CN1152835C - Method of producing glass article and glass base material for optical fiber - Google Patents
Method of producing glass article and glass base material for optical fiber Download PDFInfo
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- CN1152835C CN1152835C CNB998103616A CN99810361A CN1152835C CN 1152835 C CN1152835 C CN 1152835C CN B998103616 A CNB998103616 A CN B998103616A CN 99810361 A CN99810361 A CN 99810361A CN 1152835 C CN1152835 C CN 1152835C
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
- C03B37/0146—Furnaces therefor, e.g. muffle tubes, furnace linings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
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- Manufacture, Treatment Of Glass Fibers (AREA)
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Abstract
The present invention provides a high-quality, large glass article and a method of producing it; specifically, a long (1000 mm or longer) glass base material for optical fiber which is small in lengthwise variation and a method of producing it, the method comprising the first heating step of inserting a glass fine grain deposit synthesized by vapor phase synthesizing method into a heating furnace perpendicularly, heating the deposit at temperatures lower than a transparentizing temperature in a vacuum or depressurized atmosphere, removing gas remaining in the glass fine grain deposit and shrinking the deposit by heating, and the second heating step of heating the deposit at a transparentizing temperature to transparentize the glass fine grain deposit, characterized in that the second heating step controls heating for a preset time of not shorter than 70 min so that a glass fine grain deposit surface temperature is 1400 to 1480 DEG C and is followed by a cooling step for cooling the glass article.
Description
Technical field
The present invention relates to a kind of high-quality large glass article and manufacture method thereof, particularly relate to long size and glass base material for optical fiber and manufacture method thereof that outside diameter tolerance is little.
Background technology
In the manufacturing processed of photomask with glass articles such as base glass material and glass base material for optical fiber, in process furnace, under vacuum or reduced atmosphere, to carrying out high-temperature heating treatment, make its transparence by vapor axial deposition method (VAD method) or appearance vapour deposition gas phase synthesis method synthetic glass particulate stacked bodies such as (OVD methods).In order to obtain high-quality glass article, need do one's utmost to eliminate bubble residual in base glass material, and make the external diameter homogenizing of this mother metal.Method as using has the spy and opens the method that proposes in the flat 6-2560356 communique, wherein, will heat the transparence operation and be divided into 3 operations, suitably controls the temperature of each operation.The method is characterized in that: heat treated comprise the 1st heating process of removing the gas that residues in the glass particulate stacked body, than the Heating temperature of above-mentioned the 1st heating process high but carry out under than the low temperature of the transparence temperature of above-mentioned accumulation body heat shrink the 2nd heating process, and under above-mentioned transparence temperature, make the 3rd heating process of above-mentioned accumulation body transparence.In addition, in the 2nd heating process of this method, the heating element with the heating glass particulate stacked body is divided into multistage along the vertical direction, makes to distinguish controlled temperature independently, thereby has the effect of the external diameter variation that reduces the glass article length direction.
In recent years, from the viewpoint of the high efficiency of the necessity produced in enormous quantities and manufacturing process, wish to establish and use large-scale glass particulate stacked body factory length more than 1000mm and the method for the fibre parent material of superior in quality (no bubble is residual and the variation external diameter length direction is little).
The inventor finds, in the big length of influence of deadweight is glass base material for optical fiber more than the 1000mm, carries out above-mentioned the 3rd heating process when building heat treated under the high temperature (1490-1600 ℃), has the big problem of variation of the length direction of external diameter.
In addition, the inventor finds, when the transparence temperature is lower than 1490 ℃, as heat-up time below 1 hour, then the transparence of above-mentioned accumulation body becomes difficult, exists the two ends of above-mentioned accumulation body the problem of insufficient of heating (not the part of transparence) fully to occur.
Summary of the invention
The object of the present invention is to provide a kind of manufacture method that can obtain the stable large-scale high-quality glass article of length direction top external diameter from large-scale glass particulate stacked body.
The 1st invention relates to the manufacture method of the glass article more than a kind of length 1000mm or the 1000mm, have the 1st heating process and the 2nd heating process, in the 1st heating process, to be inserted into process furnace along vertical direction by the sub-accumulation body of gas phase synthesis method synthetic gas particles, in vacuum or reduced atmosphere, heat with the temperature lower than transparence temperature, remove residual gas in the above-mentioned glass granules daughter, and make it carry out heat shrink, in the 2nd heating process, under the transparence temperature, heat, make above-mentioned glass granules daughter transparence, above-mentioned the 1st heating process has under 1000 ℃-1300 ℃ temperature carries out degasification up to the degassing process that becomes the specified vacuum degree to above-mentioned gas; It is that 1400-1480 ℃ of ground is controlled that above-mentioned the 2nd heating process makes the glass particulate stacked body surface temperature, the specified time of heating more than 70 minutes or 70 minutes, after the 2nd heating process, has the refrigerating work procedure of cooled glass article.
The 2nd invention relates to the manufacture method of glass article of the 1st invention, and wherein, afore mentioned rules vacuum tightness is 10Pa or below the 10Pa.
The 3rd invention relates to the manufacture method of the glass article of the 1st invention, wherein, afore mentioned rules vacuum tightness is 10Pa or below the 10Pa, and above-mentioned the 1st heating process also has the heat shrink treatment process that heats under the temperature of 10Pa or the specified vacuum degree below the 10Pa and 1300-1400 ℃.
The 4th invention relates to the manufacture method of the glass article of the 1st invention, wherein, above-mentioned process furnace has the well heater of controlling independently respectively corresponding to a plurality of parts of length direction, is divided into a plurality of temperature of partly controlling above-mentioned glass particulate stacked body of length direction.
The 5th invention relates to the manufacture method of glass article of the 1st invention, wherein, in above-mentioned each heating process, measures the temperature of the stove core barrel that is used to isolate above-mentioned well heater and above-mentioned glass particulate stacked body, controls the temperature of each heating process according to its temperature.
The 6th invention relates to the manufacture method of the glass article of the 1st invention, and wherein, above-mentioned glass particulate stacked body is by transparent cane and is formed at the compound mother metal that its porous glass on every side partly constitutes.
The 7th invention relates to the manufacture method of glass article of the 1st invention, wherein, in above-mentioned the 2nd heating process, from the top towards the below continuously or stage ground improve the temperature on above-mentioned glass particulate stacked body surface.
The 8th invention relates to length 1000mm or the above glass base material for optical fiber of 1000mm, its formation method is, heating is by the transparent glass bar with to be formed at the compound mother metal with predetermined outside diameter that the porous glass around it partly constitutes be glass micro-ion accumulation body under the transparence temperature, make above-mentioned porous glass partially transparentization, the external diameter that makes the base glass material after the transparence the variation of length direction relatively the median of this external diameter length direction in ± 2%.
According to method of the present invention, can be easily from large glass particulate stacked body factory length 1000mm or more than the 1000mm and the median of the relative external diameter length direction of the variation of external diameter length direction ± 2% with interior fibre parent material.
Description of drawings
Fig. 1 is the diagrammatic illustration figure that the device formation of the vacuum sintering furnace that uses among the embodiment is shown.
Fig. 2 is the figure that the external diameter variation of the length direction of the fibre parent material of acquisition in embodiment 1 and the comparative example 1 is shown.
Fig. 3 is the mode chart that the temperature state of a control of embodiment 3 is shown.
Embodiment
The glass particulate stacked body that is obtained by gas phase synthesis methods such as VAD method or OVD methods in the 1st heating process, residues in the removal of gas of this accumulation body and the heat shrink of this accumulation body and handles in vacuum or reduced atmosphere.In this operation, be preferably under 1000-1300 ℃ the temperature degasification up to the specified vacuum degree that reaches below the 10Pa, after this, under the temperature of the specified vacuum degree below the 10Pa and 1300-1400 ℃, carry out heat shrink and handle.
Glass particulate stacked body after above-mentioned the 1st heating process is in the 2nd heating process, by at 1400-1480 ℃ temperature range internal heating more than 70 minutes and transparence.By Heating temperature being set in, having reduced the stretching of the above-mentioned accumulation body that deadweight causes than low 1400-1480 ℃ of existing transparence temperature.In this occasion, the both ends of this accumulation body that is easy to descend in Heating temperature though can produce not the part of transparence fully, by being set in the specified time more than 70 minutes heat-up time, can make the complete transparence in both ends of this accumulation body.Like this, by reducing the transparence temperature, length be the large-scale optical fiber of 1000mm with in the mother metal, the variation of the length direction of mother metal external diameter outside electrical path length direction median ± 2% in.
The process furnace that the present invention uses is controlled the temperature of glass particulate stacked body in order to be divided into a plurality of parts along its length, and a plurality of well heaters that can control independently respectively corresponding to a plurality of parts of length direction preferably are set.Like this, even the occasion that the glass particulate stacked body of long size is heated also can suitably be controlled easy tensile part and be difficult for the temperature of tensile part.
In the occasion of using the vertical heater vertically insert glass particulate stacked body, under temperature during heat treated, the stretching that deadweight causes takes place, exist external diameter attenuate on top, in the tendency of bottom chap.In such occasion, in the 2nd heating process, preferably the temperature on feed glass particulate stacked body surface make its from upside down side continuously or step type uprise.
In the diaphanisation process of glass particulate stacked body, for the well heater that makes this accumulation body and process furnace spaced apart, the stove core barrel that this accumulation body constitutes by the carbon material be inserted into and well heater between.
When in the above-mentioned the 1st and the 2nd heating process, temperature being controlled, use the temperature on radiation thermometer equitemperature sensor determination glass particulate stacked body surface, according to the output rating of its measured value control heater.The temperature on this accumulation body surface in most of the cases near the temperature of stove core barrel, in this occasion, also can be measured the stove core barrel temperature of easier mensuration, according to the output rating of its measured value control heater.
Further specifically describe the present invention by embodiment below
(embodiment 1a)
The glass particulate stacked body transparent glassization of using vacuum sintering furnace the method according to this invention shown in Figure 1 that employing VAD method synthetic is made of silicon oxide.In the vacuum sintering furnace of Fig. 1, symbol 1 is a glass particulate stacked body, symbol 2 is the vacuum sintering furnace body, symbol 3 is the stove core barrel, symbol 4 is a well heater, symbol 5 is the rare gas element feedway, symbol 6 and 7 is respectively the under meter that supplies to the rare gas element in stove core barrel 3 and the furnace body 2, symbol 8 and 9 is the supply pipe arrangement that leads to the rare gas element of stove core barrel 3 and furnace body 2 respectively, symbol 10 and 11 is a decompression suction pump in the stove, symbol 12 and 13 is respectively and is used for from furnace body 2 and stove core barrel 3 deflated pipe arrangements, symbol 14 is the grain crystalline style of supporting mother metal 1, symbol 15 is a loam cake, the vision slit that penetrates into stove core barrel 3 that symbol 16 is used for the surface temperature measurement of mother metal 1, and symbol 16 ' be the temperature survey vision slit of stove core barrel 3, symbol 17 is the thermometer of the surface temperature of measurement mother metal 1, symbol 18 is the thermometer of the temperature of measurement stove core barrel 3, and symbol 19 is a temperature-control device, and symbol 20 is a transverse-moving mechanism.Among the figure, be respectively arranged with gas supply and gas barrier at furnace body 2 and 3 liang of sides of stove core barrel, but also wherein either party can only be set.In addition, be provided with valve at pipe arrangement 8,9,12,13, though among the figure it is omitted.Switch these valves, can carry out the winding-up of vacuum (decompression) exhaust or gas.Thermometer 18 is also connected to temperature-control device 19, among the figure this is also omitted.
Glass particulate stacked body 1 is formed by the VAD method, external diameter 200mm, weight 30kg, useful length 1500mm.Remain in temperature under 400 ℃ the condition this accumulation body 1 is inserted into stove core barrel 3, in loam cake 15 Sealing furnaces, furnace pressure is reduced to 10Pa vacuum sintering furnace.Heat-up rate with 10 ℃/minute under this state makes the surface temperature in the whole zone of this accumulation body 1 rise to 1300 ℃, keeps 60 minutes, makes the gas that residues in this long-pending body 1 fully outgas (degassing process).
The surface temperature that then makes this accumulation body 1 rises with 5 ℃/minute speed, keeps 50 minutes (heat shrink treatment process) at 1350 ℃.
Then, the surface temperature that makes this accumulation body 1 rises with 5 ℃/minute speed, after the surface temperature in the whole zone of this accumulation body 1 reaches 1420 ℃, keeps 100 minutes, carries out transparence (transparence operation).
Afterwards, stop the heating of well heater, continue cooling, cooled glass article (refrigerating work procedure) take out goods at 600 ℃.
Learn after the size of the glass article that mensuration obtains that in the total length of effective minister's degree 1400mm, external diameter is 90 ± 0.5mm (change in outside diameter ± 0.56%), the variation of the length direction of external diameter is little, has good quality.
(embodiment 1b)
In addition, use the glass particulate stacked body 1 that replaces embodiment 1a with the compound mother metal of embodiment 1a same size,, obtained same good quality with embodiment 1a transparence similarly.This compound mother metal adds Ge to improve specific refractory power at central part, forms SiO by the VAD method around transparent cane
2The porous glass layer, this transparent glass bar has pure SiO at peripheral part
2Layer.
(embodiment 1c)
The external diameter of glass particulate stacked body 1 is 300mm, effectively minister's degree is 1500mm, weight is 60kg, after similarly carrying out degassing process, heating treatment step with embodiment 1a, the surface temperature that makes this accumulation body 1 rises with 5 ℃/minute speed, after the surface temperature in the whole zone of this accumulation body 1 reaches 1420 ℃, kept transparence 180 minutes.
Learn after the size of the glass article that measurement obtains that in the total length of effective minister's degree 1400mm, external diameter is 150 ± 1.2mm (change in outside diameter ± 0.6%), has obtained good quality.
(comparative example 1a)
Make glass particulate stacked body 1 transparent glassization with embodiment 1a same size under the following conditions by identical device.That is, the temperature of vacuum sintering furnace is remained on 400 ℃, in stove core barrel 3, insert this accumulation body 1, in loam cake 15 Sealing furnaces, furnace pressure is reduced to 10Pa.Heat-up rate with 10 ℃/minute under this state makes the surface temperature in the whole zone of this accumulation body 1 rise to 1300 ℃, keeps 6 minutes, makes the gas that residues in this accumulation body 1 fully outgas (degassing process).
The surface temperature that then makes this accumulation body 1 rises to 1350 ℃ with 5 ℃/minute speed, keeps 50 minutes (heat shrink treatment process) under this temperature.
Then, the surface temperature that makes this accumulation body 1 rises with 5 ℃/minute speed, after the surface temperature in the whole zone of this accumulation body 1 reaches 1500 ℃, keeps 60 minutes, carries out transparence (transparence operation).Afterwards, stop the heating of well heater, continue cooling, take out goods at 600 ℃.Learn after the size of the glass article that mensuration obtains that in the total length of effective minister's degree 1400mm, external diameter is 90 ± 4.5mm (change in outside diameter ± 5%), the variation of the length direction of external diameter is big.
(comparative example 1b)
The glass particulate stacked body 1 of use and embodiment 1c same size, transparence under the identical condition of comparative example 1a.Learn after the size of the glass article that mensuration obtains that in the total length of effective minister's degree 1550mm, external diameter is 150 ± 5.0mm (change in outside diameter ± 3.3%), the variation of the length direction of external diameter is big.
The result of embodiment 1a and comparative example 1a is as shown in table 1.In addition, Fig. 2 illustrates the tendency of the external diameter variation of the length direction in these examples.As can be seen, in the 2nd heating process (transparence operation), keep (better more than 100, then ideal more than 150 minutes) more than 70 minutes in the 1400-1480 lower ℃ scope (being preferably 1400-1440 ℃ scope) than prior art, prevent to stretch, very important to the stabilization of external diameter.
In an embodiment, the vacuum tightness in the stove is made as 10Pa, but residual in order to prevent the bubble in the glass article, and this numerical value hangs down some for well, can be 9Pa, 8Pa.
Method of the present invention glass article from great occasion, particularly, effective to the variation of reduction external diameter from focusing on 50kg when above.
The external diameter of the glass article of table 1 treatment condition and acquisition changes
| Embodiment 1a | Comparative example 1a | ||||
| Temperature (℃) | Time (branch) | Temperature (℃) | Time (branch) | ||
| The 1st heating process | Degassing process | 1300 | 60 | 1300 | 60 |
| The heat shrink operation | 1350 | 50 | 1350 | 50 | |
| The 2nd heating process | 1420 | 100 | 1500 | 60 | |
| The variation of external diameter (mm) | ±0.5 | ±4.5 | |||
(embodiment 2a)
Under identical temperature condition, make glass particulate stacked body 1 transparence with embodiment 1a same size with the equipment identical with embodiment 1a.In the present embodiment, use the temperature of the thermometer 18 control stove core barrels 3 of the hull-skin temperature of measuring stove core barrel 3, thereby carry out the temperature control in the transparence treating processes.Learn after the size of the glass article that mensuration obtains that in the total length of effective minister's degree 1400mm, external diameter is 90 ± 0.7mm (change in outside diameter ± 0.78%), the variation of the length direction of external diameter is little, has good quality.By this result as can be seen, by measuring the surface temperature that replaces measuring this accumulation body 1 than the temperature of the stove core barrel that is easier to measure, also no problem.
(embodiment 2b)
The glass particulate stacked body 1 of use and embodiment 1c same size, transparence under the condition identical with embodiment 1c.Learn after the size of the glass article that mensuration obtains that in the total length of effective minister's degree 1410mm, external diameter is 150 ± 1.5mm (change in outside diameter ± 1.0%), has obtained good quality.
(embodiment 3a)
Under the form identical with the vacuum sintering furnace of Fig. 1, use the vacuum sintering furnace that as shown in Figure 3 well heater 4 is divided into epimere well heater 4-1, stage casing well heater 4-2, reaches the such 3 sections controls of hypomere well heater 4-3, make glass particulate stacked body 1 transparence identical in the same manner with embodiment 1a than embodiment 1a.
The external diameter of this accumulation body 1 is 200mm, and effectively minister's degree is 1560mm.The temperature of vacuum sintering furnace is remained on 400 ℃, in stove core barrel 3, insert this accumulation body 1, in loam cake 15 Sealing furnaces, furnace pressure is reduced to 10Pa.Heat-up rate with 10 ℃/minute under this state makes the surface temperature in the whole zone of this accumulation body 1 rise to 1300 ℃, keeps 60 minutes, makes the gas that residues in this accumulation body 1 fully outgas (degassing process).
The surface temperature that then makes this accumulation body 1 rises to 1350 ℃ with 10 ℃/minute speed, keeps 50 minutes (heat shrink treatment process).
Then, make the surface temperature of central point of the scope A of this bigger accumulation body 1 of the influence that is subjected to epimere well heater 4-1 rise to 1400 ℃ with 5 ℃/minute speed, make the surface temperature of the central point of the bigger scope B of the influence that is subjected to stage casing well heater 4-2 rise to 1420 ℃ with 7 ℃/minute speed, make the surface temperature of the central point of the bigger scope C of the influence that is subjected to hypomere well heater 4-3 rise to 1440 ℃ with 9 ℃/minute speed, afterwards, kept 100 minutes, and made accumulation body 1 transparence (transparence operation).The temperature distribution of this moment substantially as shown in Figure 3.
Afterwards, stop the heating of well heater, continue cooling, cooled glass article (refrigerating work procedure) take out goods at 600 ℃.
Learn after the size of the glass article that mensuration obtains that in the total length of effective minister's degree 1405mm, external diameter is 90 ± 0.1mm (change in outside diameter ± 0.11%), the variation of the length direction of external diameter is little, has good quality.
(embodiment 3b)
In embodiment 3a, measure the surface temperature of the stove core barrel 3 corresponding with each heater locations, control the surface temperature of this accumulation body 1, also can obtain the good quality same (in the total length of effective minister's degree 1417mm, external diameter is 90 ± 0.3mm (change in outside diameter ± 0.33%)) with embodiment 3a.
(embodiment 3c)
Use the glass particulate stacked body 1 that replaces embodiment 3a with the compound mother metal of embodiment 3a same size,, obtained same good quality with embodiment 3a transparence similarly.This compound mother metal adds Ge at central part, forms pure SiO by the VAD method around transparent cane
2The porous glass layer, this transparent glass bar has pure SiO at peripheral part
2Layer.
(embodiment 3d)
In embodiment 3a, the heat shrink under having carried out 1350 ℃ is handled, but this heat shrink is handled and do not obtained good quality similarly.
(embodiment 3e)
In embodiment 3a, use the glass particulate stacked body 1 that replaces embodiment 3a with the glass particulate stacked body 1 of embodiment 1c same size, the hold-time of transparent operation is 180 minutes, at this moment, total length at effective minister's degree 1390mm, external diameter is 150 ± 0.7mm (change in outside diameter ± 0.46%), has obtained good quality equally.
(embodiment 3f)
In embodiment 3e, measure the surface temperature of the stove core barrel 3 corresponding with each heater locations, control the surface temperature of this accumulation body 1, also can obtain the good quality same (in the total length of effective minister's degree 1400mm, external diameter is 150 ± 1.0mm (change in outside diameter ± 0.66%)) with embodiment 3a.
(embodiment 3g)
Use the equipment identical under identical condition, to make glass particulate stacked body 1 transparence of external diameter 365mm, effective minister's degree 1560mm, weight 80kg with embodiment 3e.Learn after the size of the glass article that mensuration obtains that in the total length of effective minister's degree 1470mm, external diameter is 163 ± 1.5mm (change in outside diameter ± 0.92%).
(comparative example 2)
Make glass particulate stacked body 1 transparent glassization with embodiment 3g same size under the following conditions by the equipment identical with embodiment 3e.That is, the temperature of vacuum sintering furnace is remained on 400 ℃, in stove core barrel 3, insert this accumulation body 1, in loam cake 15 Sealing furnaces, furnace pressure is reduced to 10Pa.Heat-up rate with 10 ℃/minute under this state makes the surface temperature in the whole zone of this accumulation body 1 rise to 1300 ℃, keeps 60 minutes, makes the gas that residues in this accumulation body 1 fully outgas (degassing process).
The surface temperature that then makes this accumulation body 1 rises to 1350 ℃ with 5 ℃/minute speed, keeps 50 minutes (heat shrink treatment process) under this temperature.
Then, the surface temperature that makes this accumulation body 1 rises with 15 ℃/minute speed, after the surface temperature in the whole zone of this accumulation body 1 reaches 1500 ℃, keeps 60 minutes, carries out transparence (transparence operation).Afterwards, stop the heating of well heater, continue cooling, take out goods at 600 ℃.Learn after the size of the glass article that mensuration obtains that in the total length of effective minister's degree 1660mm, external diameter is 158 ± 7mm (change in outside diameter ± 4.43%), the variation of the length direction of external diameter is big.
Claims (8)
1. a length is the manufacture method of the above glass article of 1000mm or 1000mm, it is characterized in that: have the 1st heating process and the 2nd heating process, in the 1st heating process, to be inserted into process furnace along vertical direction by the sub-accumulation body of gas phase synthetic gas particles, in vacuum or reduced atmosphere, heat with the temperature lower than transparence temperature, remove residual gas in the above-mentioned glass granules daughter, and make it carry out heat shrink, in the 2nd heating process, under the transparence temperature, heat, make above-mentioned glass granules daughter transparence; Above-mentioned the 1st heating process has under 1000 ℃-1300 ℃ temperature carries out degasification up to the degassing process that becomes the specified vacuum degree to above-mentioned gas; Above-mentioned the 2nd heating process makes the glass particulate stacked body surface temperature control at 1400-1480 ℃, the specified time of heating more than 70 minutes or 70 minutes, after the 2nd heating process, has the refrigerating work procedure of cooled glass article.
2. the manufacture method of glass article as claimed in claim 1 is characterized in that: afore mentioned rules vacuum tightness is 10Pa or below the 10Pa.
3. the manufacture method of glass article as claimed in claim 1, it is characterized in that: afore mentioned rules vacuum tightness is 10Pa or below the 10Pa, and above-mentioned the 1st heating process also has the heat shrink treatment process that heats under the temperature of 10Pa or the specified vacuum degree below the 10Pa and 1300-1400 ℃.
4. the manufacture method of glass article as claimed in claim 1, it is characterized in that: above-mentioned process furnace has corresponding to the controlled independently respectively well heater of a plurality of parts of length direction, is divided into a plurality of temperature of partly controlling above-mentioned glass particulate stacked body of length direction.
5. the manufacture method of glass article as claimed in claim 1 is characterized in that: measure the temperature of the stove core barrel that is used to isolate above-mentioned well heater and above-mentioned glass particulate stacked body, control the temperature of each heating process according to its temperature.
6. the manufacture method of glass article as claimed in claim 1 is characterized in that: above-mentioned glass particulate stacked body is for by transparent cane be formed at the compound mother metal that the porous glass around it partly constitutes.
7. the manufacture method of glass article as claimed in claim 1 is characterized in that: in above-mentioned the 2nd heating process, from the top towards the below continuously or stage ground improve the temperature on above-mentioned glass particulate stacked body surface.
8. glass base material for optical fiber, it is characterized in that: its length is 1000mm or more than the 1000mm, its formation method for heating under the transparence temperature by the transparent glass bar with to be formed at the compound mother metal with predetermined outside diameter that the porous glass around it partly constitutes be glass particulate stacked body, make above-mentioned porous glass partially transparentization, make transparence base glass material external diameter the variation of length direction relatively the median of the length direction of this external diameter in ± 2%.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP244809/1998 | 1998-08-31 | ||
| JP24480998 | 1998-08-31 | ||
| JP296899 | 1999-01-08 | ||
| JP002968/1999 | 1999-01-08 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1315924A CN1315924A (en) | 2001-10-03 |
| CN1152835C true CN1152835C (en) | 2004-06-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB998103616A Expired - Lifetime CN1152835C (en) | 1998-08-31 | 1999-08-26 | Method of producing glass article and glass base material for optical fiber |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JP3777983B2 (en) |
| KR (1) | KR20010073057A (en) |
| CN (1) | CN1152835C (en) |
| AU (1) | AU755861B2 (en) |
| GB (1) | GB2357500B (en) |
| WO (1) | WO2000012438A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003183042A (en) * | 2001-12-14 | 2003-07-03 | Shin Etsu Chem Co Ltd | Method of manufacturing preform for optical fiber and preform for optical fiber manufactured by the same |
| CN102503114B (en) * | 2011-10-18 | 2013-09-18 | 江苏亨通光电股份有限公司 | Device and method for manufacturing quartz core rod for optical fiber |
| JP6011218B2 (en) * | 2012-10-03 | 2016-10-19 | 住友電気工業株式会社 | Manufacturing method of transparent glass base material |
| JPWO2020246499A1 (en) * | 2019-06-06 | 2020-12-10 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5420032B2 (en) * | 1973-07-06 | 1979-07-19 | ||
| JPS60256035A (en) * | 1984-06-01 | 1985-12-17 | Hitachi Ltd | X-ray diffraction method |
| JP2836302B2 (en) * | 1991-07-19 | 1998-12-14 | 住友電気工業株式会社 | Method for manufacturing glass articles |
| AU653411B2 (en) * | 1991-07-19 | 1994-09-29 | Sumitomo Electric Industries, Ltd. | Method for producing glass preform for optical fiber |
| JP2917729B2 (en) * | 1993-03-03 | 1999-07-12 | 住友電気工業株式会社 | Manufacturing method of optical fiber preform |
| JPH0781962A (en) * | 1993-09-16 | 1995-03-28 | Sumitomo Electric Ind Ltd | Production of optical fiber preform |
-
1999
- 1999-08-26 AU AU54437/99A patent/AU755861B2/en not_active Ceased
- 1999-08-26 JP JP2000567479A patent/JP3777983B2/en not_active Expired - Lifetime
- 1999-08-26 KR KR1020017002569A patent/KR20010073057A/en not_active Application Discontinuation
- 1999-08-26 GB GB0107542A patent/GB2357500B/en not_active Expired - Fee Related
- 1999-08-26 WO PCT/JP1999/004609 patent/WO2000012438A1/en not_active Application Discontinuation
- 1999-08-26 CN CNB998103616A patent/CN1152835C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1315924A (en) | 2001-10-03 |
| GB2357500A (en) | 2001-06-27 |
| AU755861B2 (en) | 2003-01-02 |
| JP3777983B2 (en) | 2006-05-24 |
| KR20010073057A (en) | 2001-07-31 |
| GB0107542D0 (en) | 2001-05-16 |
| GB2357500B (en) | 2001-12-12 |
| WO2000012438A1 (en) | 2000-03-09 |
| AU5443799A (en) | 2000-03-21 |
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