CN104513006A - Method for manufacturing glass base materials for optical fibers - Google Patents

Method for manufacturing glass base materials for optical fibers Download PDF

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Publication number
CN104513006A
CN104513006A CN201410512950.2A CN201410512950A CN104513006A CN 104513006 A CN104513006 A CN 104513006A CN 201410512950 A CN201410512950 A CN 201410512950A CN 104513006 A CN104513006 A CN 104513006A
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CN
China
Prior art keywords
mother metal
sintered glass
glass mother
base material
glass base
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Pending
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CN201410512950.2A
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Chinese (zh)
Inventor
八木干太
楠浩二
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Abstract

The invention provides a method for manufacturing glass base materials for optical fibers, which can prevent productivity from decreasing while reducing external injury occurrence rate. The maximum diameter of a porous glass base material (2) is set as D and the inner diameter of a heating furnace (11) for performing a dehydrating and sintering step is set as d; the weight of the porous glass base material of each unit length is maintained as a preset value, and the volume density of the porous glass base material before the dehydrating and sintering step is adjusted to make 30mm<=d-D<=90mm.

Description

The manufacture method of glass base material for optical fiber
Technical field
The present invention relates to the manufacture method of glass base material for optical fiber.
Background technology
Japanese Unexamined Patent Publication 7-140334 publication describes the manufacture method of the glass base material for optical fiber comprising deposition step and dehydration sintering step.In deposition step, make frit generation flame hydrolysis to generate glass granules, to become lithosomic body on the initial part making this glass granules be deposited on rotation, make this lithosomic body grow on turning axle direction thus obtain sintered glass mother metal.In dehydration sintering step, this sintered glass mother metal is put into sintering oven sintering thus transparent glass.
Summary of the invention
[inventing the problem that will solve]
The object of this invention is to provide a kind of manufacture method of glass base material for optical fiber, this glass base material for optical fiber while reduction outer damage incidence, can prevent from productivity from declining and tries hard to realize cost reducing.
[scheme of dealing with problems]
The manufacture method of glass base material for optical fiber of the present invention is such manufacture method: by making unstripped gas generation flame hydrolysis and the initial part being deposited on rotation forming sintered glass mother metal, and by dehydration sintering step, described sintered glass mother metal transparence is obtained transparent vitreous body, wherein, the maximum outside diameter of described sintered glass mother metal is set to D, when the internal diameter of the process furnace carrying out described dehydration sintering step is set to d, the weight of the described sintered glass mother metal of per unit length is remained preset value constant and regulate the volume density of the described sintered glass mother metal before described dehydration sintering step, to make 30mm≤d – D≤90mm.
Volume density can be 0.27g/cm 3~ 0.45g/cm 3.In addition, when manufacturing sintered glass mother metal, the flow of control combustion gas can regulate external diameter.
[effect of invention]
According to the present invention, can reduce glass base material for optical fiber manufacturing processed in outer damage incidence while, prevent productivity from declining, and try hard to cost reduction.
Brief Description Of Drawings
Fig. 1 shows the schematic diagram of the manufacture method of the glass base material for optical fiber according to embodiment of the present invention.
Fig. 2 shows the schematic diagram of the relation between the internal diameter d of the process furnace used in dehydration sintering step and the maximum outside diameter D of sintered glass mother metal.
Fig. 3 shows the schematic diagram of the manufacture method of the glass base material for optical fiber according to other embodiments of the present invention.
Fig. 4 shows the chart of the relation between the difference of the internal diameter d of process furnace and the maximum outside diameter D of sintered glass mother metal and the decrement of gap d-D and hydrogen flowing quantity and outer damage incidence.
Embodiment
Be described with reference to the embodiment of accompanying drawing to the manufacture method of glass base material for optical fiber of the present invention.The present invention is not limited to these examples, and the present invention is intended to comprise whole modification that are that limited by claims and that have with claims in equal connotation and scope.
If the external diameter of sintered glass mother metal is excessive, when then sintered glass mother metal being inserted in process furnace in dehydration sintering step, the inclination of equipment or the skew of central shaft, or the bending or torsion of product may cause sintered glass mother metal contact with the internal surface of process furnace and outer damage occurs.If generation outer damage, then entirety or the part of the transparent vitreous body obtained by dehydration sintering step cannot use.On the other hand, if the external diameter of sintered glass mother metal is too small, then attenuated by the transparent vitreous body that obtains of dehydration sintering step, and the transparent vitreous body and the staple length that obtains also shortens of stretching, therefore productivity is deteriorated.
Fig. 1 shows the schematic diagram of the manufacture method of the glass base material for optical fiber according to embodiment of the present invention.In present embodiment, form sintered glass mother metal (glass microbead deposit) by VAD (Vapor Phase Axial Deposition, vapor axial deposits) method.
In VAD method, first initial part 1 is suspended in reaction vessel 3.In this condition, initial part 1 is pivoted, and sprayed the glass granules generated by burner 4, thus form sintered glass mother metal (glass microbead deposit) 2.Now, glass raw material gas, incendivity gas and combustion-supporting property gas is supplied to burner 4.Then, burner 4 forms flame by incendivity gas and combustion-supporting property gas.In flame, make glass raw material gas generation flame hydrolysis to generate glass granules.Use (such as) SiCl 4as glass raw material gas.In addition, (such as) hydrogen (H is used 2) as incendivity gas.In addition, (such as) oxygen (O is used 2) as combustion-supporting property gas.
It is known that when forming sintered glass mother metal 2, by the flow of the hydrogen as incendivity gas, the bulk density change of sintered glass mother metal 2 changes.If the flow of hydrogen increases, then because the temperature of flame rises, volume density becomes large, if flow reduces, then because the temperature of flame reduces, volume density diminishes.Utilizing this rule, by controlling the flow of hydrogen, the volume density of formed sintered glass mother metal 2 can be regulated.Further, when the glass raw material gas equivalent supplied, volume density is larger, and the external diameter of the sintered glass mother metal 2 formed is thinner (contrary, volume density is less, and its external diameter is thicker).
In present embodiment, while the weight of the sintered glass mother metal 2 making per unit length is preset value, control the flow of hydrogen to regulate the volume density of sintered glass mother metal 2.The maximum outside diameter of sintered glass mother metal 2 is set to D, and when the internal diameter of the process furnace 11 (with reference to Fig. 2) carrying out aftermentioned dehydration sintering step is set to d, forms sintered glass mother metal 2 in the mode of 30mm≤d – D≤90mm.
It should be noted that, when increasing the flow as the oxygen of combustion-supporting property gas at the flow not changing hydrogen, the temperature of flame can decline.Further, if the temperature step-down of flame, then the settled density of glass granules diminishes.That is, if increase the flow of oxygen, then the volume density of sintered glass mother metal 2 diminishes.Utilize this rule, control the flow of oxygen, the volume density of sintered glass mother metal 2 can be regulated.Thus, the flow of oxygen or the flow of hydrogen and oxygen can be controlled, thus regulate the volume density of sintered glass mother metal 2, and form sintered glass mother metal 2 in the mode making the maximum outside diameter D of sintered glass mother metal 2 fall into above-mentioned scope.
But when by regulating oxygen thus making sintered glass mother metal diameter than generalized case thicker (making volume density diminish), need to flow into oxygen more more than generalized case, this becomes the major cause that cost increases.Therefore, preferably, regulate hydrogen, it can make sintered glass mother metal diameter thicker than generalized case with the amount more less than generalized case.
Fig. 2 shows the schematic diagram of the relation between the internal diameter d of the process furnace 11 used in dehydration sintering step and the maximum outside diameter D of sintered glass mother metal.Processed and sintering (dehydration sintering step) are carried out as follows to the sintered glass mother metal 2 as above obtained.Sintered glass mother metal 2 is inserted in process furnace 11.Time in the process furnace 11 sintered glass mother metal 2 being inserted into internal diameter d, the distance between the surface of part (part of maximum outside diameter D) the thickest on the internal surface of process furnace 11 and sintered glass mother metal 2 is (d-D)/2.
If the external diameter of sintered glass mother metal 2 is excessive, then, when sintered glass mother metal being inserted process furnace 11 in dehydration sintering step, contact with the internal surface of process furnace 11, sintered glass mother metal generation outer damage.On the other hand, if the external diameter of sintered glass mother metal 2 is too small, then the transparent vitreous body obtained by dehydration sintering step attenuates, and therefore productivity is deteriorated.Therefore, preferably, do not contact with the internal surface of process furnace 11 when the thickest partial insertion and occur in the scope of outer damage, make sintered glass mother metal 2 diameter thicker and formed.Therefore, in present embodiment, as mentioned above, sintered glass mother metal 2 is formed in the mode of maximum outside diameter D in the scope of 30mm≤d – D≤90mm.
Then, imported by gas introduction channel 12 in the process furnace 11 being inserted with sintered glass mother metal 2 also comprise SiCl except comprising the rare gas elementes such as He 4, Cl 2deng the importing gas of corrosive gases, and heat with well heater 13 thus carry out processed.Thereafter, make it to rise to sintering temperature with well heater 13 heating further, make it transparence by sintered porous base glass material 2, thus obtain transparent vitreous body.The glass base material for optical fiber of transparence is manufactured by such as upper type.
According to the present embodiment, adjusted volume density, and form sintered glass mother metal 2 relative to the gap d-D (hereinafter referred to as gap d-D) of process furnace 11 for the mode of 30mm≤d – D≤90mm with sintered glass mother metal 2.When gap d-D is less than 30mm, from the investigation of embodiment described later and comparative example, outer damage incidence sharply increases.In addition, when gap d-D is more than 90mm, the external diameter of sintered glass mother metal is too small, and the transparent vitreous body therefore obtained by dehydration sintering step attenuates, productivity is deteriorated.But if the weight of the sintered glass mother metal 2 of per unit length departs from preset value (fluctuation), then cannot manufacture the glass base material for optical fiber after transparent glass equably, the characteristic of optical fiber also can fluctuate.Therefore, adjusted volume density does not depart from preset value with the weight of the sintered glass mother metal making per unit length.
In addition, if volume density is less than 0.27g/cm 3, then the weakened of glass granules body (ス ス body), therefore easily breaks.If be greater than 0.45g/cm 3, then the overlong time of cost during sintering.Therefore, by volume density is located at 0.27g/cm 3~ 0.45g/cm 3scope in, can not have to break, the elongated such shortcoming of sintering time and gap d-D form sintered glass mother metal 2 for the mode of 30mm≤d – D≤90mm.
In addition, generally speaking, as a rule, the maximum outside diameter D of sintered glass mother metal is fully less than the internal diameter d of process furnace during fabrication, have more than needed, in order to gap d-D is adjusted to 30mm≤d – D≤90mm, need to make sintered glass mother metal diameter thicker than generalized case.When diminishing when making volume density to make the external diameter of sintered glass mother metal 2 become large, external diameter is regulated by the flow of control combustion gas (hydrogen), the amount ratio normal conditions of the hydrogen used during formation sintered glass mother metal 2 can be made to reduce, therefore, it is possible to reduce manufacturing cost.
Fig. 3 shows the schematic diagram of the manufacture method of the glass base material for optical fiber according to other embodiments of the present invention.Also go for employing the perpendicular type of more than 1 or 2 burner or OVD (OutsideVapor Deposition, the Outside Vapor deposits) method of horizontal type according to the manufacture method of glass base material for optical fiber of the present invention.As the example of manufacturing installation of sintered glass mother metal utilizing OVD method, illustrate in Fig. 3 and used the perpendicular type (a) of 3 burners 41,42,43 and the device of horizontal type (b).Identical with the situation of the device of Fig. 1, when using these devices, the same hydrogen flowing quantity preferably controlling each burner 41,42,43, thus regulate the volume density of sintered glass mother metal 2.
Next, embodiment and comparative example are described.Initial part 1 is inserted in the reaction vessel 3 of Fig. 1, control the flow of hydrogen, thus adjust the volume density of the sintered glass mother metal 2 formed, in embodiment 1 ~ 5 and comparative example 1,2, form sintered glass mother metal 2 respectively to be formed as the maximum outside diameter D set respectively.It should be noted that, in each embodiment and comparative example, glass raw material gas (SiCl 4), combustion-supporting property gas (O 2) flow be set to identical.
Then, each sintered glass mother metal 2 formed by embodiment 1 ~ 5 and comparative example 1,2 is implemented to the process of above-mentioned dehydration sintering step, thus obtain transparent vitreous body.It is constant that the weight of the sintered glass mother metal 2 of per unit length remains preset value, and the thickness (maximum outside diameter) of therefore obtained transparent vitreous body is all substantially identical under embodiment 1 ~ 5 with all situations of comparative example 1,2.
In each embodiment and each comparative example, the decrement (hydrogen decrement) investigating hydrogen flowing quantity when the hydrogen flowing quantity of comparative example 1 being set to 1, the rupture rate of sintered glass mother metal 2 formed and the outer damage incidence in order to transparent vitreous body when sintered glass mother metal 2 is put into process furnace by the sintering step that carries out dewatering.The results are shown in table 1.
Table 1
Fig. 4 shows the chart of the above results intermediate gap d-D and the relation between hydrogen decrement and outer damage incidence.Visible, when gap d-D is 25mm, outer damage incidence sharply increases.Visible in addition, along with gap d-D diminishes, hydrogen decrement becomes large roughly pro rata.
Under the condition of embodiment 1 ~ 5, hydrogen decrement during formation sintered glass mother metal 2 can be made to be more than 1%.Particularly gap d-D be 30mm, volume density is in the embodiment 5 of 0.27g/cm3, hydrogen decrement is 9.1%.In addition, in embodiment 1 ~ 5, the rupture rate of the sintered glass mother metal 2 that any one is formed is all 0%.In addition, although gap d-D less outer damage incidence is larger, when gap d-D is more than 30mm, by the sintered glass mother metal 2 formed respectively carry out dewatering sintering step process and the outer damage incidence of transparent vitreous body that obtains is less than 0.8%.
In the middle of embodiment 1 ~ 5, volume density increases to 0.45g/cm 3and gap d-D is in the embodiment 1 of 90mm, the outer damage incidence of transparent vitreous body can be made to be 0.0% and the rupture rate of sintered glass mother metal 2 can be made to be 0%.That is, even if as comparative example 1, (volume density is 0.49g/cm 3, gap d-D is 10mm) like that volume density is established larger than embodiment 1, for said external the rate of injury and rupture rate, there is no further room for improvement yet, also can produce the problem that sintering time is elongated and so on.In addition, volume density be made to become large, and the flow of increase hydrogen of just having to, therefore comparative example 1 is more than the hydrogen usage of embodiment 1, in vain Expenses Cost.That is, relative to comparative example 1, outer damage incidence, rupture rate, guaranteeing hydrogen decrement more than 1% with while reducing costs, can be maintained 0% by embodiment 1.
Further, from embodiment 1 to the result of embodiment 5, volume density is less, and hydrogen decrement is higher, and then can reduce costs.Even so, volume density is 0.26g/cm 3(gap d-D is 25mm) although comparative example 2 hydrogen decrement be 10.2%, higher than the decrement of embodiment 5, the rupture rate of the sintered glass mother metal 2 formed is 3%, and outer damage incidence is sharply increased to 6.0%.Therefore, for comparative example 2, obtain the transparent vitreous body that cannot use in wire drawing process thereafter, although therefore can reduce hydrogen consumption, the manufacturing cost of optical fiber but rises.
As mentioned above, by formed volume density be 0.27g/cm 3~ 0.45g/cm 3, gap d-D is the sintered glass mother metal 2 of 30mm≤d – D≤90mm, while reduction outer damage incidence, hydrogen usage can be reduced, and realizes cost cutting.

Claims (3)

1. a manufacture method for glass base material for optical fiber, comprising:
First operation, wherein, is deposited on the initial part of rotation by making unstripped gas generation flame hydrolysis, thus forms the sintered glass mother metal that maximum outside diameter is D, and
Second operation wherein, is made described sintered glass mother metal transparence by dehydration sintering step thus obtained transparent vitreous body in the process furnace of d at internal diameter,
Described first operation comprises such step: when the weight of the described sintered glass mother metal by per unit length remain preset value constant regulate described dehydration sintering step before the volume density of described sintered glass mother metal, to make described maximum outside diameter D and described internal diameter d for 30mm≤d – D≤90mm.
2. the manufacture method of glass base material for optical fiber according to claim 1, wherein, is set to 0.27g/cm by described volume density 3~ 0.45g/cm 3.
3. the manufacture method of glass base material for optical fiber according to claim 1 and 2, wherein, when manufacturing described sintered glass mother metal, the flow of control combustion gas is to regulate external diameter.
CN201410512950.2A 2013-10-04 2014-09-29 Method for manufacturing glass base materials for optical fibers Pending CN104513006A (en)

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JP2013208861A JP6545925B2 (en) 2013-10-04 2013-10-04 Method of manufacturing glass base material for optical fiber

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CN110171925A (en) * 2018-02-21 2019-08-27 住友电气工业株式会社 The manufacturing method of base material for optical fiber

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CN104926099A (en) * 2015-05-26 2015-09-23 江苏高科物流科技股份有限公司 Production method for high-purity glass

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AU774859B2 (en) * 2000-10-30 2004-07-08 Sumitomo Electric Industries, Ltd. Method of manufacturing optical fiber preform
JP3525922B2 (en) * 2000-10-30 2004-05-10 住友電気工業株式会社 Manufacturing method of optical fiber preform
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Publication number Priority date Publication date Assignee Title
CN110171925A (en) * 2018-02-21 2019-08-27 住友电气工业株式会社 The manufacturing method of base material for optical fiber
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Application publication date: 20150415