CN1026777C - Method for manufacturing silica glass base material - Google Patents
Method for manufacturing silica glass base material Download PDFInfo
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- CN1026777C CN1026777C CN 91109288 CN91109288A CN1026777C CN 1026777 C CN1026777 C CN 1026777C CN 91109288 CN91109288 CN 91109288 CN 91109288 A CN91109288 A CN 91109288A CN 1026777 C CN1026777 C CN 1026777C
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/0128—Manufacture of preforms for drawing fibres or filaments starting from pulverulent glass
- C03B37/01282—Manufacture of preforms for drawing fibres or filaments starting from pulverulent glass by pressing or sintering, e.g. hot-pressing
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/016—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by a liquid phase reaction process, e.g. through a gel phase
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Abstract
A silica-based glass rod (31) is inserted into a space portion of a mold (21). Then, a slurry (32), which is obtained by dispersing a silica glass powder material in pure water, is poured into a molding space between the glass rod (31) and the inner surface of the mold (32), whereby a porous glass shaped body (34) is formed around the glass rod (31). Drying this shaped body results in a silica glass base material which includes the glass rod (31) and the porous glass shaped body (34) surrounding the same.
Description
The present invention relates to the manufacture method of silica glass base material, this material is used for the waveguide prefabricated rods, and for example preform, biography resemble fiber preform, photoconduction prefabricated rods, post lens prefabricated rods, or the like, use in optical communication and field of optical applications.
The CVD method, for example VAD method (axially vapor deposition method), MCVD method (modified chemical vapor deposition method), OVD method (outside vapor deposition), PCVD method (PCVD (Plasma Chemical Vapor Deposition)), or the like, the method that powder slurry perfusion or a kind of VAD method and sol-gel method combine all can be used to make the waveguide prefabricated rods, for example preform, biography resemble fiber preform, photoconduction prefabricated rods, post lens prefabricated rods or the like, and these prefabricated rods are used in optical-fibre communications and field of optical applications.
According to the CVD method, halogenide gas (SiCl for example
4Or GeCl
4) as raw material, this raw material generates oxide powder, for example SiO by oxidizing reaction or flame hydrolysis
2Or GeO
2Then this oxide powder is deposited to (external peripheral surface of the top surface of loop-carrier, the inner circumferential surface of silica tube, plug) on the specific deposition surface, and it is consolidated into transparent vitreous body, thereby be made for prefabricated rods.
In order to obtain higher-quality optical fiber, also dropped into use recently based on the manufacturing installation of the prefabricated rods of complete synthesis VAD method.
In the manufacturing of single-mode fiber prefabricated rods, in this connection, have the core of suitable external diameter ratio and a porous glass body of part cortex by the VAD method is synthetic at first simultaneously.Become transparent silica-based glass rod with this porous glass body is fixed then.For the external diameter of core skin ratio is adjusted to 10/125(μ m) (to the adjustment of external diameter), therefore, on this transparent quartz glass bar, deposit the porous glass body as cortex, and sedimentary vitreum is consolidated into transparent glass preform by the OVD method.
According to the powder teeming practice, as disclosed uncensored Japanese Patent JP64-56331 etc. is disclosed, in pure water, disperse earlier to form the powder slurry through pretreated microlith English glass powder material, then the powder slurry is filled in the shaping mould, so that the water in the powder slurry is absorbed by mould.Therefore, form porous vitreum by thin glass powder material.Further that this porous vitreum is dry and be consolidated into transparent glass.
The method that combines according to this VAD method and sol-gel method, as disclosed uncensored Japanese Patent JP1-294548 etc. is disclosed, bar-shaped porous glass body (constituting) (mainly by the preparation of VAD method) by core glass and part cortex glass, with tubular porous glass body (remaining cortex part), (preparing), utilize rod in tube method to combine by sol-gel method.After this, these porous glass bodies are consolidated together into transparent vitreum.
CVD method recited above, there is following technical problem in the method that powder teeming practice and VAD method combine with sol-gel method.
Under the situation of CVD method (although qualified product is high-quality), the sedimentation effect of oxide powder is low to moderate 30～60%, and the size of equipment is very big.As mentioned above, there are some shortcomings in the economic aspect at high yield, rational product cost and equipment.
The slip casting method can be produced high-quality porous glass body in enough simple equipment high efficiency rates ground.But only technology in this way can not obtain waveguiding structure.
So under the situation of slip casting method, this method itself must be improved, perhaps, it need use some other corresponding means.But, for the slip casting method in the example of prior art also without any technical advice.
Under the method situation that VAD method and sol-gel combine, the cost of raw material-alkoxide is very high, and rib shape material is easy to break when it is dry.And, according to this method, be difficult to obtain large size prefabricated.
After having considered these situations, designed the present invention, its purpose is the method that a kind of new manufacturing silica glass base material will be provided.
Another object of the present invention is that a kind of method of reasonably making the high quality silica glass base material economically will be provided.
According to the present invention, it provides the method for making silica glass base material, and it comprises: the step of a quartz glass bar being inserted the hollow space of mould; And powder slurry is filled into model hollow space between the internal surface of glass stick and shaping mould, thus form glass powder powder body around glass stick, wherein the powder slurry obtains by the quartzy glass powder material of dispersion in pure water.
According to the present invention, form this porous vitreum by the powder teeming practice around silica-based glass rod with the usual method manufacturing, make equipment cost very low, and output is enough high.Therefore, this product is very economical.
Fig. 1 is the explanatory view of first embodiment of the invention operating method;
Fig. 2 is the longitudinal sectional drawing according to the silica glass base material of first embodiment manufacturing;
Fig. 3 is the transverse cross-sectional view that the base material with Fig. 2 is consolidated into the preform that transparent glass obtains;
Fig. 4 is the explanatory view of the operating method of second embodiment of the invention;
Fig. 5 is the longitudinal sectional drawing according to the silica glass base material of second embodiment manufacturing.
Fig. 6 is the transverse cross-sectional view that the base material with Fig. 5 is consolidated into the preform that transparent glass obtains;
Fig. 7 A and 7B are according to the longitudinal sectional drawing of the silica glass base material of the 3rd embodiment acquisition of the present invention;
Fig. 8 is the device instance sketch that is used to handle silica glass base material of the present invention.
According to the present invention, silica glass base material forms the porous glass body by the powder casting method around the silica-based glass rod and makes.
In this case, the silica-based glass rod can be made with a kind of commonsense method, this bar construction the core of silica glass base material. This rod is preferably standby by the CVD legal system, such as the VAD method.
Select the CVD method that following two reasons are arranged. At first, the method almost is full ripe technology with the major part of consequent high quality glass rod as preform. Secondly, according to the method, although the deposition efficiency of the oxide powder of use CVD method gained is lower, the percent by volume of glass bar is very low in the prefabricated rods, thereby both can limit the minimizing of total output, and can avoid the increase of its equipment size.
When becoming the porous glass body with the slip-casting method around the silica-based glass clavate, only need in mould, to pour into specific powder slurry. Therefore, by using economic equipment and simple technology can obtain with gratifying output the prefabricated component of desired shape. And, in treatment process subsequently, only need this porous glass spare drying, purifying and be consolidated into transparent vitreum.
So, when having the prefabricated rods of waveguiding structure, can produce with lower equipment cost high yield ground by method manufacturing of the present invention.Therefore, can reduce product cost, and its production is very economical.
Now the present invention is described in detail.
Fig. 1 is the explanatory view of the operating method of first embodiment of the invention.
In Fig. 1, label 11 and 21 is represented powder slurry irrigator and mould respectively.
This irrigator 11 comprises a container 14, and this container has lid 12 respectively and has outlet pipe 13 in the bottom at the top, and an agitator 15 is set in container 14.These parts for example can be made by the artificial quartz glass.
In Fig. 1, silica-based glass rod 31 is by will be for example getting the dehydration of porous glass spare by the VAD legal system, then it is consolidated into that transparent glass obtains.This glass stick 31 can only be made core glass, or makes core glass and part cortex glassy phase bonded rod.
Usually, the silica glass powder in powder slurry 32 mainly is made up of pure quartz powder.Yet in some cases, its powder can mix mutually with the oxide powder of other kind of using for the specific refractory power of adjusting quartz.
The particle diameter scope of silica glass powder is preferably between 0.6 to the 20 μ m.Can obtain gratifying characteristic with the powder of median size in this scope as the powder of slurry casting slurry.
Making according to above-mentioned arrangement in the process of prefabricated rods, at first adjusted is being poured in the container 14 of powder slurry irrigator 11 to the powder slurry 32 of predetermined viscosity, and stirred equably with agitator 15.Silica-based glass rod 31 is vertically inserted on the position of axle of mould 21, and keep this state.
Subsequently, the powder in container 14 slurry 32 is injected into the hollow space (between the inner circumferential surface of the external peripheral surface of glass stick 31 and mould 21) of shaping mould by outlet pipe 13.
After through one period scheduled time, powder slurry 32 water sorptions by mould 21 in mould 21 dewater, thereby its volume reduces, and form a moisture less porous glass body 33.
Owing to removed quite most moisture content (although moisture content is removed still not exclusively) from porous vitreum 33, this prefabricated component is dried, and reaches certain degree, thereby makes it can keep the shape of itself.
Therefore, by after forming porous glass body 33 with shaping mould 21, this vitreum 33 is taken out from mould, and put it in the moisture eliminator (not shown) dry.
After dry this porous glass body 33 of this moisture eliminator, formed the porous glass body 34 of water content hardly as shown in Figure 2.Thereby obtained the silica glass base material 35 formed by glass stick 31 and porous glass body (precast body) 34.
Subsequently, this porous glass body 34 is carried out conventional dehydration/purge process and consolidation process.Like this, just can obtain a waveguide prefabricated rods (for example preform 37), this prefabricated rods have as shown in Figure 3 glass stick 31 and around this excellent transparent vitreous body 36.
After porous glass body 34 is consolidated into transparent glass, repeatedly form porous glass body and then fixed technology, so that the diameter of transparent vitreous body 36 increases.With this, just can obtain having the prefabricated rods of larger diameter.
Second embodiment of the present invention described now.According to this embodiment, slurry casting is performed such, that is, the middle portion of shaping mould is formed by the glass powder particle of relatively large particle diameter, and its periphery uses the powder particle than small particle size to constitute.
Below the reason of making prefabricated rods in this way will be described.
Table 1 shows the characteristic of the porous glass body of the quartz particles bodily form formula that obtains under fixed model condition.
Table 1
Precast body
Particle diameter micro-pore diameter intensity bubble
Big low few
Less height is more
In this case, fixed have bubble to exist afterwards.Numerous air-bubble easily is present in the centre portions of prefabricated rods.And do not have bubble basically owing to the easy diffusion of gas in the outer ring of prefabricated rods part.
The diameter of quartz particles is more little, and the intensity of the porous glass body that is obtained is just high more.
If the intensity of the peripheral portion of porous glass body is strong more, then the crack that causes owing to the stress-strain in the forming operation process can take place more fewly, and the also easier manipulation of this vitreum.
In this embodiment, put into bigger quartz particles, so that after fixed, can limit the generation of bubble in the preform at the middle portion of mould.
Yet owing to put into thinner quartz particles on the inwall limit of mould, the physical strength of this porous glass body has had raising, so, can prevent crackle, crack etc.
Fig. 4 is the explanatory view of the operating method of second embodiment of the invention.Silica-based glass rod 31 and mould 21 can be placed in the mode that resembles first embodiment.
In this embodiment, relatively large glass powder particle 44 is provided to the middle portion near glass stick 31, and less relatively powder particle 45 is provided to its peripheral portion.
More particularly, inside and outside co-axial container 43a and 43b are inserted in the reperfusion space of mould 21, the powder slurry that contains thicker glass powder particle 44 is injected among the container 43a, and fine powder granules 45 is injected among the container 43b.
In this case, the average particulate diameter of raw glass powder particle 44 preferably is in the scope of 1 to 20 μ m.And the average particulate diameter of thin glass powder particle 45 is in the scope of 0.6 to 1 μ m.
In this embodiment, two kinds of particle diameter scopes have been adopted.Yet, can be with three kinds or more kinds of particle diameter scope.
After through one period scheduled time, utilize mould 21 that its powder slurry is dewatered to form precast body.This precast body is shifted out from mould, and, make porous glass body 46 thus with coarse grained middle portion 47 and fine grain peripheral portion 48 with a moisture eliminator drying.Therefore, make by glass stick 31 and the silica glass base material 49 formed around its peripheral porous glass body 46.
This vitreum 46 is dewatered-purifying process and sintering process, can obtain as shown in Figure 6 like this, have glass stick 31 and around the preform 54 of this rod and the transparent vitreous body 51 that becomes one.
The 3rd embodiment of the present invention described now.According to this embodiment, the both ends or one end of porous glass prefabricated component are made a taper shape or made the three-dimensional bending surface that radius-of-curvature is equal to or greater than this prefabricated component outside diameter.So, the surface-area of precast body can be reduced, and can improve the ability that it stops stress.Its result obtains following effect.
(1) has under the situation of the end of taper shape or three-dimension curved surface and limit portion at precast body, in porous glass precast body manufacturing processed, in the time will forming prefabricated component and from mould, take out by perfusion, the edge section that can prevent this precast body is chipping, and can reduce the crack in this precast body significantly.
(2) because preform is to make with the silica glass base material with pyramid type or end bent.When making it fixed in the high-temperature zone of the one end little by little being inserted a stove.Then the precast body of this silica glass base material from its terminal fixed or transparent glass thus, can obtain the middle portion of preform do not leave over bubble uniformly, extremely transparent glass.
When (3) after fixed, making optical fiber by wire drawing, can not change its shape and with a support rod or analogue welding, thereby shortened the process time, and improve its product production.
In this embodiment, around silica-based glass rod 31, form porous glass body 55 in the mode identical with first or second embodiment, each end of this porous glass body 55 is the taper (cone shape) shown in Fig. 7 A, or shown in Fig. 7 B, formation has the three dimensional curvature surface that radius-of-curvature is equal to or greater than the external diameter of this precast body.Under this condition, can be by having the mould with vitreum 55 corresponding taper shapes or three-dimension curved surface, or form the end of gas preform 55 by machine (as lathe).
The method of preferably handling this silica glass base material according to embodiment mode recited above will be described below.
To after dehydration/purifying process, be consolidated into transparent vitreous body according to the silica glass base material of above-mentioned embodiment manufacturing.After dehydration/purifying process, this material is exposed in the He atmosphere immediately, fixed in containing He atmosphere then.
Usually, gradually this porous matter prefabricated component is inserted the high-temperature zone with 100 to 300 millimeters speed per hour when fixed.Yet according to the method,, after fixed, easily there is bubble if when being lower than micron number magnitude powder as raw material with particle diameter.Especially, can have more bubble in middle portion, these gaseous diffusion are slower.
One that is made by the inventor studies show that between particle diameter and pore size distribution and has following relationship.Particle diameter is more little, and then pore diameter is more little.This shows that when pore diameter reduces the removal of gas and diffusion need be spent many times.In addition, if particle diameter is less, then precast body is easy to fixedly, and promptly hole can be easily or sealing apace, thereby gas can not more easily be discharged.These conditions can be impelled the development of bubble.
So, before consolidation technique, earlier the porous glass body is placed He gas.So, the bigger He gas of spread coefficient is filled in the hole of porous glass body,, does not have bubble to exist although so that hole is closed in consolidation process.Before He gas is filled, under vacuum condition, this porous glass body is carried out bake out.Do the dividing potential drop that can reduce adsorbed gas in the hole like this, so that this gas can more easily be removed or spread.Therefore, bubble more is not easy to exist.
To describe this treatment process of silica glass base material below in detail.
Dry in a usual manner above-mentioned silica glass base material (as to 100 ℃) is then at He and Cl
2Carry out heat treated (dehydration and purifying) under the atmosphere.Subsequently, this material exhaust to heating under vacuum condition, (1 to 10
-2Torr or higher) (if need words) then, is placed in the He atmosphere, so that the gas that in the porous glass body, adsorbs with the He displacement (air, chlorine, hydrogen chloride gas, or the like).Carry out the one or many exhaust and with He gas replacement operator after, in the atmosphere that contains He usually, make it fixed, thereby obtain prefabricated rods porous glass body heat treated (as at 1400-1600 ℃).If do not carry out exhaust, then in He atmosphere, heat-treat with many times.Aforesaid method can carry out in discrete system, or finishes in the system that He handles and vacuum-treat is carried out mutually continuously with sintering process.
Example 1
Example 1 according to first embodiment below will be described.
As the silica-based glass rod 31 among Fig. 1 is that its component of core glass is Si
2O-GeO
2, the cortex glass ingredient is SiO
2, core skin external diameter ratio is 1/3, the refringence between core skin glass is 0.3%.These glass stick 31 diameters are 15mm, and long is 500mm.
The diffusion particle diameter is the SiO of 0.6 to 20 μ m in pure water
2Fine particle, the powder for preparing the about 2000cps of viscosity is starched, as powder slurry 32.This powder slurry is poured in the container 14 of powder slurry irrigator 11 in advance.
With internal diameter be 120mm, deeply for the quartzy mould of the vapor phase process of 500mm as mould 21, it has the performance of suction and dehydration.
As in the past in the first embodiment as described in, glass stick 31 is placed mould 21,32 in powder slurry injects moulds 21 by powder slurry irrigator 11, and keeps this state 6 hours.
So, formed porous glass precast body 33 round glass stick 31.
With glass stick 31 porous glass precast body 33 is taken out from mould 21, put into electric furnace, be heated to 100 ℃, kept 12 hours as moisture eliminator.
The result has formed silica glass base material 35.More particularly, prepared quartzy 34.
This base material 35 is inserted into a top temperature rotatably with the speed of 250mm per hour to remain in 1450 ℃ the electric furnace.Thus, porous glass body 34 is sintered into transparent glass workpiece (dehydration, purifying, vitrifying), thereby obtains preform 37.
In operation, He and Cl
2Flow with 5l/min and 0.2l/min is supplied with stove, forms a kind of atmosphere (to dewater/purifying process and consolidation technique) in stove.
The prefabricated rods external diameter that is obtained thus is 62.5mm, and long is 300mm.
Wire-drawing frame with routine is made the single-mode fiber that external diameter is 125 μ m to this preform.
The single-mode fiber that obtains is in this way carried out the measurement of transmission performance at 1.55 μ m wavestrip places.Its result is for being 0.18dB/km in 1.55 mum wavelength place losses.
It is favourable that this result compares with the transmission performance of the single-mode fiber that makes with the synthetic VAD method of conventional for example total man worker.
In above-mentioned particular instance, when forming 5 kinds with powder slurry 32 when making 5 kinds of silica glass base materials (powder slurry injection speed 300l/min) that the optical fiber base material uses, about 3.7 hours of the treatment time of each material, and thin SiO
2Particulate output is 95%.
On the other hand, when making the silica glass base material suitable, work as SiO with example with conventional OVD method
2When a powder average deposition speed with 3g/min deposited, the treatment time was about 10 hours, and SiO
2The particulate productive rate is 30%.
By as can be seen above,, can make high yield and high efficiency porous glass body according to method of the present invention.
Example 2
Example 2 according to second example approach below will be described.
Diffusion 400 gram particle diameters are that quartzy powder 44 and 400 particle diameters of 1-20 μ m are the quartzy powder 45 of 0.6-1 μ m in pure water, prepare two kinds of silica powder slurries, and each particle is 1: 0.5 with the ratio of pure water.
With internal diameter is 30mm, and the water-absorbing resin mould of long 300mm is as mould 21.Silica-based glass rod 31, external diameter are 2mm, use GeO
2Mix (with the refringence of quartz be 1%), this rod is placed the middle position of mould 21.
The container 43a of two different inner diameters and 43b be placed on coaxially glass stick 31 around.The powder slurry of rubble English particle 44 is injected into around the glass stick 31 by container 43a, and the powder of microlith English particle 45 slurry is injected into the outer peripheral areas of powder 44 by container 43b.At this moment, container 43a and 43b promote gradually.After in this way having poured into, these powder slurries stay put, and water is absorbed by mould 21, thereby make a precast body.When its water-content is reduced to 10～15%, resulting precast body is shifted out from mould 21.
The precast body that shifts out is dry under 100 ℃, to obtain a silica glass base material 49 of forming by glass stick 31 and porous glass body 46.By the powder purification process of routine, with this base material 49 under 1000 ℃, at He and Cl
2Purifying is 2 hours in the atmosphere, and is fixed under 1500 ℃, He atmosphere then, thereby obtains vitrified preform 54.
The external diameter that records this preform 54 is 25mm, and long is 250mm.This prefabricated rods 54 is drawn into the optical fiber that external diameter is 125 μ m.Recording the transmission loss of this optical fiber at 1.55 mum wavelength places is 0.7dB/km.
Make 10 prefabricated rods with aforesaid method.Both do not found thereon that the crack do not find crackle yet, after fixed, do not had bubble.
Example 3
Example 3 according to the 3rd embodiment below will be described.
Diffusion 1000 gram particles directly are the quartz powder of 1-20 μ m in the container of 1.5 liters of pure water by filling one, and stir the diffusion system of gained thereupon.
Also use a resin mold, so that a silica-based glass rod is placed on the central authorities of mould, this rod VAD manufactured has about 1/3 core skin external diameter ratio.This powder slurry is injected in the mould.
The precast body of gained is thus shifted out from mould, in a stove with 110 ℃ temperature drying.Thereby obtain a silica glass base material of forming by this glass stick and porous glass body (precast body).
Then, the end of porous glass body is whittled into shape shown in Fig. 7 A and Fig. 7 B with lathe.
With the silica glass base material of turning by this way under 800-1200 ℃ of condition at He and Cl
2In heat-treat, thereby make its dehydration.Then the leading end of this material from it little by little heated, at He and O
2Under 1500-1650 ℃ of condition that it is fixed in the mixed atmosphere, thus the predispersed fiber molding obtained.
This preform is drawn into optical fiber, and its measured transmission loss at 1.55 mum wavelength places is 0.2dB/km.
Then, this silica glass base material with porous vitreum end shape that the above mode is made and conventional cylindrical base material are at the productive rate of qualified product (do not have crackle on base material and break), compare aspect the defensive ability/resistance ability of the defective that caused by bubble and analogue and overall yield.Its comparative result is shown in table 2.
Table 2
Prior art example 3
Qualified productive rate (%) 70 95
Still, zero defect rate (%) 60 90
Overall yield (%) 42 86
From table 2, can find out, exceed twice basically according to the productive rate of example 3 resulting productivity ratio ordinary methods.
Example 4
The preferred example of handling the method for silica glass base material below will be described.
In a water container, directly be that the quartz powder of 0.6-10 μ m diffuses in the water with 400 gram particle degree, prepare the powder slurry with the ratio of 1: 0.5 powder and water.On the other hand, the plug (glass stick) with the 2mm external diameter is placed on the central authorities that internal diameter is the water-absorbing resin mould of 30mm, long 300mm.In this state, the powder slurry is injected in the mould, thereby the water in the powder slurry is absorbed by resin mold, and formation precast body, when the quartz powder precast body becomes the suitably high precast body of intensity, it is shifted out from mould, at this moment, it sticks on the external peripheral surface of plug, and has formed silica glass base material.With thus obtained material under 70 ℃ of conditions dry 5 hours, then with the silica glass base material of gained at Cl
2With handled 2 hours with ordinary method in the He atmosphere, under 1100 ℃ of conditions.Thereby water in material and impurity are removed, and make it purifying more., this material is moved in the vacuum vessel, and to remain on temperature be that 1100 ℃, vacuum tightness are 10 thereupon
-3Torr to 10
-4Under the condition of torr, to remove gas.Then import He,, and this base material remained on wherein 30 minutes so that reach standard atmosphere pressure.This capacity is taken out a vacuum so that degas again with above-mentioned vacuum tightness, import He gas, make it to reach standard atmosphere pressure, and unload to normal temperature this material is cold keeping under the non-pressurized situation.This material moves to rapidly in the consolidation device then, and adds hot consolidation by ordinary method in He gas atmosphere, under 1500 ℃ of conditions.Resulting prefabricated rods external diameter is 27mm and the long 260mm of being, and still.When the method according to this example prepared 10 prefabricated rods, they did not all have bubble.Can judge that these prefabricated rods are without any practical problems.
Example 5
According to example 4 preparation silica glass base materials, and use Cl
2Purifying.The material 60 of purifying is arranged in the core pipe 61 of equipment as shown in Figure 8.Gas processing stove 62 among Fig. 8 is heated to 1100 ℃, closes hermatic door 64.By vent valve 65 emission gases, so that vacuum tightness reaches 10
-2To 10
-3The level of torr kept this state 30 minutes.Then, by first gas feed 66, the flow importing He gas with 0.3l/min makes this material be filled by He gas, and kept its place 30 minutes in this state.Subsequently, open air door 64, stop the gas by import 66 supply He, and material 60 descends gradually and enter in the consolidation furnace 63, this moment, this stove was heated to 1500 ℃, simultaneously by second inlet mouth 67, with the flow importing He gas of 0.5l/min.The prefabricated rods of gained is 27mm through measuring its external diameter, and long is 260mm, and does not have bubble, when the method with this example prepares ten prefabricated rods, has obtained same result.Can judge the problem of these prefabricated rods without any practicality.When the equipment with Fig. 8 prepared example 5, its gas processing and consolidation process can be carried out continuously, so its result is better than example 4, and this moment, there was not pollution in material in moving, and higher operation efficiency has been guaranteed higher productivity.
Claims (11)
1, a kind of method that is used to make silica glass base material is characterized in that comprising the following steps:
Silica based rod 31 is inserted into the hollow space of mould 21 with suction and dewatering;
Powder slurry 32 is filled in the space of the shaping mould between glass stick 31 and described mould 21 internal surfaces, and this powder slurry 32 obtains by diffusion quartz glass powder in pure water, thereby forms porous glass precast body 34 around glass stick 31.
2, by the method for claim 1, it is characterized in that: described glass stick 31 is to prepare with the chemical vapor deposition hydrolysis method.
3, by the method for claim 2, it is characterized in that: described glass stick 31 is to prepare with the VAD method.
4, according to the method for the manufacturing silica glass base material of claim 1, it is characterized in that: the mean particle size range of described fused silica powder powder material is between 0.6-20 μ m.
5, according to the method for claim 1, it is characterized in that powder slurry with the glass powder material (44) of relatively large particle diameter is filled between glass stick 31 and the mould internal surface middle portion near the modular space of glass stick 31, and will be relatively be filled into shaping mould spatial peripheral portion than the powder slurry of the glass powder material 45 of small particle size.
6, according to the method for claim 5, it is characterized in that: the average particle size range of described larger particles glass powder material is between the 1-20 μ m, and the average particle size range of described less particulate glass powdered material is between the 0.6-1 μ m.
7, according to the method for claim 1, it is characterized in that: the both ends or one end of described porous glass body 34 are made into that circular cone forms or radius-of-curvature is equal to or greater than the three-dimensional bending surface of this precast body external diameter.
8, according to the method for claim 1, it is characterized in that: prepare preform with described silica glass base material.
9, a kind of method that is used to handle silica glass base material, wherein in the powder slurry 32 shaping mould spaces that are injected between glass stick and mould 21 internal surfaces, this powder slurry is to be obtained by diffusion fused silica powder powder material in pure water, thereby around forming the porous glass precast body on this glass stick 31, this silica glass base material comprises glass stick 31 and porous glass body 34, and described method comprises step:
This base material is dewatered and purifying;
This material is placed nitrogen atmosphere, make the gas in this material of nitrogen replacement; And fixed this material in containing helium.
10, according to the method for claim 9, wherein further be included in dehydration-purifying process and replace with helium between the technology of the gas in this base material, have one under vacuum condition this material of heating make this material deflated step simultaneously.
11, according to the method for claim 9, it is characterized in that: prepare preform with described silica glass base material.
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP224732/90 | 1990-08-27 | ||
| JP22473290 | 1990-08-27 | ||
| JP92028/91 | 1991-04-23 | ||
| JP122695/91 | 1991-04-25 | ||
| JP122752/91 | 1991-04-25 | ||
| JP3122695A JPH04325432A (en) | 1991-04-25 | 1991-04-25 | Production of optical fiber preform |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1061203A CN1061203A (en) | 1992-05-20 |
| CN1026777C true CN1026777C (en) | 1994-11-30 |
Family
ID=26459778
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91109288 Expired - Fee Related CN1026777C (en) | 1990-08-27 | 1991-08-27 | Method for manufacturing silica glass base material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1026777C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198201A (en) * | 2015-10-21 | 2015-12-30 | 长飞光纤光缆股份有限公司 | Preparation method of silica glass prefabricated member |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4742429B2 (en) * | 2001-02-19 | 2011-08-10 | 住友電気工業株式会社 | Method for producing glass particulate deposit |
-
1991
- 1991-08-27 CN CN 91109288 patent/CN1026777C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198201A (en) * | 2015-10-21 | 2015-12-30 | 长飞光纤光缆股份有限公司 | Preparation method of silica glass prefabricated member |
| CN105198201B (en) * | 2015-10-21 | 2019-02-12 | 长飞光纤光缆股份有限公司 | A kind of preparation method of silica glass preform |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1061203A (en) | 1992-05-20 |
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