CN1330597C - Method for preparing low hydroxy content optical-fiber precast rod by tubular CVD process - Google Patents
Method for preparing low hydroxy content optical-fiber precast rod by tubular CVD process Download PDFInfo
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- CN1330597C CN1330597C CNB2003101061112A CN200310106111A CN1330597C CN 1330597 C CN1330597 C CN 1330597C CN B2003101061112 A CNB2003101061112 A CN B2003101061112A CN 200310106111 A CN200310106111 A CN 200310106111A CN 1330597 C CN1330597 C CN 1330597C
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- 238000000034 method Methods 0.000 title claims abstract description 98
- 239000013307 optical fiber Substances 0.000 title claims abstract description 56
- 230000008569 process Effects 0.000 title claims description 52
- 125000002887 hydroxy group Chemical group [H]O* 0.000 title abstract description 17
- 229910052805 deuterium Inorganic materials 0.000 claims abstract description 108
- 239000007789 gas Substances 0.000 claims abstract description 105
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims abstract description 87
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000001257 hydrogen Substances 0.000 claims abstract description 66
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 66
- 229910052734 helium Inorganic materials 0.000 claims abstract description 53
- 239000001307 helium Substances 0.000 claims abstract description 52
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 52
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 34
- 238000005516 engineering process Methods 0.000 claims abstract description 33
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001301 oxygen Substances 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- 230000008021 deposition Effects 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000006467 substitution reaction Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 238000005137 deposition process Methods 0.000 claims description 23
- 238000005229 chemical vapour deposition Methods 0.000 claims description 19
- 238000000151 deposition Methods 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 230000000155 isotopic effect Effects 0.000 claims description 16
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 claims description 13
- 241000720974 Protium Species 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 150000002431 hydrogen Chemical class 0.000 claims description 12
- 238000006073 displacement reaction Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 230000002950 deficient Effects 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 4
- 238000005649 metathesis reaction Methods 0.000 claims description 3
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- 239000000567 combustion gas Substances 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 239000011737 fluorine Substances 0.000 claims 1
- 239000012159 carrier gas Substances 0.000 abstract 1
- 238000001947 vapour-phase growth Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 36
- 239000000835 fiber Substances 0.000 description 25
- 238000010521 absorption reaction Methods 0.000 description 20
- 238000005253 cladding Methods 0.000 description 7
- 238000007906 compression Methods 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 229910003902 SiCl 4 Inorganic materials 0.000 description 4
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- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229960001866 silicon dioxide Drugs 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000012792 core layer Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
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- 238000003860 storage Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- 229910020175 SiOH Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- 125000005843 halogen group Chemical group 0.000 description 1
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- RLOWWWKZYUNIDI-UHFFFAOYSA-N phosphinic chloride Chemical compound ClP=O RLOWWWKZYUNIDI-UHFFFAOYSA-N 0.000 description 1
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- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
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Abstract
The present invention relates to a method for preparing an optical fiber precast rod with low hydroxyl content in a tube by a chemical vapor phase deposition technology. A hydrogen isotope substitution technology is introduced into a conventional MCVD or PCVD technology. When an optical fiber precast rod is prepared by the MCVD method or the PCVD method, hydrogen elements in a base tube and a deposition layer are simultaneously substituted by using deuterium elements, and hydrogen elements in the base tube and the deposition layer are substituted by repeatedly and intermittently by using deuterium elements in the preparation process. The substitution method comprises: first, helium or nitrogen is led into the base tube to expel the oxygen in the base tube; then, the helium or nitrogen led into the base tube is stopped, and deuterium or a mixture of deuterium and helium starts to be led into the base tube, and substitutes hydrogen elements in a certain depth from the inner surface to the outside in the base tube; the deuterium led into the base tube is stopped, helium or nitrogen is led into the base tube to expel the mixture of hydrogen and deuterium, and the temperature starts to be raised; and then, the leading of the helium or the nitrogen is stopped, and carrier gas carrying raw materials and auxiliary gas start to be led into the base tube. By the method, optical fiber precast rods with low hydroxyl content and optical fibers with low hydroxyl content can be obtained.
Description
One, technical field
The present invention relates to a kind of interior chemical vapor deposition method of pipe that utilizes and make low hydroxy radical content preform in conjunction with the replacing process of hydrogen isotope, relate in particular to the method for the low hydroxy radical content preform of chemical vapor deposition process preparation in the pipes such as a kind of MCVD and PCVD, thereby obtain the processing method of low water peak or allwave fiber, belong to optical fiber and make the field.
Two, background technology
The optical wavelength that the silicon-dioxide single-mode fiber can transmit is subjected to the restriction of single-mode fiber cutoff wavelength (about 1260nm) at short wavelength's end, be subjected to the earth silicon material intrinsic of optical fiber own at long wavelength's end and absorb restriction, if operation wavelength surpasses 1650nm, far IR shielding effect loss during intrinsic absorbs will increase sharply, so the theory of single-mode fiber transmission wavelength region is the 390nm between 1260nm～1650nm.Usually we are divided into following four windows with the transmission spectrum of single-mode fiber: 1) 1280～1350nm, abbreviate the 1310nm window as, and also claim second wave band (windows2); 2) 1530nm～1560nm simply can be described as the 1550nm window, is also referred to as triband (windows3) or C-band; 3) 1560nm～1620nm is called the 4th wave band (window4) or L-band; 4) 1350～1530nm is also referred to as the 5th wave band (window5).But wavelength region commonly used at present has only about 1/3rd of this theoretical value, and this mainly is because the water absorption peak at 1385nm place causes.
There is the hydroxyl absorption peak in the silicon-dioxide single-mode fiber near the 1385nm wavelength, as long as have several ppb (parts per billion) hydroxyl just to be enough to cause near 1385nm, to produce several decibels decay at inside of optical fibre, make that decay is approximately 1dB/km in the wide frequency spectrum of about 100nm among 1350～1450nm, therefore the 5th wave band of this wide 180nm fails to utilize always, and use at present second, third, also 160nm only of the 4th wave band sum.If can manage to eliminate this water peak, then can make full use of the 5th wave band of optical fiber, realize all wave band utilization of silicon-dioxide single-mode fiber substantially.
For this reason, each company all is devoted to eliminate the hydroxyl absorption peak, exploitation " allwave fiber ".Except not having the water peak, all-wave fiber is the same with common standard G.652 matched clad optical fiber.Yet, owing to do not had water peak, optical fiber can open the 5th low damage transmission window, thus a series of benefits brought.
1) the wavelength available scope increases 100nm, be equivalent to 125 wavelength channel 100GHz channel spacings, make optical fiber that the wave band of the complete transmission from 1280nm to 1625nm can be provided, all the wavelength available scopes are made an appointment with half than the conventional fiber increase, and reusable number of wavelengths increases greatly.
2) because in above-mentioned wavelength region, CHROMATIC DISPERSION IN FIBER OPTICS only is half of 1550nm wavelength zone, thereby, realize the long Distance Transmission of high bit rate easily.For example near the 1400nm wavelength, the signal of 10Gbps speed can transmit 200km and need not dispersion compensation.
3) can distribute different business to give the wavelength transmission of suitable this business, improve network management.For example can in 1350～1450nm wavelength zone transmit high-speed signals (up to 10Gbps), transmit other signals in 1310nm wavelength zone transportation simulator picture signal at the above wavelength zone of 1450nm.
4) after the wavelength available scope is expanded greatly, allow and use wavelength interval broad, wavelength accuracy and lower light source, wave multiplexer, channel-splitting filter and other elements of stability requirement, make components and parts particularly the cost of passive device descend significantly, reduced the cost of total system.
For example, by increasing the wavelength interval, network can use the more cheap nothing direct modulated laser that freezes, and has avoided expensive externally modulated laser.For film filter, after the wavelength interval was increased to 200GHz from 100GHz, the wave filter cost can reduce about 50%, and after the wavelength interval further was increased to 400GHz, the wave filter cost can reduce about 70%.
Hydroxyl source in the optical fiber mainly comprises hydrogen or the hydroxyl impurity that processes such as optical fiber preparation, optical fiber cabling, optical cable installation and use are introduced.In actual applications, people are difficult to guarantee do not produce or do not contact hydrogen in the optical cable installation fully with the whole life period that uses.The defective reaction of hydrogen and optical fiber itself produces loss, is divided into two classes usually.The first kind is the loss of OH type, H-H reaction meeting formation SiOH and GeOH absorption peak in the residual amount of hydrogen that the whole life period of the installation of optical cable and use occurs and optical fiber between various silicon or the germanium defective, its centre wavelength is just at 1385nm, and this causes the fibre loss absorption peak to increase.Second class is the loss of SiH type, occurs in the 1530nm place, and often follows the OH absorption peak that the 1385nm place takes place to increase.At room temperature, the OH absorption peak of following of most SiH absorption peak and small portion can disappear behind several days or some months automatically, i.e. the loss increase that causes of SiH is temporary transient, and its hazardness is far away from the loss of OH type.Thereby the key of the good allwave fiber of design performance is: optical fiber need possess low hydroxy radical content and can not produce the loss of OH type because of the existence of hydrogen at subsequently whole life period.
In order to prevent that low hydroxy radical content optical fiber in use is subjected to the influence of hydrogen loss and increases the water peak, can adopt optical fiber is handled.This wherein just comprises the method for optical fiber being oozed deuterium, because the absorption spectral coverage of OD group is not in the opticfiber communication window ranges, therefore under certain processing condition, in glass optical fiber, penetrate into the D atom that finite concentration distributes gradually to internal layer by skin, the defective of itself and optical fiber itself is reacted, thereby make the external hydrogen atom in the optical fiber use be difficult to enter the defective locations of optical fiber, thereby just can avoid the generation of oh type loss.
With respect to optical fiber is handled the increase that prevents hydrogen loss by deuterate for, low hydroxy radical content optical fiber then is the prerequisite of low water peak of preparation or allwave fiber, low hydroxy radical content optical fiber then derives from low hydroxy radical content preform, promptly require the prefabricated rods sandwich layer with must be very low near hydroxy radical content in the covering in the sandwich layer certain thickness.This has just proposed harsh requirement to the preparation of preform.For technologies such as OVD, VAD, by can easier make the preform of low hydroxy radical content before the sintering to the deshydroxy technology of loose body, but for chemical vapor deposition process in the pipes such as MCVD, PCVD, owing in sedimentary process, promptly realized the sintering of loose body, can not adopt the deshydroxy technology of technologies such as being similar to OVD and VAD, the hydroxyl in the vitreum behind the sintering is to be difficult to get rid of.Therefore, the Perfected process of the low hydroxy radical content preform of chemical vapor deposition process preparation is not introduce hydrogen or hydroxyl in guaranteeing production process in the pipes such as MCVD and PCVD, perhaps promptly carries out deshydroxy and handle in deposition process successively.
The main source of OH comprises following aspect in the optical fiber that chemical vapor deposition process prepares in the pipes such as MCVD: the one, and the moisture that hydrogen containing foreign in the optical fiber preparation raw material and reactant gases are brought into; The 2nd, a small amount of OH of deposition parent tube itself at high temperature spreads to fiber core layer; The 3rd, owing to the system sealing performance causes the aqueous vapor in the environment to enter reaction compartment inadequately, comprise the pollution of oxyhydrogen flame in the MCVD technological process.
MCVD and PCVD technology are raw materials used mainly to be halogenide, as SiCl
4, GeCl
4Deng.SiCl
4In main hydrogen containing foreign be trichlorosilane (SiHCl
3).SiHCl
3Can be eliminated by repeatedly distilling, but SiCl
4In also contain other hydrogen containing foreign such as HCl, CH
4And H
2O etc., these impurity have caused the pollution of OH in the optical fiber just.Therefore the hydrogen containing foreign concentration in the necessary strict control raw material generally is controlled in the 0.5ppm.Hydrogen containing foreign in halid current-carrying gas such as the oxygen also is a major reason that causes hydroxyl contamination, in order to remove water vapour wherein, must carry out multistage purifying to gas.Simultaneously, the sealing property of total system also is crucial, and this comprises that the junction of all gas pipeline, mass rate take into account positions such as magnetic valve, and the swivel joint that particularly deposits parent tube raw material input terminus causes the major reason of leakage especially.
In deposition and molten compression process, the OH that parent tube itself is contained can be diffused in the settled layer.It is estimated that before becoming rod, its diffusion length reaches and is about 40-50 μ m.So, enter the sandwich layer position in order to prevent OH, before the sandwich layer deposition, stopping of adequate thickness of deposition is very necessary earlier.Reduce depositing temperature and the molten temperature that contracts and also help to reduce in the parent tube OH to the diffusion of sandwich layer.But above-mentioned two kinds of methods all can reduce sedimentation rate, have prolonged depositing time, have increased production cost.
After adopting high pure raw material, high-purity gas and doped capillary tube optical fibre, the hydroxy radical content in the optical fiber can be well controlled, but still is difficult to reach allwave fiber is lower than 0.31dB/km in the loss of 1385nm place requirement.
Three, summary of the invention
The purpose of this invention is to provide a kind of method that reduces hydroxy radical content in the parent tube of managing interior chemical vapor deposition process.Second purpose of the present invention provides a kind of method that reduces hydroxy radical content in interior chemical vapor deposited prefabricated rods inner cladding of pipe and the sandwich layer, especially the technology of hanging down hydroxy radical content in interior chemical vapor deposited prefabricated rods inner cladding of pipe such as MCVD and PCVD and the sandwich layer.The 3rd purpose of the present invention provides the method for the fully low hydroxy radical content preform of chemical vapor deposition in a kind of pipe.The 4th purpose of the present invention provides the method that chemical vapor deposition hangs down water peak or allwave fiber fully in a kind of pipe.
In order to achieve the above object, in traditional MCVD technology and PCVD technology, introduce the hydrogen isotope replacing process, when being equipped with preform, MCVD method and PCVD legal system utilize the protium in deuterium element substitution parent tube and the settled layer, making the most of OH groups converted in the final preparation prefabricated rods is the OD group, reduce the hydroxy radical content in the prefabricated rods, thereby the absorption loss that makes optical fiber be positioned at 1385nm reduces, and obtains low-water-peak fiber or allwave fiber.
Purpose of the present invention realizes like this: the method for the low hydroxy radical content preform of chemical vapor deposition process preparation in the pipe, in traditional MCVD or PCVD technology, introduce the hydrogen isotope replacing process, when being equipped with preform, MCVD or PCVD legal system utilize the protium in deuterium element substitution parent tube and the settled layer, and be that alternative repeatedly when beginning to prepare and in the preparation process utilizes the protium in deuterium element substitution parent tube and the settled layer, method of replacing is: the helium or the nitrogen that feed certain flow earlier in parent tube, keep certain hour to drive away the inner oxygen that exists of parent tube, then parent tube is heated to the needed suitable temp of hydrogen deuterium exchange, stop in pipe, to feed helium or nitrogen, beginning is with the certain flow velocity feeding deuterium gas or the mixed gas of deuterium gas and helium, and the displacement parent tube is by the protium in the outside certain depth of internal surface; Stop to feed deuterium gas, the helium or the nitrogen flooding that feed certain flow rate in pipe are removed hydrogen and deuterium oxygen mixture in the pipe, and the beginning elevated temperature; Stop the input of helium or nitrogen behind the certain hour, begin to feed the delivering gas and the assist gas that carry raw material and deposit.
The needed suitable temp of hydrogen deuterium exchange is generally at 300-1100 ℃, and the metathetical number of times is decided on the control of technology and deposition process parameters and size repeatedly in deposition process, generally at 2-10 time.Feed helium or nitrogen when driving away residual gas and keep certain hour, generally at 2-20 minute.
The present invention is applied to hydrogen-deuterium exchange principle chemical vapor deposition process in the pipes such as MCVD and PCVD exactly, by hydrogen-deuterium exchange (as shown in the formula) make the OH group of positions such as prefabricated rods sandwich layer, inner cladding and parent tube whole or most change the OD group into, thereby the absorbed wavelength is moved on to beyond the communication window, thereby the low hydroxy radical content preform of preparation.
As can be seen from Table 1, after hydrogen-deuterium exchange, formerly be positioned at vibration that the opticfiber communication window produces big absorption loss corresponding to O-H and all be displaced to beyond the communication window, like this, the absorption loss that optical fiber is positioned at the 1385nm place reduces greatly.
The harmonic vibration of OH in table 1 quartz glass network and OD correspondence
| O-H bond wavelength (nm) OH key resonance wavelength | Identification microcosmic correspondence | Intensity intensity (dB/km ppm) | O-D bond wavelength (nm) OD key resonance wavelength |
| 2730 | v′ 3 | ≌10,000 | 3750 |
| 2220 | v 1+v′ 3 | 256.500 | 3050 |
| 1900 | 2v 1+v′ 3 | 90.060 | 2610 |
| 1380 | 2v′ 3 | 40.278 | 1895 |
| 1240 | v 1+2v′ 3 | 2.083 | 1700 |
| 1125 | 2v 1+2v′ 3 | 0.047 | 1545 |
| 1030 | 3v 1+2v′ 3 | 0.006 | 1410 |
| 940 | 3v′ 3 | 1.000 | 1290 |
| 880 | v 1+3v′ 3 | 0.092 | 1210 |
| 825 | 2v 1+3v′ 3 | 0.011 | 1135 |
| 775 | 3v 1+3v′ 3 | 0.001 | 1065 |
| 725 | 4v′ 3 | 0.089 | 995 |
| 685 | v 1+4v′ 3 | 0.012 | 940 |
| 585 | 5v′ 3 | 0.007 | 805 |
O-D key bond energy is 466kJ/mol, and O-H key bond energy is 460466kJ/mol, therefore utilizes the certain excitation energy of process need of deuterium exchange hydrogen.If utilize the mode of heat that this excitation energy is provided, need can obtain displacement efficiency preferably in temperature more than 300 ℃.
Simultaneously, D
2With H
2All be a kind of inflammable gas, work as H
2, D
2Perhaps when both mixed gass and oxygen mix, hydrogen molecule or deuterium molecules a large amount of in the mixed gas fully contact with oxygen molecule, light back reaction rapidly, emit a large amount of heat in the short period of time at the utmost point.If gas is limited in the confined spaces, gas sharply expands, and just blasts.Under the normal temperature and pressure, if sneak into the 4%-74.2% that the volume of hydrogen reaches cumulative volume in the air, will explode when lighting, this scope is called the limits of explosion of hydrogen.Therefore, in hydrogen deuterium isotopic process, must avoid hydrogen or deuterium gas and oxygen mix, perhaps avoid its content to enter the hydrogen explosion limit.
The method that the present invention prepares low water peak or allwave fiber prefabricated rods comprises the steps:
1) will be fixed on the anchor clamps through the doped capillary tube optical fibre of clean, and the quartzy parent tube that utilizes the thermals source such as oxyhydrogen flame that laterally move to rotate is heated to high temperature, in parent tube, feeds Cl
2, SF
6Deng gas the parent tube internal surface is carried out chemical etching, remove the impurity on the parent tube internal surface;
2) reduce the parent tube temperature, and in parent tube, feed the helium or the nitrogen of certain flow, keep certain hour so that drive away the inner oxygen that exists of parent tube, then parent tube is heated to the needed suitable temp of hydrogen deuterium exchange, stop in pipe, to feed helium or nitrogen, beginning is with the certain flow velocity feeding deuterium gas or the mixed gas of deuterium gas and helium, and the displacement parent tube is by the protium in the outside certain depth of internal surface;
3) stop to feed deuterium gas, the helium or the nitrogen flooding that feed certain flow rate in pipe are removed hydrogen and deuterium oxygen mixture in the pipe, and the beginning elevated temperature; Stop the input of helium or nitrogen behind the certain hour, begin to feed the delivering gas and the assist gas that carry raw material, enter the deposition process of prefabricated rods;
When 4) finishing the settled layer of certain number of plies, stop to feed the delivering gas and the oxygen that carry raw material, and begin to lower the temperature, in parent tube, feed the helium or the nitrogen of certain flow rate simultaneously, keep certain hour so that drive away the oxygen that exists in the pipe,, stop in pipe, to feed helium or nitrogen when parent tube is heated to the needed suitable temp of hydrogen deuterium exchange, beginning is with the certain flow velocity feeding deuterium gas or the mixed gas of deuterium gas and helium, and settled layer is by the protium in the outside certain depth of internal surface in the displacement pipe;
5) after the isotopic process of setting is finished, according to 3) to 4) program loop carry out deposition process and the isotopic replacement process of hydrogen deuterium, up to finishing deposition process;
6) after deposition process is finished, directly on the MCVD lathe, melt and contract, perhaps transfer to melt on the special sintering oven and contract.Can continue to pipe in feed the GeCl of certain flow for fear of the volatilization of central core germanium this moment
4With O
2, perhaps feed fluoro-gas central core etched away.In a kind of technology in back, also can introduce the isotopic replacement process of hydrogen deuterium.
Simultaneously, present method is applicable to that also the PCVD prepared hangs down the hydroxy radical content preform.Similar with MCVD technology, PCVD technology also is to carry out vapour deposition and high temperature oxidation reaction in the purity quartz glass pipe for high pipe, and institute's difference is thermal source and reaction mechanism.PCVD technology is to have changed the oxyhydrogen flame type of heating in the MCVD method into microwave heating.In the PCVD deposition process, also can be the same to above-mentioned improved MCVD technology, in deposition process, increase hydrogen deuterium isotopic process with certain interval.Directly on lathe, do not continue molten compression process after the PCVD deposition process is finished, contract but deposited tube transferred to melt in the special sintering oven, and also can introduce hydrogen deuterium exchange process in this process with the H-O content in the minimizing plug central core.
Utilize aforesaid method, can obtain the very low preform of hydroxy radical content, and then draw the optical fiber that obtains low hydroxy radical content.Investigate the hydrogen loss situation of optical fiber subsequently.Find in the test, at room temperature silica-based optical fibers is exposed to 0.01 hydrogen-pressure after following 4 days, different fiber types presents different characteristics, the absorption loss of the optical fiber of MCVD method and VAD manufactured at the 1385nm place increases less than 0.01dB/km, the approximately average 0.04dB/km of increasing of the no OH optical fiber that utilizes blended VAD process to make, and the absorption loss increase of other types optical fiber is all apparent in view, and scope is roughly at 0.06～0.21dB/km.As seen, behind the optical fiber cabling of MCVD method preparation the absorption loss increase at 1385nm place in use very little, its 1385nm place absorption loss should be mainly derived from hydrogen or the hydroxyl contamination in the optical fiber preparation process.Therefore, hydrogen or hydroxyl contamination by in control or the elimination optical fiber preparation process just might be prepared into low water peak or allwave fiber.
Compare by prefabricated rods finished product or optical fiber finished product are handled the method that reduces optical fiber water peak again with some, present method has made full use of the processing unit and the technological merit of MCVD method and PCVD method, thereby not only having reduced H-O content in the parent tube can stop in covering in prefabricated rods preparation process and the fiber draw process or the parent tube hydroxyl to the diffusion of fiber core layer portion more effectively, simultaneously owing to reduced prefabricated rods inner cladding and the interior hydroxy radical content of sandwich layer, thereby the absorption peak that makes optical fiber be positioned at the 1385nm place reduces even reaches the state at anhydrous peak, and can keep secular stability.
Other features and advantages of the present invention will be described in more detail below, and can be by below in conjunction with becoming obvious in the description of the drawings book and the claims.
Should be appreciated that above general introduction and following detailed all are illustrative and illustrative, be intended to the present invention is illustrated further that not wanting has any restriction to the protection scope of the present invention that goes out appended power specification sheets qualification.
Four, description of drawings
Fig. 1 illustrates that utilization MCVD makes the traditional method of preform
Fig. 2 explanation uses MCVD to make the method for low water peak or allwave fiber prefabricated rods according to the present invention
The storage purification system of deuterium gas and delivery system 1, seal swivel joint 2, doped capillary tube optical fibre 3, blowtorch 4, heating zone, sedimentary province.
Five, embodiment
The method of common MCVD prepared preform is as shown in Figure 1: earlier in pure quartzy parent tube inside from inwall to center deposition covering and sandwich layer, will deposit silica glass molten solid plug that shortens under 2100-2300 ℃ of high temperature of sandwich layer then.In order to increase hydrogen deuterium exchange technology, need do to a certain degree improvement in common MCVD lathe and technology.
The present invention does corresponding the improvement on traditional MCVD technology, its embodiment is according to as shown in Figure 2 technology and device.
Increase the storage purification system and the delivery system 1 of deuterium gas in the inlet end front of common MCVD lathe.Deuterium gas after the purification enters silica tube inside on the MCVD lathe by its delivery system, by the flow of accurate mass flowmeter control deuterium gas.The concrete conveying and the mode of connection of deuterium gas can have multiple: a kind of method is that deuterium gas can be connected to deposition parent tube head seal swivel joint 2 places by independent delivery system; Another kind method is at first needed helium in deuterium gas and the MCVD deposition process to be mixed mutually, enter the inner replacement(metathesis)reaction of participating in of parent tube by seal swivel joint 2 together by the helium delivery system then, but the flow of deuterium gas still needs independent control, promptly when MCVD or PCVD deposition process are being carried out, deuterium gas will be closed and not enter the helium delivery system.
In the actual production, at first select the doped capillary tube optical fibre 3 of suitable dimension for use, utilize chemical such as distilled water, HF its internal surface to be cleaned and drying according to the setting of optical fibre refractivity section design and processes parameter.Parent tube 3 is installed on the MCVD depositing lathe, and two ends are fixed in the swivel joint 2, utilize motor to drive the parent tube rotation, light blowtorch 4 heating parent tubes then, the transverse movement of blowtorch parent tube length direction.Check whether parent tube exists defective, and the feeding fluoro-gas carries out etching to its internal surface in parent tube, removes the impurity on the internal surface.
Reduce the temperature of parent tube 3 subsequently, in parent tube 3, feed the helium or the nitrogen of certain flow (as 500-10000mL/ minute) simultaneously and keep certain hour (as 3-10 minute) so that drive away the inner oxygen that exists of parent tube, then parent tube 3 is heated to the hydrogen deuterium exchange and reacts needed suitable temp (between 300 ℃-1000 ℃), stop in pipe, to feed separately helium or nitrogen, beginning feeds the mixed gas (deuterium gas effective discharge is between 20mL/ minute-1000mL/ minute) of deuterium gas or deuterium gas/helium with certain flow (20mL/ minute-1000mL/ minute between), maintain in certain positive pressure scope by gas near the pressure equaliser holding tube the tail pipe simultaneously, begin the parent tube internal layer is carried out the isotopic heat exchange of hydrogen deuterium.Whole exchange process comprises following content: 1) absorption, infiltration and the diffusion of deuterium gas in quartzy network; 2) hydrogen-deuterium isotropic substance heat exchange; 3) hydrogen spreads and overflows.Flow, pipe internal pressure, temperature of reaction and reaction times by adjustment deuterium gas can be controlled the deuterium impervious degree of depth and exchange efficiency, and processing parameters such as the flow of deuterium gas, pipe internal pressure, temperature of reaction and reaction times are then according to the hydroxy radical content in the parent tube, inner cladding and the settings such as (b/a) of sandwich layer radius ratio.Simultaneously, for fear of temperature reduce with pipe in the pipe afterbody may exist during the gaseous tension conversion steam enter in the pipe, can be in pipe in the process of hydrogen deuterium exchange the Cl of feeding certain flow
2Gas.
To parent tube carry out deuterate handle reach the process goal requirement after, stop to feed deuterium gas, in pipe, feed the helium or the nitrogen of certain flow (as 500-10000mL/ minute) and keep certain hour (as 3-10 minute), begin elevated temperature simultaneously so that drive away hydrogen and deuterium oxygen mixture in the pipe.Stop the independent input of helium or nitrogen behind the certain hour, begin to enter the deposition process of prefabricated rods, a series of gas chemistry mixture (SiCl
4, GeCl
4, POCl
3Deng) under the drive of current-carrying oxygen, by bubble systems (Bubbler), and by accurate mass flow controller dominant discharge and some other reactant gases (He, Cl
2And O
2Deng), chemical reaction takes place in unstripped gas in the heating zone under 1400-1900 ℃ of left and right sides temperature of oxyhydrogen flame, produces particulate.The particulate that generates moves along the heat transfer fluid flow direction, is lower than to temperature in the sedimentary province of Heating Zone Temperature in thermophoretic forces effect deposit, forms settled layer.Along with moving of blowtorch 4, the settled layer that has just generated is sintered gradually, forms transparent glass coating.Like this one time one time deposition repeatedly, the settled layer progressive additive.
Hydrogen deuterium isotopic in beginning settled layer after the deposition process of finishing certain number of plies, this settled layer quantity at interval is by the final hydroxy radical content that requires of H-O content, prefabricated rods of corresponding these layers position in the traditional technology prefabricated rods, factors such as the hydrogen deuterium exchange process system decision of employing, and considers corresponding production rate and production efficiency.Before hydrogen deuterium isotopic process begins, stop in pipe, to feed current-carrying oxygen and other reactant gases that carries raw material, and begin to lower the temperature, feed the helium or the nitrogen of certain flow (as 500-10000mL/ minute) in the changed course pipe simultaneously and keep certain hour (as 3-10 minute) so that drive away the oxygen that exists in the pipe, when being heated to the needed suitable temp of hydrogen deuterium exchange (between 300 ℃-1000 ℃), parent tube stops in pipe, to feed separately helium or nitrogen, beginning feeds the mixed gas (deuterium gas effective discharge is between 20mL/ minute-1000mL/ minute) of deuterium gas or deuterium gas/helium with certain flow, maintains in certain positive pressure scope by gas near the pressure equaliser holding tube the tail pipe simultaneously.After deuterium gas enters in the pipe, under the energy that temperature provides to settled layer and the glass coating infiltration and the displacement protium wherein that generate by the settled layer sintering, the hydrogen that obtains after the displacement and fail to participate in the deuterium gas of replacement(metathesis)reaction along with tail gas such as helium enter exhaust collection and treatment system together.According to the absorption intensity requirement at the needed 1385nm of optical fiber designs place, adjust the effective discharge of deuterium gas in conjunction with the information such as variation of hydroxy radical content, inner cladding and sandwich layer radius ratio (b/a), deposit thickness in parent tube thickness, the parent tube.Simultaneously, for fear of temperature reduce with pipe in the pipe afterbody may exist during the gaseous tension conversion steam enter in the pipe, can be in pipe in the process of hydrogen deuterium exchange the Cl of feeding certain flow
2Gas.
After the isotopic process of setting is finished, stop to feed deuterium gas, in pipe, feed the helium or the nitrogen of certain flow rate (as 500-10000mL/ minute) and keep certain hour (especially better), to begin elevated temperature simultaneously so that drive away hydrogen and deuterium oxygen mixture remaining in the pipe with 3-10 minute.Stop helium then or nitrogen is imported separately, begin to feed the current-carrying oxysome and other reactant gases that carry raw material once more, proceed the deposition process of prefabricated rods.
According to certain time interval or deposition number of plies interval, carry out prefabricated rods deposition process and the isotopic replacement process of hydrogen deuterium repeatedly, until finish deposition process.When prefabricated rods inner cladding and sandwich layer all deposit finish after, carry out the isotopic replacement process of hydrogen deuterium again one time, then after driving away hydrogen and deuterium gas remaining in the pipe, pipe is carried out high temperature melts and contract with helium.Increase blowtorch 4 internal combustion gas flows, improve Heating temperature, make silica tube molten contracting under 2100-2300 ℃ of high temperature, and final preform or the prefabricated rod mandrel of closed formation.Perhaps the pipe that deposition is finished is transferred to melt in the special sintering oven and is contracted.
In molten compression process, the GeO in the tube hub layer
2Can produce volatilization under high temperature action, thereby make the prefabricated rod mandrel refractive index of the centre be lower than the expection specific refractory power, this refractive index of the centre depressed phenomenon will directly influence optical fiber property.In order to reduce or to eliminate this influence, can in molten compression process, continue in pipe, to feed and contain certain flow GeCl
4Current-carrying oxygen and other reactant gases, continue at central core deposition GeO
2, promptly mend core; Perhaps in molten compression process, in pipe, feed the fluoro-gas of certain flow, the center deposition layer is etched away.In etching technics, can feed the deuterium gas or the deuterium gas/helium mix gas of certain flow simultaneously, continue hydrogen deuterium isotopic process.
The process that the PCVD legal system is equipped with preform is similar to the MCVD method, but every layer of settled layer is thinner in the PCVD technology, and it is more always to deposit the number of plies.The method of introducing hydrogen deuterium exchange operation in PCVD technology is identical with MCVD technology, in parent tube etching and deposition process, can intermittent introducing deuterium gas or contain the mixed gas of deuterium gas, different is, must continual introducing in the PCVD technology be used to produce the energizing gas (as helium) of plasma body.Simultaneously, molten compression process in the PCVD technology is not finished on the PCVD lathe continuously, contract but after deposition is finished, pipe transferred to melt in the special sintering oven, in this molten compression process, also can in fully closed as yet pipe, feed deuterium gas or contain the mixed gas of deuterium gas, to reduce the H-O content at tube hub position by specialized system.
By aforesaid method, can obtain very low prefabricated rods of hydroxy radical content or prefabricated rod mandrel.Utilize method cleaning prefabricated rods surfaces such as high temperature polishing or hydrofluoric acid clean subsequently, obtain high-quality prefabricated rods finished product, perhaps obtain prefabricated rod mandrel and utilize outsourcing technologies such as OVD, tiretube process to increase prefabricated rods surrounding layer thickness.
As mentioned above, according to concrete scheme of the present invention, in MCVD technology or PCVD technology, introduce hydrogen-deuterium isotopic process, can effectively reduce the hydroxy radical content that parent tube is interior and settled layer is interior of preform (perhaps plug), reduced the absorption loss of optical fiber at the 1385nm place.
From described the present invention, clearly can also many kinds of modes change, these change and should not be considered to break away from the spirit and scope of the present invention, all such modifications are conspicuous for those skilled in the art, and they will be included within the scope of claims.
Claims (8)
1, the method of the low hydroxy radical content preform of chemical vapor deposition process preparation in the pipe, it is characterized in that in traditional MCVD or PCVD technology, introducing the hydrogen isotope replacing process, when being equipped with preform, MCVD or PCVD legal system utilize the protium in deuterium element substitution parent tube and the settled layer, and be when beginning to prepare and deposition is alternately utilized protium in quartzy parent tube of deuterium element substitution and the settled layer in the preparation process, the displacement number of times is 2-10 time, method of replacing is: feed 500-10000mL/ minute helium or nitrogen earlier and keep the 2-20 minute inner oxygen that exists of expeling parent tube in parent tube, then parent tube is heated to the needed 300-1100 of hydrogen deuterium exchange ℃ temperature, stop in pipe, to feed helium or nitrogen, begin to feed the mixed gas of 20mL/ minute-1000mL/ minute deuterium gas or deuterium gas and helium, the displacement parent tube is by the protium in the outside certain depth of internal surface; Stop to feed deuterium gas, the helium or the nitrogen flooding that fed in pipe 500-10000mL/ minute are removed hydrogen and deuterium oxygen mixture in the pipe; Stop the input of helium or nitrogen after 3-10 minute, begin to feed the delivering gas and the assist gas that carry raw material and be prepared growth again.
2, the method for hanging down the hydroxy radical content preform by chemical vapor deposition process preparation in the described pipe of claim 1, it is characterized in that concrete grammar is: 1) will be fixed to through the doped capillary tube optical fibre of clean on the anchor clamps, and the quartzy parent tube that utilizes the oxyhydrogen flame thermal source that laterally moves to rotate is heated to high temperature, feeds Cl in parent tube
2, SF
6Gas carries out chemical etching to the parent tube internal surface, removes the impurity on the parent tube internal surface; 2) reduce the parent tube temperature, and in parent tube, feed 500-10000mL/ minute helium or nitrogen and keep the 2-20 minute inner oxygen that exists of expeling parent tube, then parent tube is heated to the needed 300-1100 of hydrogen deuterium exchange ℃, stop in pipe, to feed helium or nitrogen, beginning feeds the mixed gas of deuterium gas or deuterium gas and helium with the flow velocity of 20mL/ minute-1000mL/ minute, replaces parent tube by the protium in the outside certain depth of internal surface; 3) stop to feed deuterium gas, the helium or the nitrogen flooding that feed certain flow rate in pipe are removed hydrogen and deuterium oxygen mixture in the pipe, and the beginning elevated temperature; Stop the input of helium or nitrogen after 3-10 minute, begin to feed the delivering gas and the assist gas that carry raw material, enter the deposition process of prefabricated rods; When 4) finishing the settled layer of certain number of plies, stop to feed the delivering gas and the assist gas that carry raw material, and begin to lower the temperature, in parent tube, feed 500-10000mL/ minute helium or nitrogen simultaneously and keep driving away in 2-20 minute the oxygen that exists in the pipe, when parent tube is heated to the needed 300-1100 of hydrogen deuterium exchange ℃, stop in pipe, to feed helium or nitrogen, beginning is with the mixed gas of 20mL/ minute-1000mL/ minute feeding deuterium gas or deuterium gas and helium, and settled layer is by the protium in the outside certain depth of internal surface in the displacement pipe; 5) after the isotopic process of setting is finished, according to 3) to 4) program loop carry out deposition process and the isotopic replacement process of hydrogen deuterium, up to finishing deposition process; 6) after deposition process is finished, directly on the MCVD lathe, melt and contract, perhaps transfer to melt on the special sintering oven and contract.
3, by the method for the low hydroxy radical content preform of chemical vapor deposition process preparation in the described pipe of claim 2, feed fluoro-gas when it is characterized in that molten contracting central core is etched away, also introduce the isotopic displacement of hydrogen deuterium simultaneously.
4,, it is characterized in that deuterium gas is connected to deposition parent tube head seal swivel joint (2) by independent delivery system and locates by the method for the low hydroxy radical content preform of chemical vapor deposition process preparation in claim 1 or the 2 described pipes.
5, the method for hanging down the hydroxy radical content preform by chemical vapor deposition process preparation in the described pipe of claim 1, the mode of movement that it is characterized in that deuterium gas be deuterium gas with MCVD or PCVD deposition process in needed helium mix mutually, enter the inner participation of parent tube replacement(metathesis)reaction by seal swivel joint (2) together by the helium delivery system then, but the flow of deuterium gas or independent control.
6, the method for hanging down the hydroxy radical content preform by chemical vapor deposition process preparation in the described pipe of claim 1, it is characterized in that deuterium gas effective discharge is between 20mL/ minute-1000mL/ minute, the flow of helium or nitrogen is at 500-10000mL/ minute, and keeps 3-10 minute.
7, the method for hanging down the hydroxy radical content preform by chemical vapor deposition process preparation in the described pipe of claim 1, it is characterized in that selecting for use the doped capillary tube optical fibre (3) of suitable dimension, utilize distilled water, HF chemical its internal surface to be cleaned and drying, parent tube (3) is installed on the MCVD depositing lathe, two ends are fixed in the swivel joint (2), utilize motor to drive the parent tube rotation, light blowtorch (4) heating parent tube then, the transverse movement of blowtorch parent tube length direction; Check whether parent tube exists defective, and the feeding fluorine gas carries out etching to its internal surface in parent tube, removes the impurity on the internal surface; Use the certain thickness protium of deuterium element substitution parent tube internal layer then.
8, the method for hanging down the hydroxy radical content preform by chemical vapor deposition process preparation in the described pipe of claim 1, it is characterized in that after settled layer is finished in the prefabricated rods, increase blowtorch (4) internal combustion gas flow, improve Heating temperature, silica tube is at high temperature melted to contract, and closed final preform, the deuterium gas of feeding certain flow in this process of forming.
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| CNB2003101061112A CN1330597C (en) | 2003-10-21 | 2003-10-21 | Method for preparing low hydroxy content optical-fiber precast rod by tubular CVD process |
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| CNB2003101061112A CN1330597C (en) | 2003-10-21 | 2003-10-21 | Method for preparing low hydroxy content optical-fiber precast rod by tubular CVD process |
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| CN1330597C true CN1330597C (en) | 2007-08-08 |
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| CN102621629B (en) * | 2012-04-11 | 2014-02-12 | 江苏法尔胜光子有限公司 | A kind of 980 optical fiber for coupler and its production method |
| CN103359927A (en) * | 2013-07-22 | 2013-10-23 | 中国科学院西安光学精密机械研究所 | Doping device and doping method for optical fiber preform |
| CN111056740B (en) * | 2020-01-13 | 2023-09-12 | 成都翱翔拓创光电科技合伙企业(有限合伙) | A device and method for preparing active optical fiber preforms by PCVD method |
| CN111116038A (en) * | 2020-01-13 | 2020-05-08 | 成都翱翔拓创光电科技合伙企业(有限合伙) | Gas phase doping device and method for preparing rare earth doped optical fiber preform |
| CN115747743B (en) * | 2022-12-20 | 2023-11-28 | 安徽纯源镀膜科技有限公司 | Workpiece coating and high-temperature deuterium permeation equipment and process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4504297A (en) * | 1983-07-06 | 1985-03-12 | At&T Bell Laboratories | Optical fiber preform manufacturing method |
| WO2001047822A1 (en) * | 1999-12-28 | 2001-07-05 | Corning Incorporated | Low water peak optical waveguide and method of manufacturing same |
| US20030084684A1 (en) * | 2001-10-19 | 2003-05-08 | Jds Uniphase Corporation | Method of reducing a hydrogen content of an optical fiber or preform |
-
2003
- 2003-10-21 CN CNB2003101061112A patent/CN1330597C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4504297A (en) * | 1983-07-06 | 1985-03-12 | At&T Bell Laboratories | Optical fiber preform manufacturing method |
| WO2001047822A1 (en) * | 1999-12-28 | 2001-07-05 | Corning Incorporated | Low water peak optical waveguide and method of manufacturing same |
| US20030084684A1 (en) * | 2001-10-19 | 2003-05-08 | Jds Uniphase Corporation | Method of reducing a hydrogen content of an optical fiber or preform |
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