CN107540209A - The sintering equipment and corresponding sintering method of a kind of preform female rod - Google Patents
The sintering equipment and corresponding sintering method of a kind of preform female rod Download PDFInfo
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- CN107540209A CN107540209A CN201711014996.1A CN201711014996A CN107540209A CN 107540209 A CN107540209 A CN 107540209A CN 201711014996 A CN201711014996 A CN 201711014996A CN 107540209 A CN107540209 A CN 107540209A
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- central tube
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Abstract
The invention provides a kind of sintering equipment of preform female rod, sintered using the device, when can solve vacuum-sintering loose media, the problem of graphite heating part is oxidized, and can solve the problems, such as that bubble is more in loose media sintering process and OH contents are high, so as to obtain the sintering plug that bubble is few and OH contents are low.It includes vacuum sintering furnace, quartzy central tube is disposed with the cavity of the vacuum sintering furnace, Si-Mo rod heating member, graphite heat-insulation layer, heat-insulation layer is provided with the top of the quartzy central tube, draw bar interior interior intracavitary for extending the quartzy central tube after the heat-insulation layer, the lower end for drawing bar connects target rod by adapter sleeve, the deposition that the target rod is used for loose media is adhered to, the external annulus ring of the length direction for corresponding to loose media deposition attachment of the quartzy central tube is furnished with the Si-Mo rod heating member, the outer ring portion of the Si-Mo rod heating member is provided with the graphite heat-insulation layer of ring cloth.
Description
Technical field
The present invention relates to the technical field that preform makes, the sintering dress of specially a kind of preform female rod
Put, present invention also offers the sintering method corresponding to the device.
Background technology
At present, during preform female rod is prepared, the method being commonly used at present is prepared using Hydrolyze method
The loose media of preform female rod, its sinter molding is made using the method for sintering afterwards.The deposition process of the process is to use
SiCl4For raw material, coordinate oxyhydrogen flame, prepare loose media.Therefore, the loose media is inevitably formed with Si-O and O-H (trips
The water and hydroxyl of amorph) be main key body loose media.
Vacuum-sintering belongs to a kind of and sinters the higher sintering of efficiency, and sintered discharge gas might as well processing.Meanwhile in sintering process
In, because equipment sealing is preferable, thermal field is uniform, and the loose media bubble sintered is less, and relatively conventional sintering has very big change
Enter.Need to be passed through oxidizing gas (Cl into sintering furnace in sintering process2And O2)。
The vaccum sintering device heating mentioned in document disclosed in CN 1213650A and heat preservation member use graphite material
Material, therefore O can not be used2Carbon removal treatment is carried out to loose media.So, in sintering process, after loose media is contaminated, burning can be caused
It is unqualified to form the plug wire drawing decay of type, causes product quality to lose.
The content of the invention
In view of the above-mentioned problems, the invention provides a kind of sintering equipment of preform female rod, sintered using the device,
When can solve vacuum-sintering loose media, the problem of graphite heating part is oxidized, and can solve gas in loose media sintering process
The problem of bubble is more and OH contents are high, so as to obtain the sintering plug that bubble is few and OH contents are low.
A kind of sintering equipment of preform female rod, it is characterised in that：It includes vacuum sintering furnace, the vacuum-sintering
Quartzy central tube, Si-Mo rod heating member, graphite heat-insulation layer are disposed with the cavity of stove, is provided with the top of the quartzy central tube
Heat-insulation layer, draw bar interior interior intracavitary for extending the quartzy central tube after the heat-insulation layer, the lower end for drawing bar passes through company
Female connector connects target rod, and the deposition that the target rod is used for loose media is adhered to, and being deposited corresponding to loose media for the quartzy central tube is attached
The external annulus ring for the length direction is furnished with the Si-Mo rod heating member, and the outer ring portion of the Si-Mo rod heating member is provided with ring
The graphite heat-insulation layer of cloth, spaced cavities are reserved between the inwall of the graphite heat-insulation layer and the Si-Mo rod heating member, it is described true
Two air inlet pipe, specially the first air inlet pipe, the second air inlet pipe, first air inlet are preset with the upper portion side wall of empty sintering furnace
Pipe is passed through its inner chamber after the outer wall of the quartzy central tube, and second air inlet pipe runs through the side wall of the vacuum sintering furnace
After connect its cavity, the bottom of the quartzy central tube is provided with outer logical downtake pipe, and the vacuum sintering furnace is provided with
Logical second exhaust pipe outside.
It is further characterized by：
First air inlet pipe, the second air inlet pipe are respectively provided with pressure relative to the outside of the vacuum sintering furnace and passed
Sensor, valve mechanism, first air inlet pipe, the second air inlet pipe are external to corresponding source of the gas respectively；
The region of the non-quartzy central tube in bottom of the vacuum sintering furnace is provided with outer logical second exhaust pipe, and described first
Pressure sensor is connected on blast pipe, second exhaust pipe；
The outlet of the downtake pipe, second exhaust pipe is connected in parallel to vacuum exhaust house steward, the vacuum exhaust house steward's
The port of export is provided with vavuum pump.
A kind of sintering method of sintering equipment using preform female rod, it is characterised in that：The pine obtained will be deposited
Granular media is placed in quartzy central tube, and covers heat-insulation layer, synchronous to reduce vacuum sintering furnace inner chamber body and outer chamber pressure extremely, and is protected
Certain time A is held, afterwards while and He is passed through to the outer chamber of vacuum sintering furnace by the second air inlet pipe respectively, entered by first
The inner chamber of tracheae to quartzy central tube is passed through O2、Cl2And He, and the differential pressure ranges of both sides is always ensured that in safe range, directly
Pressure to the inner chamber of quartzy central tube reaches preset value, keeps certain time B sufficiently to remove the gas inside loose media,
Pass through Si-Mo rod heating member heat temperature raising afterwards so that OH and Cl in loose media2Sufficiently reaction, synchronous averaging vavuum pump,
Quartzy central tube external pressure is kept to be increased to relative to the big certain numerical value of internal pressure, then by the temperature of vacuum-sintering furnace interior
1500 DEG C, special time is kept, makes the abundant vitrifying of loose media, is down to 500 DEG C again afterwards, then pass through the first air inlet pipe, the
Two air inlet tracheaes are passed through N into stove simultaneously2, while keep within the pressure differential 40pa inside and outside suprasil central tube, treat pressure
When increasing to atmospheric pressure, the loose media of sinter molding is taken out.
It is further characterized by：The span of the A is 15min~25min；
The span of the B is 25min~35min.
After structure using the present invention, heated by the inner chamber of quartzy central tube, Si-Mo rod in the cavity of vacuum sintering furnace
Part and graphite insulation are formed, and it can be by O in preform female rod loose media2Or H2O is removed in the lumen, is reduced graphite and is protected
The oxidized probability of warm layer, simultaneously as this kind of device good airproof performance, can make it that temperature is more equal on the different radii circumference of section
It is even, so that loose media is heated evenly, in sintering process, because the pressure difference inside and outside quartz ampoule can not be too big, therefore pass through two
Pressure sensor on root blast pipe monitors the pressure differential on quartzy central tube both sides, by pressure difference control within 0~40Pa；
Vacuum-sintering early stage, after treating that loose media enters in stove, low-temperature bake (generally below 1000 DEG C) is first carried out to loosening body, with except
The O gone in loosening body2And H2O and other impurities class gases, avoid during the later stage sinters, in the loose media of sinter molding
There is bubble；After gas drains in loosening body, quartzy central tube is heated using Si-Mo rod heating member and then heats pine
Granular media to 1200 DEG C, the now pressure value control of the air inlet pipe of pressure sensor first in 40~50Pa, using the first air inlet pipe to
He, Cl are passed through in quartzy central tube2And O2, to remove the H not eliminated in loosening body2O (refers mainly to hydroxyl), afterwards to heating member
Continue to heat up so that SiO2The temperature of loosening body reaches 1500 DEG C, and vitrifying processing is carried out to it, to obtain the pine of sinter molding
Granular media
Brief description of the drawings
Fig. 1 is the main view schematic diagram of the present invention；
Title in figure corresponding to sequence number is as follows：
Loose media 1, draw bar 2, adapter sleeve 3, target rod 4, heat-insulation layer 5, quartzy central tube 6, Si-Mo rod heating member 7, graphite guarantor
Warm layer 8, vacuum sintering furnace 9, pressure sensor 10, valve mechanism 11, the second air inlet pipe 12, pressure sensor 13, valve mechanism
14th, the first air inlet pipe 15, pressure sensor 16, pressure sensor 17, vavuum pump 18, vacuum exhaust house steward 19, downtake pipe
20th, second exhaust pipe 21.
Embodiment
A kind of sintering equipment of preform female rod, is shown in Fig. 1：It includes vacuum sintering furnace 9, the chamber of vacuum sintering furnace 9
Quartzy central tube 6, Si-Mo rod heating member 7, graphite heat-insulation layer 8 are disposed with vivo, and the top of quartzy central tube 6 is provided with heat-insulation layer
5, draw the interior interior intracavitary for extending quartzy central tube 6 after heat-insulation layer 5 of bar 2, the lower end for drawing bar 2 passes through the connection target rod of adapter sleeve 3
4, target rod 4 is adhered to for the deposition of loose media 1, outside the length direction for corresponding to the deposition attachment of loose media 1 of quartzy central tube 6
Ring wall ring is furnished with Si-Mo rod heating member 7, and the outer ring portion of Si-Mo rod heating member 7 is provided with the graphite heat-insulation layer 8 of ring cloth, and graphite is protected
Spaced cavities are reserved between the inwall and Si-Mo rod heating member 7 of warm layer 8, two are preset with the upper portion side wall of vacuum sintering furnace 9
Air inlet pipe, specially the first air inlet pipe 15, the second air inlet pipe 12, the first air inlet pipe are led to after passing through 15 outer walls for wearing quartzy central tube 6
Enter its inner chamber, the second air inlet pipe 12 connects its cavity after the side wall of vacuum sintering furnace 9, and the bottom of quartzy central tube 6 is set
There is outer logical downtake pipe 20, vacuum sintering furnace 9 is provided with outer logical second exhaust pipe 21.
First air inlet pipe 15 is relative to being provided with pressure sensor 10, valve mechanism 11 on the outside of vacuum sintering furnace, and second
Air inlet pipe 12 is relative to being provided with pressure sensor 13, valve mechanism 14, the first air inlet pipe 15, second on the outside of vacuum sintering furnace
Air inlet pipe 12 is external to corresponding source of the gas respectively；
The region of the non-quartzy central tube 6 in bottom of vacuum sintering furnace 9 is provided with outer logical second exhaust pipe 21, first exhaust
Pipe 20 is connected with pressure sensor 16, second exhaust pipe 21 is connected with pressure sensor 17；
The outlet of downtake pipe 20, second exhaust pipe 21 is connected in parallel to vacuum exhaust house steward 19, vacuum exhaust house steward's 19
The port of export is provided with vavuum pump 18.
A kind of sintering method of sintering equipment using preform female rod：The loose media for depositing acquisition is placed in quartz
In central tube, and heat-insulation layer is covered, it is synchronous to reduce vacuum sintering furnace inner chamber body and outer chamber pressure extremely, and certain time A is kept,
Afterwards simultaneously and He is passed through to the outer chamber of vacuum sintering furnace by the second air inlet pipe respectively, by the first air inlet pipe into quartz
The inner chamber of heart pipe is passed through O2、Cl2And He, and the differential pressure ranges of both sides is always ensured that in safe range, until quartzy central tube
The pressure of inner chamber reach preset value, keep certain time B sufficiently to remove the gas inside loose media, pass through silicon molybdenum afterwards
Rod heating member heat temperature raising so that OH and Cl in loose media2Sufficiently reaction, synchronous averaging vavuum pump, keeps quartzy center
Pipe external pressure increases to 1500 DEG C relative to the big certain numerical value of internal pressure, then by the temperature of vacuum-sintering furnace interior, keeps
Special time, make the abundant vitrifying of loose media, be down to 500 DEG C again afterwards, it is then same by the first air inlet pipe, the second air inlet tracheae
N is passed through in Shi Xianglu2, while keep within the pressure differential 40pa inside and outside suprasil central tube, treat that pressure increases to atmospheric pressure
When, the loose media of sinter molding is taken out.
Specific embodiment one：With H2、O2For reacting gas, with SiCl4For raw material, deposition obtains 0.1~0.4g/cm of density3
Loose media 1.The loose media 1 for depositing acquisition is placed in the quartzy central tube 6 in the present invention, and covers heat-insulation layer 5.Synchronous drop
Low vacuum sintering furnace inner chamber body and outer chamber pressure keep 20min to below 5Pa.Pass through simultaneously and respectively the second air inlet pipe
12 are passed through He to vacuum sintering furnace outer chamber, and 2slm O is passed through by the first air inlet pipe 15 and to the quartzy inner chamber body of central tube 62、
1slm Cl2, 2slm He.The pressure of the both sides of suprasil central tube 6 is monitored by pressure sensor 16 and pressure sensor 17
Power, and it is always ensured that the differential pressure range of both sides in 0~20Pa.When vacuum sintering furnace inner chamber body pressure reaches 104Stop during pa
Ventilated to furnace chamber body and outer chamber, keep 30min, the gas inside loose media is sufficiently removed.With 10 DEG C/min speed
The temperature of loose media 1 is risen to 1200 DEG C by degree, makes OH and Cl in loose media2Sufficiently reaction, synchronous averaging vavuum pump 18, protect
Suprasil central tube external pressure is held relative to the big 30Pa of internal pressure.Again with 5 DEG C/min speed by vacuum sintering furnace
The temperature in portion increases to 1450 DEG C, keeps 30min, makes the abundant vitrifying of loose media.500 DEG C are down to 5 DEG C/min speed again,
Then N is passed through into stove by the second air inlet pipe 12 and the first air inlet pipe 15 simultaneously2, while keep in suprasil central tube 6
Within outer pressure differential 40pa, when pressure increases to 101kpa, the loose media of sinter molding is taken out.As a result OH is obtained to contain
Measure the sintering plug for being 1 for 0.6ppb and bubble number.
Specific embodiment two：With H2, O2For reacting gas, with SiCl4For raw material, deposition obtains 0.1~0.4g/cm of density3
Loose media 1.The loose media 1 for depositing acquisition is placed in the quartzy central tube 6 in the present invention, and covers heat-insulation layer 5.Synchronous drop
Low vacuum sintering furnace inner chamber body and outer chamber pressure keep 20min to below 5Pa.Pass through simultaneously and respectively the second air inlet pipe
12 are passed through He to vacuum sintering furnace outer chamber, and 2slm O is passed through by the first air inlet pipe 15 and to the quartzy inner chamber body of central tube 62、
1slm Cl2, 2slm He.The pressure of the both sides of suprasil central tube 6 is monitored by pressure sensor 16 and pressure sensor 17
Power, and it is always ensured that the differential pressure range of both sides in 0~20Pa.When vacuum sintering furnace inner chamber body pressure reaches 104Stop during pa
Ventilated to furnace chamber body and outer chamber, keep 30min, the gas inside loose media is sufficiently removed.With 10 DEG C/min speed
The temperature of loose media 1 is risen to 1200 DEG C by degree, makes OH and Cl in loose media2Sufficiently reaction.Synchronous averaging vavuum pump 18, protect
Suprasil central tube external pressure is held relative to the big 30Pa of internal pressure.Again with 5 DEG C/min speed by vacuum sintering furnace
The temperature in portion increases to 1500 DEG C, keeps 30min, makes the abundant vitrifying of loose media.500 DEG C are down to 5 DEG C/min speed again,
Then N is passed through into stove by the second air inlet pipe 12 and the first air inlet pipe 15 simultaneously2, while keep in suprasil central tube 6
Within outer pressure differential 40pa, when pressure increases to 101kpa, the loose media of sinter molding is taken out.As a result OH is obtained to contain
Measure the sintering plug for being 0 for 0.1ppb and bubble number.
Specific embodiment three：With H2, O2For reacting gas, with SiCl4For raw material, deposition obtains 0.1~0.4g/cm of density3
Loose media 1.The loose media 1 for depositing acquisition is placed in the quartzy central tube 6 in the present invention, and covers heat-insulation layer 5.Synchronous drop
Low vacuum sintering furnace inner chamber body and outer chamber pressure keep 20min to below 5Pa.Pass through simultaneously and respectively the second air inlet pipe
12 are passed through He to vacuum sintering furnace outer chamber, and 2slm O is passed through by the first air inlet pipe 15 and to the quartzy inner chamber body of central tube 62、
1slm Cl2, 2slm He.The pressure of the both sides of suprasil central tube 6 is monitored by pressure sensor 16 and pressure sensor 17
Power, and it is always ensured that the differential pressure range of both sides in 0~20Pa.When vacuum sintering furnace inner chamber body pressure reaches 104Stop during pa
Ventilated to furnace chamber body and outer chamber, keep 30min, the gas inside loose media is sufficiently removed.With 10 DEG C/min speed
The temperature of loose media 1 is risen to 1200 DEG C by degree, makes OH and Cl in loose media2Sufficiently reaction.Synchronous averaging vavuum pump 18, protect
Suprasil central tube external pressure is held relative to the big 30Pa of internal pressure.Again with 5 DEG C/min speed by vacuum sintering furnace
The temperature in portion increases to 1550 DEG C, keeps 30min, makes the abundant vitrifying of loose media.500 DEG C are down to 5 DEG C/min speed again,
Then N is passed through into stove by the second air inlet pipe 12 and the first air inlet pipe 15 simultaneously2, while keep in suprasil central tube 6
Within outer pressure differential 40pa, when pressure increases to 101kpa, the loose media of sinter molding is taken out.As a result OH is obtained to contain
Measure the sintering plug for being 2 for 0.5ppb and bubble number.
The specific embodiment of the present invention is described in detail above, but content is only the preferable implementation of the invention
Example, it is impossible to be considered as the practical range for limiting the invention.All impartial changes made according to the invention application range
Change and improvement etc., all should still be belonged within this patent covering scope.
Claims (7)
- A kind of 1. sintering equipment of preform female rod, it is characterised in that：It includes vacuum sintering furnace, the vacuum sintering furnace Cavity in be disposed with quartzy central tube, Si-Mo rod heating member, graphite heat-insulation layer, be provided with guarantor at the top of the quartzy central tube Warm layer, draw bar interior interior intracavitary for extending the quartzy central tube after the heat-insulation layer, the lower end for drawing bar passes through connection Set connection target rod, the deposition that the target rod is used for loose media are adhered to, and the quartzy central tube corresponds to loose media deposition attachment The external annulus ring of length direction be furnished with the Si-Mo rod heating member, the outer ring portion of the Si-Mo rod heating member is provided with ring cloth Graphite heat-insulation layer, spaced cavities, the vacuum are reserved between the inwall of the graphite heat-insulation layer and the Si-Mo rod heating member Two air inlet pipe, specially the first air inlet pipe, the second air inlet pipe, first air inlet pipe are preset with the upper portion side wall of sintering furnace Its inner chamber is passed through after the outer wall of the quartzy central tube, second air inlet pipe is after the side wall of the vacuum sintering furnace Its cavity is connected, the bottom of the quartzy central tube is provided with outer logical downtake pipe, and the vacuum sintering furnace is provided with outer Logical second exhaust pipe.
- A kind of 2. sintering equipment of preform female rod as claimed in claim 1, it is characterised in that：First air inlet Pipe, the second air inlet pipe are respectively provided with pressure sensor, valve mechanism relative to the outside of the vacuum sintering furnace, and described the One air inlet pipe, the second air inlet pipe are external to corresponding source of the gas respectively.
- A kind of 3. sintering equipment of preform female rod as claimed in claim 1, it is characterised in that：The vacuum sintering furnace The region of the non-quartzy central tube in bottom be provided with outer logical second exhaust pipe, on the downtake pipe, second exhaust pipe point Pressure sensor is not connected with it.
- A kind of 4. sintering equipment of preform female rod as claimed in claim 3, it is characterised in that：The first exhaust Pipe, the outlet of second exhaust pipe are connected in parallel to vacuum exhaust house steward, and the port of export of the vacuum exhaust house steward is provided with vavuum pump.
- A kind of 5. sintering method of sintering equipment using preform female rod, it is characterised in that：The loose of acquisition will be deposited Body is placed in quartzy central tube, and covers heat-insulation layer, synchronous to reduce vacuum sintering furnace inner chamber body and outer chamber pressure extremely, and is kept Certain time A, afterwards while and He is passed through, by the first air inlet to the outer chamber of vacuum sintering furnace by the second air inlet pipe respectively The inner chamber of pipe to quartzy central tube is passed through O2、Cl2And He, and the differential pressure ranges of both sides is always ensured that in safe range, until The pressure of the inner chamber of quartzy central tube reaches preset value, keeps certain time B sufficiently to remove the gas inside loose media, it Pass through Si-Mo rod heating member heat temperature raising afterwards so that OH and Cl in loose media2Sufficiently reaction, synchronous averaging vavuum pump, protect Quartzy central tube external pressure is held to increase to relative to the big certain numerical value of internal pressure, then by the temperature of vacuum-sintering furnace interior 1500 DEG C, special time is kept, makes the abundant vitrifying of loose media, is down to 500 DEG C again afterwards, then pass through the first air inlet pipe, the Two air inlet tracheaes are passed through N into stove simultaneously2, while keep within the pressure differential 40pa inside and outside suprasil central tube, treat pressure When increasing to atmospheric pressure, the loose media of sinter molding is taken out.
- A kind of 6. sintering method of sintering equipment using preform female rod as claimed in claim 5, it is characterised in that： The span of the A is 15min~25min.
- A kind of 7. sintering method of sintering equipment using preform female rod as claimed in claim 5, it is characterised in that： The span of the B is 25min~35min.
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| CN201711014996.1A CN107540209A (en) | 2017-10-25 | 2017-10-25 | The sintering equipment and corresponding sintering method of a kind of preform female rod |
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| CN201711014996.1A CN107540209A (en) | 2017-10-25 | 2017-10-25 | The sintering equipment and corresponding sintering method of a kind of preform female rod |
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| CN110550857A (en) * | 2019-08-19 | 2019-12-10 | 湖州维德光电科技有限公司 | Optical fiber perform gaseous economizer |
| CN111320375A (en) * | 2020-04-13 | 2020-06-23 | 远东通讯有限公司 | VAD loose body dehydration sintering device |
| CN111423106A (en) * | 2020-03-17 | 2020-07-17 | 烽火通信科技股份有限公司 | Sintering device and sintering method for loose body of optical fiber preform |
| CN112645583A (en) * | 2021-01-13 | 2021-04-13 | 烽火通信科技股份有限公司 | System and method for automatically controlling pressure in optical fiber preform sintering furnace |
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| CN110550857A (en) * | 2019-08-19 | 2019-12-10 | 湖州维德光电科技有限公司 | Optical fiber perform gaseous economizer |
| CN110550857B (en) * | 2019-08-19 | 2022-06-24 | 湖州维德光电科技有限公司 | Optical fiber perform gaseous economizer |
| CN110510863B (en) * | 2019-09-25 | 2023-12-29 | 江苏亨通光导新材料有限公司 | VAD lifting control device and corresponding control method |
| CN110510863A (en) * | 2019-09-25 | 2019-11-29 | 江苏亨通光导新材料有限公司 | A kind of VAD method hoisting control device and corresponding control method |
| CN111423106A (en) * | 2020-03-17 | 2020-07-17 | 烽火通信科技股份有限公司 | Sintering device and sintering method for loose body of optical fiber preform |
| WO2021184713A1 (en) * | 2020-03-17 | 2021-09-23 | 烽火通信科技股份有限公司 | Sintering device and sintering method for optical fiber preform soot body |
| CN111320375A (en) * | 2020-04-13 | 2020-06-23 | 远东通讯有限公司 | VAD loose body dehydration sintering device |
| CN112645583A (en) * | 2021-01-13 | 2021-04-13 | 烽火通信科技股份有限公司 | System and method for automatically controlling pressure in optical fiber preform sintering furnace |
| CN113511806A (en) * | 2021-07-02 | 2021-10-19 | 浙江富通光纤技术有限公司 | Machining method of mandrel |
| CN114735927A (en) * | 2022-04-15 | 2022-07-12 | 江苏亨芯石英科技有限公司 | Method for producing synthetic quartz material for semiconductor mask plate |
| CN115974400A (en) * | 2022-12-24 | 2023-04-18 | 藤仓烽火光电材料科技有限公司 | Loose body sintering device and loose body sintering method |
| CN116444144A (en) * | 2023-06-16 | 2023-07-18 | 武汉长进光子技术股份有限公司 | Bismuth-doped optical fiber for reducing hydroxyl content and preparation method thereof |
| CN116444144B (en) * | 2023-06-16 | 2023-08-22 | 武汉长进光子技术股份有限公司 | Bismuth-doped optical fiber for reducing hydroxyl content and preparation method thereof |
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