a lot of fields, such as fibre optic gyroscope, fibre optic hydrophone, polarization sensor, multiplexing coherent communication etc., it is to have the special optical fiber that widespread use is worth, wherein panda type polarization-preserving fiber is high with its birefringence effect, simple in structure, it is high to make efficient, and the characteristics such as stable performance have the leading position in dual-use market.The manufacturing process of panda type polarization-preserving fiber adopts combined method usually.Soon stress rods is inserted into female rod upward and in centrosymmetric two holes, then carries out wire drawing and just obtain panda type polarization-preserving fiber.CN1557754A discloses a kind of method of producing panda type polarization-preserving fiber, but the not explanation of counter stress rod production method.
Maturation along with the preform technology, the main production method of prefabricated rods comprises, the combination of MCVD, PCVD, VAD and OVD and front four kinds of techniques, but for the used stress rods of panda type polarization-preserving fiber adopt MCVD or PCVD method (MCVD with the PCVD method main difference to provide the mode of thermal source different, can claim the CVD method) production.Mix B
2O
3The production of stress rods is adopted the interior sedimentation of CVD pipe as shown in Figure 1 more.B is mixed in sedimentation production in the CVD pipe at present
2O
3Stress rods is existent defect and deficiency also, and for example, the dimensions of deposited tube 104 has limited external diameter and the length of stress rods; Sedimentation rate is 2～3g/min, and production efficiency is lower; CVD technique head tube 106 ends and 107 tail pipe ends are mixed B
2O
3Prefabricated rods external diameter and doping content there are differences.In addition because B
2O
3Fusing point low and the deposited tube fusing point is higher, if doping content is higher, the molten contracting stage of deposited tube 104 is difficult to successfully.In order to overcome the problems referred to above, general CVD produces mixes B
2O
3The stress rods doping content is controlled at lower level, mixing B
2O
3Stress rods is equally divided into two sections to mate two holes (as shown in Figure 2) on female rod, obtains 307 stress rods after then these two sections stress rods being ground off skin by mechanical mill, again 307 stress rods is carried out mechanical polishing and grinds off surrounding layer.As shown in Figure 3, because mechanical grinding machine chuck 301 is only fixedly mixed B
2O
3One end of glass preform 304 is mixed B
2O
3Glass preform 304 is longer, and working accuracy is poorer, therefore can have a strong impact on the quality of stress rods.The CVD method is produced and is mixed B
2O
3The Production Flow Chart of prefabricated rods needs manual operation more as shown in Figure 4 in the course of processing, working accuracy is poor; Be subjected to the restriction of deposited tube size, the stress rods size is less, and the external diameter homogeneity is poor, and production efficiency is low.
The stress rods that the VAD method is produced in the panda type polarization-preserving fiber prefabricated rods has significant advantage, and than CVD, its uniform doping can design the stress rods of producing different levels of doping, and production efficiency is high, and external diameter and length such as can control according to demand at the advantage.(as shown in Figure 6) mixes B in the VAD production technique
2O
3Glass granules is deposition growing vertically.About 8～the 9g/min of the sedimentation rate of VAD is 3 times of CVD, and VAD production technique doping content is high than CVD, can realize Uniform Doped in 0wt% ~ 50wt% scope.Doping B
2O
3The glass granules prefabricated rods obtains the transparent B that mixes after by sintering
2O
3Prefabricated rods (as shown in Figure 7), annealed and extension process (such as Fig. 8 and shown in Figure 9) can design the stress rods of producing various outer diameter and design dissimilar panda type polarization-preserving fibers to satisfy again.The VAD method is produced mixes B
2O
3The prefabricated rods external diameter is than large 4 times of the production of CVD method, and OH removes comparatively abundant simultaneously.As shown in Figure 5, VAD method production doping B
2O
3The glass granules prefabricated rods can share sintering and stretcher with ordinary optic fibre glass granules prefabricated rods, has reduced a large amount of manual operationss when can reduce equipment investment.Owing to mix B
2O
3There is larger stress in glass, so mix B
2O
3Stress rods has strict demand to VAD, sintering, annealing and extension process parameter.
Summary of the invention
The purpose of this invention is to provide a kind of production and mix B
2O
3The method and apparatus of stress rods.The method and device production efficiency height, uniform doping, doping content scope are large, and the stress rods size can be carried out flexible design according to demand.
The invention provides a kind of production and mix B
2O
3The method of stress rods, the method may further comprise the steps:
Step (1) VAD method production doping B
2O
3Glass granules prefabricated rods, blowtorch 606 relative level angles are 25 degree～65 degree, and doping content is 28wt%, doping B
2O
3Glass granules prefabricated rods 604 external diameters＜100mm, speed of growth 1mm/min, density is 0.20-0.40g/cm
3, B finally mixes
2O
3Glass granules prefabricated rods 604 length 900～1000mm;
Step (2) is with doping B
2O
3Glass granules prefabricated rods 604 is put in the sintering oven, Cl
2Flow 0.8L/min, He flow 15L/min, dehydration temperaturre is 700 ℃-1000 ℃, and dewatering speed is 2～7mm/min, and temperature is 1200～1500 ℃ during sintering, and sintering velocity is 3～7mm/min, insulation is not less than 30min when being sintered to initiating terminal, then will mix B
2O
3Prefabricated rods is mentioned and being taken out after the cooling of muffle tube upper end is not less than 2 hours, places annealing furnace again;
Step (3) will be mixed B
2O
3Prefabricated rods is put in the holding furnace, then slowly is warmed up to 800-1000 ℃, slowly is down to room temperature after annealing time is not less than 5 hours and takes out and mix B
2O
3Prefabricated rods;
Step (4) will be mixed B
2O
3Be installed to extension device after the prefabricated rods welding, High Temperature Furnaces Heating Apparatus slowly is warming up to 1350-1450 ℃, and extension speed is made as 5-8mm/min, extends and finishes rear slow cooling.
Further, if need to stop in the extension process of step (4), High Temperature Furnaces Heating Apparatus is also wanted slow cooling.
The present invention also provides a kind of production to mix B
2O
3The device of stress rods, this device comprises:
Production doping B
2O
3Glass granules prefabricated rods device, this device comprises: draw bar 601, laser generator 602, initial excellent 603, laser 605, blowtorch 606 is used for spraying into hydrogen and oxygen 607, silicon tetrachloride and boron tribromide 608, laser pickoff 609, reaction casing 610 is used for discharging the outlet of thermochemistry gas 611;
Sintering oven comprises and draws bar 701, is positioned at the venting port 702 of sintering oven upper end, can hold and mix B
2O
3The muffle tube 703 of prefabricated rods, initial excellent 704, High Temperature Furnaces Heating Apparatus 706 is used for passing into the inlet end that is positioned at the sintering oven lower end 707 of chlorine and helium; Doping B
2O
3Insulation was not less than 30min when the glass granules prefabricated rods was sintered to initiating terminal, then will mix B
2O
3Prefabricated rods is mentioned and being taken out after the cooling of muffle tube upper end is not less than 2 hours;
Annealing furnace comprises and draws bar 801, and holding furnace 803 is positioned at the insulating pipe 804 of holding furnace inside;
Extension apparatus comprises and draws bar 901, and High Temperature Furnaces Heating Apparatus 904 is positioned at the temperature footpath instrument 905 of High Temperature Furnaces Heating Apparatus bottom.
Further, holding furnace slowly is warmed up to 800-1000 ℃, slowly is down to room temperature after annealing time is not less than 5 hours and takes out and mix B
2O
3Prefabricated rods.
Further, High Temperature Furnaces Heating Apparatus slowly is warming up to 1350-1450 ℃, and the extension speed of extension apparatus is made as 5-8mm/min, extends and finishes rear slow cooling.
Description of drawings
Fig. 1 is that CVD production is mixed B
2O
3The glass preform synoptic diagram.Wherein 101 is SiCl
4, 102 is boron tribromide, 103 is chuck, 104 are deposition, 105 for except ash pipe, 106 is head tube, 107 is tail pipe, 108 be blowtorch (MCVD) or etc. from generating hot body (PCVD), 109 temperature measurers, 110 thermal exhausts, 111 chemical exhausts.
Fig. 2 A is that CVD production is mixed B
2O
3One of cutting synoptic diagram of glass preform.Wherein 201 is the hand blowtorch, and 202 mix B
2O
3Glass preform.
Fig. 2 B is that CVD production is mixed B
2O
3Two of the cutting synoptic diagram of glass preform.Wherein 201 is the hand blowtorch, and 202 mix B
2O
3Glass preform.
Fig. 2 C is that CVD production is mixed B
2O
3Three of the cutting synoptic diagram of glass preform.Wherein 201 is the hand blowtorch, and 202 mix B
2O
3Glass preform.
Fig. 3 is that CVD production is mixed B
2O
3Glass preform surrounding layer grinding machine working method synoptic diagram.Wherein 301 is chuck, and 302 is wheel-guard, and 303 is emery wheel, and 304 mix B
2O
3Glass preform, 305 emery wheel bearings, 306 is mobile platform, 307 stress rods that process.
Fig. 4 is CVD production stress rods schema.
Fig. 5 is with the schema of VAD production stress rods according to the present invention.
Fig. 6 is VAD production doping B
2O
3Glass granules prefabricated rods synoptic diagram.Wherein 601 for drawing bar, and 602 is laser generator, and 603 is initial rod, and 604 are doping B
2O
3The glass granules prefabricated rods, 605 is laser, and 606 is blowtorch, and 607 is hydrogen and oxygen, and 608 is silicon tetrachloride and boron tribromide, 609 is laser pickoff, 610 reaction casings, 611 is the thermochemistry exhaust.
Fig. 7 is VAD production doping B
2O
3Glass granules prefabricated rods sintering synoptic diagram.Wherein 701 for drawing bar, and 702 is venting port, and 703 is muffle tube, and 704 is initial rod, and 705 are doping B
2O
3The glass granules prefabricated rods, 706 is High Temperature Furnaces Heating Apparatus, 707 is chlorine and helium inlet end.
Fig. 8 is doping B
2O
3Prefabricated rods annealing synoptic diagram.Wherein 801 for drawing bar, and 802 are doping B
2O
3Prefabricated rods, 803 holding furnaces, 804 is insulating pipe.
Fig. 9 is doping B
2O
3Prefabricated rods extension method synoptic diagram.Wherein 901 for drawing bar, and 902 has been rod, and 903 are doping B
2O
3Prefabricated rods, 904 is High Temperature Furnaces Heating Apparatus, and 905 is temperature footpath instrument, and 906 is stress rods.
Embodiment
The present invention will be further described below in conjunction with Figure of description and embodiment.
According to shown in Figure 5, be that the flow process of VAD production stress rods is implemented.
VAD explained hereafter doping B
2O
3Glass granules prefabricated rods (as shown in Figure 6), blowtorch 606 relative level angles are 25 degree～65 degree, are preferably 42 degree, and doping content is 28wt%, doping B
2O
3Glass granules prefabricated rods 604 external diameters＜100mm, speed of growth 1mm/min, density is 0.20-0.40g/cm
3, be preferably 0.28g/cm
3, B finally mixes
2O
3Glass granules prefabricated rods 604 length 900～1000mm.
With doping B
2O
3Glass granules prefabricated rods 604 is put into (as shown in Figure 7) in the sintering oven, Cl
2Flow 0.8L/min, He flow 15L/min, dehydration temperaturre is 700 ℃-1000 ℃, is preferably 800 ℃, dewatering speed is 2～7mm/min, is preferably 6mm/min; Temperature is 1200～1500 ℃ during sintering, is preferably 1320 ℃, and sintering velocity is 3～7mm/min, is preferably 6.5mm/min, and insulation is not less than 30min when being sintered to initiating terminal, and then 30min preferably for mixing B
2O
3Prefabricated rods is mentioned the cooling of muffle tube upper end and is not less than 2 hours, preferably takes out after 120 minutes, places annealing furnace again.
To mix B
2O
3Prefabricated rods is put in the holding furnace (being annealing furnace) (as shown in Figure 8), then slowly is warmed up to 800-1000 ℃, is preferably 800 ℃, and annealing time is not less than 5 hours, slowly is down to room temperature after being preferably 10 hours and takes out and mix B
2O
3Prefabricated rods.
To mix B
2O
3Be installed to extension device (as shown in Figure 9) after the prefabricated rods welding, 904 High Temperature Furnaces Heating Apparatuss slowly heat up, and extension is wanted slow cooling after finishing.If need to stop in the extension process, High Temperature Furnaces Heating Apparatus is also wanted slow cooling.Elongating temperature is made as 1350-1450 ℃, is preferably 1400 ℃, and extension speed is made as 5-8mm/min, is preferably 7.5mm/min, extends external diameter and is set as 10mm.
The present invention also provides a kind of production to mix B
2O
3The device of stress rods, this device comprises:
Production doping B
2O
3Glass granules prefabricated rods device, as shown in Figure 6, this device comprises: draw bar 601, laser generator 602, initial excellent 603, laser 605, blowtorch 606 is used for spraying into hydrogen and oxygen 607, silicon tetrachloride and boron tribromide 608, laser pickoff 609, reaction casing 610 is used for discharging the outlet of thermochemistry gas 611;
As shown in Figure 7, sintering oven comprises and draws bar 701, is positioned at the venting port 702 of sintering oven upper end, can hold and mix B
2O
3The muffle tube 703 of prefabricated rods, initial excellent 704, High Temperature Furnaces Heating Apparatus 706 is used for passing into the inlet end that is positioned at the sintering oven lower end 707 of chlorine and helium; Doping B
2O
3Insulation was not less than 30min when the glass granules prefabricated rods was sintered to initiating terminal, then will mix B
2O
3Prefabricated rods is mentioned and being taken out after the cooling of muffle tube upper end is not less than 2 hours;
As shown in Figure 8, annealing furnace comprises and draws bar 801, and holding furnace 803 is positioned at the insulating pipe 804 of holding furnace inside;
As shown in Figure 9, extension apparatus comprises and draws bar 901, and High Temperature Furnaces Heating Apparatus 904 is positioned at the temperature footpath instrument 905 of High Temperature Furnaces Heating Apparatus bottom.
Further, holding furnace slowly is warmed up to 800-1000 ℃, slowly is down to room temperature after annealing time is not less than 5 hours and takes out and mix B
2O
3Prefabricated rods.
Further, High Temperature Furnaces Heating Apparatus slowly is warming up to 1350-1450 ℃, and the extension speed of extension apparatus is made as 5-8mm/min, extends and finishes rear slow cooling.
The above, it only is exemplary embodiments of the present invention, be not that technical scope of the present invention is imposed any restrictions, any trickle modification, equivalent variations and modification that every foundation technical spirit of the present invention is made above enforcement all still belong in the technical scheme scope of the present invention.
Claims (5)
1. B is mixed in a production
2O
3The method of stress rods is characterized in that:
Step (1) VAD method production doping B
2O
3Glass granules prefabricated rods, blowtorch (606) relative level angle are 25 degree～65 degree, and doping content is 28wt%, doping B
2O
3Glass granules prefabricated rods (604) external diameter＜100mm, speed of growth 1mm/min, density is 0.20-0.40g/cm
3, B finally mixes
2O
3Glass granules prefabricated rods (604) length 900～1000mm;
Step (2) is with doping B
2O
3Glass granules prefabricated rods (604) is put in the sintering oven Cl
2Flow 0.8L/min, He flow 15L/min, dehydration temperaturre is 700 ℃-1000 ℃, and dewatering speed is 2～7mm/min, and temperature is 1200～1500 ℃ during sintering, and sintering velocity is 3～7mm/min, insulation is not less than 30min when being sintered to initiating terminal, then will mix B
2O
3Prefabricated rods is mentioned and being taken out after the cooling of muffle tube upper end is not less than 2 hours, places annealing furnace again;
Step (3) will be mixed B
2O
3Prefabricated rods is put in the holding furnace, then slowly is warmed up to 800-1000 ℃, slowly is down to room temperature after annealing time is not less than 5 hours and takes out and mix B
2O
3Prefabricated rods;
Step (4) will be mixed B
2O
3Be installed to extension device after the prefabricated rods welding, High Temperature Furnaces Heating Apparatus slowly is warming up to 1350-1450 ℃, and extension speed is made as 5-8mm/min, extends and finishes rear slow cooling.
2. method according to claim 1, it is characterized in that: if need to stop in the extension process of step (4), High Temperature Furnaces Heating Apparatus is also wanted slow cooling.
3. B is mixed in a production
2O
3The device of stress rods is characterized in that this device comprises:
Production doping B
2O
3Glass granules prefabricated rods device, this device comprises: draw bar (601), laser generator (602), initial rod (603), laser (605), blowtorch (606), be used for spraying into hydrogen and oxygen (607), silicon tetrachloride and boron tribromide (608), laser pickoff (609), reaction casing (610) is used for discharging the outlet of thermochemistry gas (611);
Sintering oven comprises and draws bar (701), is positioned at the venting port (702) of sintering oven upper end, can hold and mix B
2O
3The muffle tube of prefabricated rods (703), initial rod (704), High Temperature Furnaces Heating Apparatus (706) is for the inlet end that is positioned at the sintering oven lower end (707) that passes into chlorine and helium; Doping B
2O
3Insulation was not less than 30min when the glass granules prefabricated rods was sintered to initiating terminal, then will mix B
2O
3Prefabricated rods is mentioned and being taken out after the cooling of muffle tube upper end is not less than 2 hours;
Annealing furnace comprises and draws bar (801), and holding furnace (803) is positioned at the insulating pipe (804) of holding furnace inside;
Extension apparatus comprises and draws bar (901), and High Temperature Furnaces Heating Apparatus (904) is positioned at the temperature footpath instrument (905) of High Temperature Furnaces Heating Apparatus bottom.
4. device according to claim 3 is characterized in that:
Holding furnace slowly is warmed up to 800-1000 ℃, slowly is down to room temperature after annealing time is not less than 5 hours and takes out and mix B
2O
3Prefabricated rods.
5. device according to claim 4 is characterized in that:
High Temperature Furnaces Heating Apparatus slowly is warming up to 1350-1450 ℃, and the extension speed of extension apparatus is made as 5-8mm/min, extends and finishes rear slow cooling.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105543058A CN102976608A (en) | 2012-12-19 | 2012-12-19 | Method and device for producing diboron trioxide-doped stress rod |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105543058A CN102976608A (en) | 2012-12-19 | 2012-12-19 | Method and device for producing diboron trioxide-doped stress rod |
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| Publication Number | Publication Date |
|---|---|
| CN102976608A true CN102976608A (en) | 2013-03-20 |
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|---|---|---|---|
| CN2012105543058A Pending CN102976608A (en) | 2012-12-19 | 2012-12-19 | Method and device for producing diboron trioxide-doped stress rod |
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| CN (1) | CN102976608A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541102A (en) * | 2015-12-03 | 2016-05-04 | 富通集团有限公司 | Thermal stress relief process of prefabricated rod and thermal stress relief equipment thereof |
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|---|---|---|---|---|
| CN105541102A (en) * | 2015-12-03 | 2016-05-04 | 富通集团有限公司 | Thermal stress relief process of prefabricated rod and thermal stress relief equipment thereof |
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Application publication date: 20130320 |