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CN110066122A - The manufacturing method of optical fiber - Google Patents

The manufacturing method of optical fiber Download PDF

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Publication number
CN110066122A
CN110066122A CN201910067902.XA CN201910067902A CN110066122A CN 110066122 A CN110066122 A CN 110066122A CN 201910067902 A CN201910067902 A CN 201910067902A CN 110066122 A CN110066122 A CN 110066122A
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CN
China
Prior art keywords
optical fiber
deuterium
gas
concentration
manufacturing
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Application number
CN201910067902.XA
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CN110066122B (en
Inventor
川崎希一郎
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Publication of CN110066122A publication Critical patent/CN110066122A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/60Surface treatment of fibres or filaments made from glass, minerals or slags by diffusing ions or metals into the surface
    • C03C25/607Surface treatment of fibres or filaments made from glass, minerals or slags by diffusing ions or metals into the surface in the gaseous phase

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)

Abstract

A kind of equipment that simplicity can be used is provided, while inhibiting the dosage of deuterium, certainly inhibits the increased methods for optical fiber manufacture of hydrogen loss.A kind of manufacturing method of optical fiber, in treatment trough (12) after optical fiber (3) to be wherein put into the gas under defined pressure full of the deuterium containing normal concentration, it is exposed to optical fiber (3) in gas at an established temperature with the defined time, it is spread in deuterium molecule in optical fiber (3), the optical fiber (3), which has, adds germanium and the fiber core part formed and the cladding part being made of pure silicon dioxide glass formed in the periphery of fiber core part in pure silicon dioxide glass, wherein, according to the relative fefractive index difference of fiber core part and cladding part, make the pressure in treatment trough (12), deuterium concentration in treatment trough (12), at least one of the Exposure Temperature of gas and the exposure duration of gas change.

Description

The manufacturing method of optical fiber
Technical field
The present invention relates to the manufacturing methods of optical fiber.
Background technique
The optical fiber of known quartz glass (silica glass) system is the transmission light that transmission wavelength is in infrared band Optical fiber the, if diffusion hydrogen (H in quartz glass2) then transmission loss increase.The main reason for increasing as the transmission loss, The H spread in glass can be enumerated2The reaction product of molecule and the lattice defect (Si-O) being present in quartz glass (Si-OH) absorption caused by.
In order to inhibit the increase for increasing i.e. so-called hydrogen loss of the transmission loss as caused by the defect of Si-O key, have to light Fibre carries out method of the deuterium processing to fill up defect using deuterium.It is known to optical fiber carry out deuterium processing when, need to consider optical fiber In the amount of non-bridge oxygen hole (Non-Bridging Oxygen Hole Center (hereinafter referred to as " NBOHC ")) set deuterium Treatment conditions, but the amount for the NBOHC being not suitable in optical fiber due to deuterium treatment conditions, there are following situations: occur by It is bad caused by deuterium undertreatment, or in order to prevent deuterium undertreatment and exceedingly carry out deuterium processing cause manufacturing time to increase Add, operating efficiency reduces.
Therefore, Patent Document 1 discloses: provide by carrying out deuterium according to the amount of residual NBOHC in a fiber It handles so as to which the methods for optical fiber manufacture of deuterium processing will not be carried out over or underly, therefore at measurement wavelength 630nm Deuterium processing is carried out while absorption loss.
It is disclosed in patent document 2: about optical fiber and its manufacturing method, by measuring wavelength 1410 in deuterium treatment process The transmission loss at any wavelength in~1430nm, thus judge fault of construction and whether completed with reacting for deuterium molecule, Seek reduction in processing time.
[existing technical literature]
[patent document]
[patent document 1] Japanese Unexamined Patent Publication 2006-220824 bulletin
[patent document 2] Japanese Unexamined Patent Publication 2005-170690 bulletin
Summary of the invention
[problems to be solved by the invention]
In patent document 1 and method disclosed Patent Document 2, although deuterium will not can be carried out over or underly Processing, but need for the measurement device or equipment mechanism that are used to measure absorption loss to be set in deuterium processing unit, the equipment Mechanism is to be used to for the terminal part of optical fiber extending out to the outside of deuterium processing unit to measure loss, therefore the dress of deuterium processing sometimes Setting becomes complicated.In addition, the outside per treatment for needing for the terminal of optical fiber to extend out to deuterium processing unit, thus deuterium processing is set It sets cumbersome.
Therefore, the object of the present invention is to provide the equipment that simplicity can be used, while inhibiting the dosage of deuterium, The increased methods for optical fiber manufacture of hydrogen loss can certainly be inhibited.
[means for solving the problems]
One embodiment of the present invention relates to the manufacturing method of optical fiber be,
A kind of manufacturing method of optical fiber, wherein place the fiber under defined pressure full of containing normal concentration In treatment trough after the gas of deuterium, the optical fiber is exposed in the gas with the defined time at an established temperature, is made Deuterium molecule is spread in the optical fiber, wherein the optical fiber have by added with germanium the fiber core part that constitutes of silica glass and In the cladding part being made of pure silicon dioxide glass that the periphery of the fiber core part is formed, wherein
According to the relative fefractive index difference of the fiber core part and the pure silicon dioxide glass, make the pressure in the treatment trough At least one of the Exposure Temperature of deuterium concentration, the gas in power, the treatment trough and the exposure duration of the gas Variation.
[The effect of invention]
It according to foregoing invention, is capable of providing and easy equipment can be used, while inhibiting the dosage of deuterium, certainly Inhibit the increased methods for optical fiber manufacture of hydrogen loss.
Detailed description of the invention
[Fig. 1] is the figure for indicating an example of composition for optical fiber treating device of the present embodiment.
[explanation of label]
1: fiber spool
2: spool
3: optical fiber wire
10: optical fiber treating device
12: treatment trough
14: closed container
16: heater
18: pressure gauge
19: pressure regulator
20: gas supply part
22: first gas feed path
23: on/off valve
24: second gas feed path
25: on/off valve
26: deuterium supply unit
28: diluent gas supply unit
30: gas mixing machine
31: densimeter
32: third gas feed path
33: on/off valve
40: gas exhaust path
42: on/off valve
44: densimeter
46: thermometer
Specific embodiment
(explanations of embodiments of the present invention)
Firstly, enumerating embodiments of the present invention and being illustrated.
One embodiment of the present invention relates to the manufacturing method of optical fiber be,
(1) a kind of manufacturing method of optical fiber, wherein place the fiber under defined pressure full of comprising normal concentration Deuterium gas after treatment trough in, be exposed to the optical fiber in the gas at an established temperature with the defined time, It is spread in deuterium molecule in the optical fiber, wherein the optical fiber has the fiber core part being made of the silica glass added with germanium With the cladding part being made of pure silicon dioxide glass formed in the periphery of the fiber core part, wherein
According to the relative fefractive index difference of the fiber core part and the pure silicon dioxide glass, make the pressure in the treatment trough At least one of the Exposure Temperature of deuterium concentration, the gas in power, the treatment trough and the exposure duration of the gas Variation.
According to the above method, easy equipment can be used, while inhibiting the dosage of deuterium, certainly inhibit hydrogen loss Consumption increases.
(2) Exposure Temperature can be 35 DEG C or more and 50 DEG C or less.
According to the above method, the deterioration of the transmission characteristic as caused by the increase of hydrogen loss can be inhibited.
(3) relative fefractive index difference is being set as Δ n (%), the pressure in the treatment trough is set as to P (kPa), is being incited somebody to action When deuterium concentration in the treatment trough is set as C (%), the exposure duration of the gas is set as to t (hour), it can set described P, the value of the C and the t are so that P × C × t >=37000 × Δ n2.5
(4) it is longer to can be set to the relative fefractive index difference more big then described exposure duration, and makes the pressure, described Deuterium concentration, the Exposure Temperature do not change.
(5) it is higher to can be set to the more big then described pressure of the relative fefractive index difference.
(6) it is higher to can be set to the more big then described deuterium concentration of the relative fefractive index difference.
According to these above-mentioned methods, it can be realized simultaneously the increase for inhibiting hydrogen loss and inhibit the dosage of deuterium.
(7) relative fefractive index difference can be 0.3% or more.
For optical fiber biggish for relative fefractive index difference, it is particularly effective for carrying out deuterium processing by above-mentioned method.
(8) the deuterium concentration can be 3% or less.
Hydrogen explosion in order to prevent, deuterium concentration are preferably set to above range.
(detailed contents of embodiments of the present invention)
Hereinafter, being illustrated referring to attached drawing to the methods for optical fiber manufacture that embodiments of the present invention are related to.
It illustrates, but is indicated by the range of claims, and be intended to it should be noted that the present invention is not restricted to these Whole changes in the meaning and range being equal including the range with claims.
Hereinafter, being described in detail based on preferred embodiment of the attached drawing to the manufacturing method of optical fiber of the present invention.
(wire-drawing process)
Firstly, preparing the optical fiber base material for being used for fiber manufacturing.Optical fiber base material is configured to realize manufactured optical fiber The light-transfer characteristic that should have.For example, optical fiber base material is included by added with germanium or germanium-containing compound (such as GeO2) dioxy SiClx glass constitute fiber core part and fiber core part periphery be arranged by high-purity silicon dioxide glass (pure silicon dioxide glass One example of glass) constitute cladding part.Germanium is added to improve the refractive index of fiber core part.Fiber core part is relative to high-purity The relative fefractive index difference for spending quartz glass is, for example, Δ n=0.30~0.80% or so.
Next, optical fiber base material is installed in defined wire-drawing frame, wire drawing is then carried out.The condition of wire drawing is with made The outer diameter for the optical fiber made for example is suitably determined as 125 μm of mode.The coating tree in the periphery of the optical fiber manufactured after wire drawing Rouge, to manufacture optical fiber wire.
(deuterium treatment process)
Next, batching optical fiber wire on fiber spool, optical fiber is placed in by optical fiber wire for each fiber spool In processing unit, deuterium processing is carried out.
Fig. 1 is the schematic diagram being illustrated for the manufacturing method to optical fiber of the present embodiment.As shown in Figure 1, Optical fiber treating device 10 has treatment trough 12, gas supply part 20 and gas mixing machine 30.Gas supply part 20 is via the first gas Body feed path 22 and second gas feed path 24 and be connected to gas mixing machine 30.Gas mixing machine 30 is via third gas Body feed path 32 and be connected to treatment trough 12.In addition, treatment trough 12 is connected to gas exhaust path 40.
Treatment trough 12 has closed container 14, heater 16, pressure gauge 18 and pressure regulator 19.Closed container 14 is can The space 14A for accommodating fiber spool 1 to be ensured to be to the container of air-tight state.For fiber spool 1, rolled up on spool 2 It is wound with the optical fiber wire 3 obtained in wire-drawing process.Be provided with for closed container 14 in the outside of closed container 14 and The heater 16 that space 14A is heated.
In addition, being connected with the pressure gauge 18 for being measured to the pressure in closed container 14 on closed container 14. Also, the pressure regulator 19 for the pressure in closed container 14 to be adjusted is provided on closed container 14.Pressure Adjuster 19 is such as may include vacuum pump, pressure-regulating valve, pressure control circuit.
Gas supply part 20 is supplied by storing the deuterium supply unit 26 of deuterium and storing the diluent gas of diluent gas Portion 28 is constituted.Gas supply part 20 is via first gas feed path 22 by deuterium (D2) supply to gas mixing machine 30, and Diluent gas is supplied to gas mixing machine 30 via second gas feed path 24.
The deuterium and diluent gas that flow into from gas supply part 20 are mixed to mixed gas by gas mixing machine 30, will The mixed gas is supplied via third gas feed path 32 to treatment trough 12 (closed container 14).In gas mixing machine 30 Densimeter 31 is provided in the third gas flow path 32 in downstream.Densimeter 31 is used to mix to when mixing deuterium and diluent gas Composition and division in a proportion rate is controlled.That is, the deuterium concentration of 31 pairs of mixed gas being mixed with using gas mixing machine 30 of densimeter is surveyed It is fixed, and information relevant to the measured value of deuterium concentration is sent to gas supply part 20.Gas supply part 20 is based on by densimeter The deuterium concentration of 31 measurements, to become the side of defined range by the blending ratio of the mixed mixed gas of gas mixing machine 30 The flow of formula, flow to the deuterium supplied from deuterium supply unit 26 and the diluent gas supplied from diluent gas supply unit 28 into Row is adjusted.
It is provided in first gas feed path 22 by the on/off valve of the opening and closing switching of first gas feed path 22 23.It is provided in second gas feed path 24 by the on/off valve 25 of the opening and closing switching of second gas feed path 24.? Third gas feed path 32 (downstream side compared with densimeter 31), which is provided with, cuts the opening and closing of third gas feed path 32 The on/off valve 33 changed.It is provided in gas exhaust path 40 by the on/off of the opening and closing switching of gas exhaust path 40 Valve 42.
In addition, being provided with densimeter 44 and thermometer 46 in gas exhaust path 40.Using densimeter 44 to from gas The concentration for the gas that body discharge path 40 is discharged into the atmosphere is measured.Using thermometer 46 to from 40 row of gas exhaust path The temperature of mixed gas out is measured.Pass through the concentration and temperature using densimeter 44 and 46 pairs of thermometer discharge gases Degree is measured, so as to the concentration (deuterium concentration) and closed container 14 of the deuterium to the mixed gas in closed container 14 Interior temperature is confirmed.It is concentration 4% since the explosion of deuterium is critical, preferably by the mixed gas in closed container 14 Deuterium concentration is set as 3% hereinafter, so that critical with abundant surplus apart from the explosion.It is further preferred, that based on by temperature The temperature for the discharge gas that meter 46 measures, is adjusted heating temperature by heater 16, so that fiber spool 1 is exposed to The surface temperature (that is, temperature (Exposure Temperature) in closed container 14) of optical fiber wire 3 when mixed gas becomes 35 DEG C or more And 50 DEG C or less.The surface temperature of optical fiber wire 3 is adjusted to 35 DEG C or more and 50 DEG C or less as a result,.By by closed container The Exposure Temperature of mixed gas in 14 is adjusted into above range, so as to inhibit the increase of hydrogen loss.
Next, being illustrated to the methods for optical fiber manufacture for having used above-mentioned optical fiber treating device 10.
Firstly, accommodating the fiber spool 1 for batching optical fiber wire 3 in closed container 14, and closed container 14 is kept For air-tight state.Next, operation on/off valve 23,25,33,42, first gas feed path 22, second gas are supplied It is set as opening state to path 24, third gas feed path 32, and gas exhaust path 40 is set as opening state.
Next, deuterium is supplied from gas supply part 20 (deuterium supply unit 26) via first gas feed path 22 To gas mixing machine 30, and diluent gas is supplied from gas supply part 20 (diluent gas supply unit 28) via second gas Path 24 and supply to gas mixing machine 30.Next, deuterium and diluent gas are mixed in gas mixing machine 30 For mixed gas.Herein, the concentration (deuterium concentration) of the deuterium in mixed gas is for example set as 2%.
Next, mixed mixed gas will be supplied extremely via third gas feed path 32 in gas mixing machine 30 In the closed container 14 for the treatment of trough 12.At this point, the gas in closed container 14 is discharged by gas exhaust path 40, it is discharged into In atmosphere.
It is measured, is confirmed by concentration of the densimeter 44 to the deuterium for the mixed gas being discharged from gas exhaust path 40 Concentration becomes 2%.Due to the concentration and supply to closed container 14 of the deuterium for the mixed gas being discharged from gas exhaust path 40 The deuterium concentration of interior mixed gas is identical, is all 2%, it may thus be appreciated that the concentration of the deuterium in closed container 14 is 2%, i.e. gas Body displacement is completed.
After the deuterium concentration that confirmed closed container 14 reaches normal concentration (such as 2%), operation on/off valve 23,25,33,42, first gas feed path 22, second gas feed path 24, third gas feed path 32 are set to off Closed state, and gas exhaust path 40 is set as closed state.The concentration of the deuterium in closed container 14 is remained as a result, About 2%.In this state, the temperature in closed container 14 is remained about 45 DEG C by heater 16.Also, in closed container It is exposed to the optical fiber wire 3 of fiber spool 1 in deuterium with the stipulated time.
In addition, knowing the defect level of the fiber core part of optical fiber according to the germanium (example added to improve the refractive index of fiber core part Such as, GeO2) amount and correspondingly increase.Therefore, it was found by the inventors of the present invention that by according to the opposite of fiber core part and cladding part Refractive indices n changes the deuterium treatment conditions of the fiber spool 1 in closed container 14, thus even if fiber core part Defect level changes, and can use deuterium also fully to fill up the defect of fiber core part.
Specifically, in the present embodiment, according to the fiber core part of the optical fiber wire 3 batched on fiber spool 1 with it is pure The relative fefractive index difference Δ n of silica glass, make accommodate fiber spool 1 closed container 14 (treatment trough 12) in pressure, Deuterium concentration in closed container 14, the Exposure Temperature of mixed gas containing deuterium and in the exposure duration of mixed gas extremely Few one changes.
For example, the fiber core part of optical fiber wire 3 and the relative fefractive index difference Δ n of pure silicon dioxide glass are bigger, then make closed The exposure duration that fiber spool 1 in container 14 is carried out by the mixed gas containing deuterium is longer.It should be noted that at this point, The Exposure Temperature of the pressure in closed container 14, the deuterium concentration of mixed gas and mixed gas is not set to change.In this way, By keeping the exposure duration of the more big then mixed gas of relative fefractive index difference Δ n longer, and do not make pressure in closed container 14, Deuterium concentration and Exposure Temperature change, and inhibit optical fiber so as to the equipment that uses optical fiber treating device 10 easy like that The increase of the hydrogen loss of plain line 3.In addition, in the method, due to not making pressure, deuterium concentration and exposure in closed container 14 Temperature changes, therefore handles simplicity, and can inhibit the dosage of deuterium.
It should be noted that the example that substitution is above-mentioned, can also make the more big then closed container of relative fefractive index difference Δ n Pressure in 14 is higher.Pressure in closed container 14 can be adjusted by pressure regulator 19.It, can also according to this method Certainly hydrogen loss to be inhibited to increase, and inhibit the dosage of deuterium.
Alternatively, it is also possible to keep the more big then supply of relative fefractive index difference Δ n dense to the deuterium of the mixed gas in closed container 14 It spends higher.The deuterium concentration of supply to the mixed gas in closed container 14 can be by making the deuterium from the supply of deuterium supply unit 26 It is changed with the ratio of the supply amount of the diluent gas supplied from diluent gas supply unit 28 to be adjusted.According to this Method certainly can also inhibit hydrogen loss to increase.It should be noted that as described above, it is preferred to the upper limit of deuterium concentration is set as 3%.
Also, relative fefractive index difference Δ n can also be made more big, the Exposure Temperature of mixed gas (is contained in closed container 14 The surface temperature of interior optical fiber wire 3) it is higher.According to this method, it can be realized simultaneously and hydrogen loss is inhibited to increase and inhibit deuterium Dosage.It should be noted that as described above, it is preferred to by the surface temperature of optical fiber wire 3 be set as 35 DEG C or more and 50 DEG C with Under.This is because: hydrogen loss increases when making surface temperature outside 35 DEG C or more and 50 DEG C of ranges below, transmission characteristic is bad A possibility that change, is high.
In this way, making deuterium treatment conditions (pressure, mixed gas in closed container 14 by according to relative fefractive index difference Δ n Deuterium concentration, the Exposure Temperature of mixed gas and mixed gas exposure duration) change, so as to use simplicity Equipment, certainly hydrogen loss is inhibited to increase, and the dosage of deuterium can be inhibited.
It should be noted that by above-mentioned method to the relative fefractive index difference Δ n of fiber core part and pure silicon dioxide glass It carries out deuterium to handle being particularly effective for the optical fiber wire 3 of 0.3% or more (that is, relative fefractive index difference Δ n is larger).
Next, the embodiment to present embodiment is illustrated.
(embodiment 1)
Using optical fiber treating device 10 of the present embodiment, the gas for carrying out the closed container 14 for the treatment of trough 12 is set It changes, and deuterium processing is carried out to optical fiber.Specifically, having prepared the relative fefractive index difference Δ of fiber core part and pure silicon dioxide glass The optical fiber wire 3 that n is 0.330% is wound in fiber spool 1 obtained by spool 2, which is put into treatment trough 12 In closed container 14.Also, by deuterium (D2) concentration be 2%, nitrogen (N2) concentration be 98% mixed gas supply to closed Container 14, the interior pressure by the mixed gas in 100kPa are filled to closed container 14.Next, by heater 16 to close Container 14 is closed to be heated so that the surface temperature of optical fiber wire 3 soaks optical fiber wire 3 in closed container 14 as 45 DEG C Stain is 36 hours in mixed gas.Then, the wavelength loss characteristic of the deuterium treated optical fiber wire 3 is measured.
Next, filling hydrogen (H with the interior pressure below of 1 atmospheric pressure2) concentration be 1% and nitrogen (N2) concentration is In treatment trough after 99% mixed gas, which is impregnated 48 hours.To the hydrogen treated optical fiber wire 3 Wavelength loss characteristic is measured.
To hydrogen before and after the processing (that is, deuterium (D2) after processing and hydrogen (H2) after processing) and the transmission loss of 1380nm wave band carry out Compare, as a result, the value of the transmission loss of (deuterium processing after) is 0.30dB/km before hydrogen processing, the value of hydrogen treated transmission loss For 0.30dB/km, increase after hydrogen processing without hydrogen loss.
In the same manner as in the above embodiment 1, each item shown in embodiment 2~10 and comparative example 1~3 shown in the following table 1 Under part, the optical fiber wire 3 with different relative fefractive index difference Δ n is subjected to deuterium (D in closed container 142) processing.Also, Hydrogen (H is carried out to deuterium treated optical fiber wire 3 under the same conditions as example 12) processing, to the transmission of hydrogen before and after the processing Loss characteristic is compared.The condition of deuterium processing in embodiment 2~10 and comparative example 1~3 is shown in table 1.
[table 1]
Table 1
In embodiment 2~5, the relative fefractive index difference Δ n of optical fiber is bigger, then the exposure duration of deuterium is longer.It needs Bright, the pressure in closed container 14 at this time, the concentration of deuterium in closed container 14 and the surface temperature of optical fiber exist It is identical between each embodiment.In addition, as shown in table 1, in embodiment 2~5, about the pressure in closed container 14, deuterium The relative fefractive index difference of optical fiber is being set as Δ n (%), by the pressure in closed container 14 by the exposure duration of the concentration of gas, deuterium Power is set as P (kPa), the concentration of the deuterium in closed container 14 is set as C (%), the exposure duration of deuterium is set as to t (hour) When, the value of setting pressure P, concentration C and exposure duration t are so that P × C × t >=37000 × Δ n2.5(hereinafter referred to as condition Formula (1)).
It on the other hand,, will using the optical fiber with relative fefractive index difference Δ n same as Example 3 in comparative example 1 The exposure duration t of deuterium is set as the time (20hr) shorter than the exposure duration (27hr) of embodiment 3.It should be noted that In comparative example 1, for concentration C, the surface temperature of optical fiber of pressure P, deuterium in closed container 14, it is set as and embodiment 2~5 Identical value, therefore it is unsatisfactory for above-mentioned conditional (1).
In above-described embodiment 2~5, the transmission loss characteristic of hydrogen before and after the processing is compared, as a result, before hydrogen processing The value of the transmission loss of (deuterium processing after) is 0.30dB/km, and the value of hydrogen treated transmission loss is 0.30dB/km, without hydrogen Loss increases.On the other hand, in the comparative example 1 for being unsatisfactory for conditional (1), the transmission loss characteristic of hydrogen before and after the processing is carried out Compare, as a result, the value of the transmission loss of (deuterium processing after) is 0.30dB/km before hydrogen processing, the value of hydrogen treated transmission loss For 0.33dB/km, hydrogen loss is increased.From the result can be confirmed to: by make the relative fefractive index difference Δ n of optical fiber more it is big then The exposure duration t of deuterium is longer, so as to inhibit the increase of transmission characteristic caused by being increased by hydrogen loss.It needs to illustrate Be, the deuterium in closed container 14 concentration C reach 2% stage in, it is each turn on/off valve be close, therefore even if The exposure duration t of deuterium changes, and the dosage of deuterium can also be suppressed to a certain amount of.
In embodiment 6~8, the relative fefractive index difference Δ n of optical fiber becomes bigger, then the pressure P of closed container 14 is higher. It should be noted that the exposure duration t of deuterium at this time, deuterium concentration C and optical fiber surface temperature each embodiment it Between be identical.In addition, in the same manner as embodiment 2~4, in embodiment 6~8, for pressure P, the deuterium in closed container 14 The exposure duration t of the concentration C of gas, deuterium, the value of setting pressure P, concentration C and exposure duration t are to meet conditional (1).
On the other hand, in comparative example 2, using the biggish optical fiber of relative fefractive index difference Δ n compared with Example 6, and will Pressure P in closed container 14 is set as the identical pressure (38kPa) with the pressure of embodiment 6 (38kPa).It needs to illustrate Be, in comparative example 2, for the exposure duration t of deuterium, the concentration C of deuterium, the surface temperature of optical fiber, be set as with embodiment 6~ 8 is identical, therefore is unsatisfactory for conditional (1).
In above-described embodiment 6~8, the transmission loss characteristic of hydrogen before and after the processing is compared, as a result, before hydrogen processing The value of the transmission loss of (deuterium processing after) is 0.30dB/km, and the value of hydrogen treated transmission loss is 0.30dB/km, without hydrogen Loss increases.On the other hand, in the comparative example 2 for being unsatisfactory for conditional (1), the transmission loss characteristic of hydrogen before and after the processing is carried out Compare, as a result, the value of the transmission loss of (deuterium processing after) is 0.30dB/km before hydrogen processing, the value of hydrogen treated transmission loss For 0.33dB/km, hydrogen loss is increased.It can be confirmed according to the result: by keeping the relative fefractive index difference Δ n of optical fiber bigger Then the pressure P of closed container 14 is higher, so as to inhibit the increase of transmission characteristic caused by being increased by hydrogen loss.
In embodiment 9 and embodiment 10, relative fefractive index difference Δ n becomes bigger, then the concentration C of deuterium is higher.It needs It is noted that the surface temperature of pressure P and optical fiber in closed container 14 at this time are in embodiment 9 and embodiment 10 Identical value, and embodiment 10 shortens the exposure duration t of deuterium compared with Example 9.In addition, same as embodiment 2~8 Ground, in embodiment 9 and embodiment 10, for the exposure duration of the concentration C of pressure P, deuterium in closed container 14, deuterium T, the value of setting pressure P, concentration C and exposure duration t are to meet conditional (1).
On the other hand, in comparative example 3, using the optical fiber with relative fefractive index difference Δ n same as in Example 10, and The concentration C of deuterium is set as the concentration (2%) lower than the concentration (3%) of embodiment 10.It should be noted that in comparative example 3 In, the pressure P in closed container 14 is set as the pressure (50kPa) lower than the pressure (100kPa) of embodiment 10, by deuterium Exposure duration t be set as time longer than the exposure duration (18hr) of embodiment 10 (for 24 hours r), and by the surface temperature of optical fiber Degree is set as (40 DEG C) same as in Example 10.As above the comparative example 3 set is unsatisfactory for conditional (1).
In above-described embodiment 9 and embodiment 10, the transmission loss characteristic of hydrogen before and after the processing is compared, as a result, The value of the transmission loss of (deuterium processing after) is 0.30dB/km before hydrogen processing, and the value of hydrogen treated transmission loss is 0.30dB/ Km increases without hydrogen loss.On the other hand, in the comparative example 3 for being unsatisfactory for conditional (1), the transmission of hydrogen before and after the processing is damaged Consumption characteristic is compared, as a result, the value of the transmission loss of (deuterium processing after) is 0.30dB/km before hydrogen processing, and treated passes for hydrogen The value of defeated loss is 0.33dB/km, and hydrogen loss increases.It can be confirmed according to the result: the relative by making optical fiber The concentration C of the more big then deuterium of rate difference Δ n is higher, so as to inhibit the increase of transmission characteristic caused by being increased by hydrogen loss.
More than, in detail and the present invention is described referring to specific embodiment, but for those skilled in the art For member, it is clear that can make various changes, modify under the premise without departing from the spirit and scope of the present invention.In addition, above-mentioned Quantity, position, shape of the component parts of explanation etc. are not limited to the above embodiment, in order to implement the present invention, Neng Goubian Quantity, position, shape for being more suitable for etc..

Claims (9)

1. a kind of manufacturing method of optical fiber, wherein place the fiber under defined pressure full of the deuterium containing normal concentration Gas after treatment trough in, be exposed to the optical fiber in the gas at an established temperature with the defined time, make deuterium Molecule is spread in the optical fiber, wherein the optical fiber have by added with germanium the fiber core part that constitutes of silica glass and The cladding part being made of pure silicon dioxide glass that the periphery of the fiber core part is formed, wherein
According to the relative fefractive index difference of the fiber core part and the pure silicon dioxide glass, make pressure in the treatment trough, institute At least one of the exposure duration for stating the deuterium concentration in treatment trough, the Exposure Temperature of the gas and the gas changes.
2. the manufacturing method of optical fiber according to claim 1, wherein
The Exposure Temperature is 35 DEG C or more and 50 DEG C or less.
3. the manufacturing method of optical fiber according to claim 2, wherein
The relative fefractive index difference is set as Δ n (%), the pressure in the treatment trough is set as to P (kPa), by the processing When deuterium concentration in slot is set as C (%), the exposure duration of the gas is set as to t (hour), the P, the C and institute are set The value of t is stated to become following formula
P×C×t≥37000×Δn2.5
4. the manufacturing method of optical fiber according to claim 1, wherein
The the relative fefractive index difference the big, keeps the exposure duration longer, and does not make the pressure, the deuterium concentration, described Exposure Temperature changes.
5. the manufacturing method of optical fiber according to claim 1, wherein
The the relative fefractive index difference the big, keeps the pressure higher.
6. the manufacturing method of optical fiber according to claim 1, wherein
The the relative fefractive index difference the big, keeps the deuterium concentration higher.
7. the manufacturing method of optical fiber according to any one of claim 1 to 6, wherein
The relative fefractive index difference is 0.3% or more.
8. the manufacturing method of optical fiber according to any one of claim 1 to 6, wherein
The deuterium concentration is 3% or less.
9. the manufacturing method of optical fiber according to claim 7, wherein
The deuterium concentration is 3% or less.
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