CN105859112A - Treating process for photosensitive quartz tube - Google Patents
Treating process for photosensitive quartz tube Download PDFInfo
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- CN105859112A CN105859112A CN201610189555.4A CN201610189555A CN105859112A CN 105859112 A CN105859112 A CN 105859112A CN 201610189555 A CN201610189555 A CN 201610189555A CN 105859112 A CN105859112 A CN 105859112A
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- quartz ampoule
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B29/00—Reheating glass products for softening or fusing their surfaces; Fire-polishing; Fusing of margins
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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- Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
Abstract
The invention relates to the technical field of production of quartz tubes, specifically to a treating process for a photosensitive quartz tube. The preparation method comprises the following five steps: disk filling, heating, cooling, heat treatment and annealing. Directed at the disadvantages of excessively large hydroxyl recovery amount of a quartz tube in the subsequent processing process, devitrification of the quartz tube due to electrode oxidization during releasing of oxygen atoms, and shortened service life of the quartz tube due to reduced luminous flux in the prior art, the invention provides a dehydroxylation process for the photosensitive quartz tube which can effectively reduce the content and the recovery amount of the hydroxyl in the quartz tube, thereby prolonging the service life of the photosensitive quartz tube.
Description
Technical field
The present invention relates to production of quartz tubes technical field, be specifically related to the process technique of a kind of photosensitive quartz ampoule.
Background technology
Quartz ampoule glass is made up of pure transparent silicon dioxide, a series of excellent process based prediction model such as have that coefficient of thermal expansion is little, high temperature resistant, electrical insulation capability is good and radiance is superior thoroughly, are a kind of the most excellent high temperature resistant lamp basic materials of electric light source industry.Current domestic quartz glass industry development is quickly; main employing electric furnace continuous smelting method produces quartz ampoule; this method at high temperature aoxidizes to prevent tungsten net heater; use hydrogen as protective gas; utilize the feature that hydrogen molecule diameter is little, penetration is strong simultaneously; when being melted by raw material glass sand, produced bubble is taken out of external, thus improves the presentation quality of product.The generation hydroxyl but the hydrogen introduced easily reacts with the oxygen in silicon dioxide, how many direct relations of hydroxy radical content service life and the quality of the fluorescent tubes such as halogen tungsten lamp.This is because lamp is when lighting, halogen cycle agent chemically reactive in high temperature makes hydroxyl escape into lamp from tube wall and in bulb, generate water, water resolves into the most rapidly hydrogen and oxygen, oxygen reacts generation tungsten oxide then with tungsten, evaporates the most immediately, and deposits on colder bubble wall, make bubble wall turn black, shorten the service life of bulb.This phenomenon is especially prevalent existence in megathermal gas-discharge lamp, is again one of key factor affecting discharge lamp startability, affects Metal halogen lamp more very.Because there being hydrogen in hydroxyl, in discharge tube, hydrogen is many, and it is high that it restarts due to voltage spikes, the easy blow-out of lamp.Therefore, in the processing technique of quartz ampoule, it is necessary to quartz glass is carried out deshydroxy process.
In prior art, Chinese invention patent mandate publication number CN103771692B discloses a kind of heavy caliber hydroxyl removal of quartz tube method, by being provided with certain heating curve and temperature retention time reaches the effect of deshydroxy, but it is unreasonable that its parameter is arranged, even if causing the hydroxy radical content in quartz tubing to decline, but during follow-up heat treatment, hydroxyl rise amount is big, shortens the service life of quartz ampoule and finished product.
Additionally, the majority that existing heat processing technique uses is single coal oxygen flame or oxyhydrogen flame, the c h bond that quartz ampoule ruptures because of deshydroxy in the course of processing can recombine-OH key, cause the rise of quartz ampoule hydroxyl.
Summary of the invention
Excessive for the hydroxyl rise amount during following process of quartz ampoule in prior art, understand oxidizing electrode when causing oxygen atom to discharge and cause quartz ampoule crystallize devitrification, luminous flux reduces and shortens the deficiency in product service life, the invention provides the deshydroxy technique of a kind of photosensitive quartz ampoule, effectively reduce the hydroxy radical content in quartz ampoule and rise amount, thus extend the service life of photosensitive quartz ampoule.
For realizing object above, the present invention is achieved by the following technical programs:
The process technique of a kind of photosensitive quartz ampoule, comprises the steps:
S1. sabot: by quartz ampoule block pattern row pattern on the graphite charging tray of at least two-layer, the quartz ampoule number of plies that every layer of graphite charging tray is stacked is 8-12 layer；
S2. heat up: under room temperature, the graphite charging tray piled up being put into deshydroxy stove, is at the uniform velocity warming up to 600 DEG C, programming rate is 4-6 DEG C/min, be incubated 20-50min；Then it is warming up to 800 DEG C by the programming rate of 3-5 DEG C/min, is incubated 20-50 minute；It is warming up to 1050 DEG C by the programming rate of 2-4 DEG C/min again, is incubated 210-250min；
S3. cooling: be naturally cooling to 650 DEG C, then pass to nitrogen, be cooled to 300 DEG C；The most air-cooled to less than 60 DEG C, come out of the stove；
S4. heat treatment: by the mixed gas of coal gas, methane gas and oxygen, the surfaces externally and internally of quartz ampoule is carried out fire throwing and process；
S5. annealing: quartz ampoule is put in annealing furnace, be warming up to 1150 DEG C by the speed of 300 DEG C/h, be incubated 30 minutes, furnace cooling, obtain product.
Further, the process technique of described photosensitive quartz ampoule, comprise the steps:
S1. sabot: by quartz ampoule block pattern row pattern on the graphite charging tray of at least two-layer, the quartz ampoule number of plies that every layer of graphite charging tray is stacked is 10 layers；
S2. heat up: under room temperature, the graphite charging tray piled up being put into deshydroxy stove, is at the uniform velocity warming up to 600 DEG C, programming rate is 5 DEG C/min, be incubated 30min；Then it is warming up to 800 DEG C by the programming rate of 4 DEG C/min, is incubated 30 minutes；It is warming up to 1050 DEG C by the programming rate of 3 DEG C/min again, is incubated 240min；
S3. cooling: be naturally cooling to 650 DEG C, then pass to nitrogen, be cooled to 300 DEG C；Open cycle blower fan is cooled to less than 60 DEG C again, comes out of the stove；
S4. heat treatment: by the mixed gas of coal gas, methane gas and oxygen, the surfaces externally and internally of quartz ampoule is carried out fire throwing and process；
S5. annealing: quartz ampoule is put in annealing furnace, be warming up to 1150 DEG C by the speed of 300 DEG C/h, be incubated 30 minutes, furnace cooling, obtain product.
Further, after described step S3 terminates, quartz ampoule is cut, back cover, crimping, special bent pipe and sealing process.
Further, in described step S4, the use ratio of the mixed gas of coal gas, methane gas and oxygen is: coal gas: methane: oxygen=2:1:5.
Further, the raw material that described photosensitive quartz ampoule uses is SiO2Content quartz, aluminium oxide and bismuth silicate more than 99.98%.
Further, when described photosensitive quartz ampoule is in deshydroxy stove, in holding deshydroxy stove, relative pressure is 9 × 10-5MPa。
Further, described photosensitive quartz ampoule after deshydroxy and heat treatment, hydroxy radical content≤1ppm in body.
Compared with prior art, the method have the advantages that
1, use Multi-layer graphite charging tray to bank up quartz ampoule, improve yield and work efficiency；
2, by optimizing every heating and heat preservation parameter of deshydroxy technique so that photosensitive quartz ampoule is hydroxy radical content≤1ppm after deshydroxy；Hydroxyl rise amount≤20ppm；
3, improve the service life of product, 15000 hours can be extended to the service life of photosensitive quartz ampoule；
4, use the mixed gas of coal gas, methane and oxygen as thermal source during heat treatment, reduce the hydroxyl rise rate of quartz ampoule, and improve heating efficiency, can effectively reduce the energy consumption of 20%.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below in conjunction with embodiments of the invention, the technical scheme in the embodiment of the present invention is clearly and completely described.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
Embodiment
1
:
The process technique of a kind of photosensitive quartz ampoule, comprises the steps:
S1. sabot: will be by SiO2The quartz ampoule block pattern row pattern of the quartz of content >=99.98%, aluminium oxide and bismuth silicate composition is on the graphite charging tray of at least two-layer, and the quartz ampoule number of plies that every layer of graphite charging tray is stacked is 8 layers；
S2. heating up: under room temperature, the graphite charging tray piled up is put into deshydroxy stove, in holding deshydroxy stove, relative pressure is 9 × 10-5MPa, is at the uniform velocity warming up to 600 DEG C, and programming rate is 4 DEG C/min, is incubated 20min；Then it is warming up to 800 DEG C by the programming rate of 3 DEG C/min, is incubated 20 minutes；It is warming up to 1050 DEG C by the programming rate of 2 DEG C/min again, is incubated 210min；
S3. cooling: be naturally cooling to 650 DEG C, then pass to nitrogen, be cooled to 300 DEG C；Open cycle blower fan is cooled to less than 60 DEG C again, cooling of coming out of the stove, and cuts quartz ampoule, back cover, crimping, special bent pipe and sealing process；
S4. heat treatment: by the mixed gas that volume ratio is the coal gas of 2:1:5, methane gas and oxygen, the surfaces externally and internally of quartz ampoule is carried out fire throwing and process；
S5. annealing: quartz ampoule is put in annealing furnace, be warming up to 1150 DEG C by the speed of 300 DEG C/h, be incubated 30 minutes, furnace cooling, obtain product.
Embodiment
2
:
The process technique of a kind of photosensitive quartz ampoule, comprises the steps:
S1. sabot: will be by SiO2The quartz ampoule block pattern row pattern of the quartz of content >=99.98%, aluminium oxide and bismuth silicate composition is on the graphite charging tray of at least two-layer, and the quartz ampoule number of plies that every layer of graphite charging tray is stacked is 10 layers；
S2. heating up: under room temperature, the graphite charging tray piled up is put into deshydroxy stove, in holding deshydroxy stove, relative pressure is 9 × 10-5MPa, is at the uniform velocity warming up to 600 DEG C, and programming rate is 5 DEG C/min, is incubated 30min；Then it is warming up to 800 DEG C by the programming rate of 4 DEG C/min, is incubated 30 minutes；It is warming up to 1050 DEG C by the programming rate of 3 DEG C/min again, is incubated 240min；
S3. cooling: be naturally cooling to 650 DEG C, then pass to nitrogen, be cooled to 300 DEG C；Open cycle blower fan is cooled to less than 60 DEG C again, cooling of coming out of the stove, and cuts quartz ampoule, back cover, crimping, special bent pipe and sealing process；
S4. heat treatment: with use ratio be the coal gas of 2:1:5, methane gas and oxygen mixed gas the surfaces externally and internally of quartz ampoule is carried out fire throwing process.
S5. annealing: quartz ampoule is put in annealing furnace, be warming up to 1150 DEG C by the speed of 300 DEG C/h, be incubated 30 minutes, furnace cooling, obtain product.
Embodiment
3
:
The process technique of a kind of photosensitive quartz ampoule, comprises the steps:
S1. sabot: will be by SiO2The quartz ampoule block pattern row pattern of the quartz of content >=99.98%, aluminium oxide and bismuth silicate composition is on the graphite charging tray of at least two-layer, and the quartz ampoule number of plies that every layer of graphite charging tray is stacked is 11 layers；
S2. heating up: under room temperature, the graphite charging tray piled up is put into deshydroxy stove, in holding deshydroxy stove, relative pressure is 9 × 10-5MPa, is at the uniform velocity warming up to 600 DEG C, and programming rate is 5 DEG C/min, is incubated 40min；Then it is warming up to 800 DEG C by the programming rate of 4 DEG C/min, is incubated 40 minutes；It is warming up to 1050 DEG C by the programming rate of 3 DEG C/min again, is incubated 220min；
S3. cooling: be naturally cooling to 650 DEG C, then pass to nitrogen, be cooled to 300 DEG C；Open cycle blower fan is cooled to less than 60 DEG C again, cooling of coming out of the stove, and cuts quartz ampoule, back cover, crimping, special bent pipe and sealing process；
S4. heat treatment: with use ratio be the coal gas of 2:1:5, methane gas and oxygen mixed gas the surfaces externally and internally of quartz ampoule is carried out fire throwing process.
S5. annealing: quartz ampoule is put in annealing furnace, be warming up to 1150 DEG C by the speed of 300 DEG C/h, be incubated 30 minutes, furnace cooling, obtain product.
Embodiment
4
:
The process technique of a kind of photosensitive quartz ampoule, comprises the steps:
S1. sabot: will be by SiO2The quartz ampoule block pattern row pattern of the quartz of content >=99.98%, aluminium oxide and bismuth silicate composition is on the graphite charging tray of at least two-layer, and the quartz ampoule number of plies that every layer of graphite charging tray is stacked is 12 layers；
S2. heating up: under room temperature, the graphite charging tray piled up is put into deshydroxy stove, in holding deshydroxy stove, relative pressure is 9 × 10-5MPa, is at the uniform velocity warming up to 600 DEG C, and programming rate is 6 DEG C/min, is incubated 50min；Then it is warming up to 800 DEG C by the programming rate of 5 DEG C/min, is incubated 50 minutes；It is warming up to 1050 DEG C by the programming rate of 4 DEG C/min again, is incubated 250min；
S3. cooling: be naturally cooling to 650 DEG C, then pass to nitrogen, be cooled to 300 DEG C；Open cycle blower fan is cooled to less than 60 DEG C again, cooling of coming out of the stove, and cuts quartz ampoule, back cover, crimping, special bent pipe and sealing process；
S4. heat treatment: with use ratio be the coal gas of 2:1:5, methane gas and oxygen mixed gas the surfaces externally and internally of quartz ampoule is carried out fire throwing process.
S5. annealing: quartz ampoule is put in annealing furnace, be warming up to 1150 DEG C by the speed of 300 DEG C/h, be incubated 30 minutes, furnace cooling, obtain product.
Compared with prior art, the method have the advantages that
1, use Multi-layer graphite charging tray to bank up quartz ampoule, improve yield and work efficiency；
2, by optimizing every heating and heat preservation parameter of deshydroxy technique so that photosensitive quartz ampoule is hydroxy radical content≤1ppm after deshydroxy；Hydroxyl rise amount≤20ppm；
3, improve the service life of product, 15000 hours can be extended to the service life of photosensitive quartz ampoule；
4, use the mixed gas of coal gas, methane and oxygen as thermal source during heat treatment, reduce the hydroxyl rise rate of quartz ampoule, and improve heating efficiency, can effectively reduce the energy consumption of 20%.
Above example only in order to technical scheme to be described, is not intended to limit；Although the present invention being described in detail with reference to previous embodiment, it will be understood by those within the art that: the technical scheme described in foregoing embodiments still can be modified by it, or wherein portion of techniques feature is carried out equivalent；And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (7)
1. the process technique of a photosensitive quartz ampoule, it is characterised in that comprise the steps:
S1. sabot: by quartz ampoule block pattern row pattern on the graphite charging tray of at least two-layer, the quartz ampoule number of plies that every layer of graphite charging tray is stacked is 8-12 layer；
S2. heat up: under room temperature, the graphite charging tray piled up being put into deshydroxy stove, is at the uniform velocity warming up to 600 DEG C, programming rate is 4-6 DEG C/min, be incubated 20-50min；Then it is warming up to 800 DEG C by the programming rate of 3-5 DEG C/min, is incubated 20-50 minute；It is warming up to 1050 DEG C by the programming rate of 2-4 DEG C/min again, is incubated 210-250min；
S3. cooling: be naturally cooling to 650 DEG C, then pass to nitrogen, be cooled to 300 DEG C；The most air-cooled to less than 60 DEG C, come out of the stove；
S4. heat treatment: by the mixed gas of coal gas, methane gas and oxygen, the surfaces externally and internally of quartz ampoule is carried out fire throwing and process；
S5. annealing: quartz ampoule is put in annealing furnace, be warming up to 1150 DEG C by the speed of 300 DEG C/h, be incubated 30 minutes, furnace cooling, obtain product.
The process technique of photosensitive quartz ampoule the most as claimed in claim 1, it is characterised in that comprise the steps:
S1. sabot: by quartz ampoule block pattern row pattern on the graphite charging tray of at least two-layer, the quartz ampoule number of plies that every layer of graphite charging tray is stacked is 10 layers；
S2. heat up: under room temperature, the graphite charging tray piled up being put into deshydroxy stove, is at the uniform velocity warming up to 600 DEG C, programming rate is 5 DEG C/min, be incubated 30min；Then it is warming up to 800 DEG C by the programming rate of 4 DEG C/min, is incubated 30 minutes；It is warming up to 1050 DEG C by the programming rate of 3 DEG C/min again, is incubated 240min；
S3. cooling: be naturally cooling to 650 DEG C, then pass to nitrogen, be cooled to 300 DEG C；Open cycle blower fan is cooled to less than 60 DEG C again, comes out of the stove；
S4. heat treatment: by the mixed gas of coal gas, methane gas and oxygen, the surfaces externally and internally of quartz ampoule is carried out fire throwing and process；
S5. annealing: quartz ampoule is put in annealing furnace, be warming up to 1150 DEG C by the speed of 300 DEG C/h, be incubated 30 minutes, furnace cooling, obtain product.
The process technique of photosensitive quartz ampoule the most as claimed in claim 1 or 2, it is characterised in that after described step S3 terminates, quartz ampoule is cut, back cover, crimping, special bent pipe and sealing process.
The process technique of photosensitive quartz ampoule the most as claimed in claim 1 or 2, it is characterised in that in described step S4, the use ratio of the mixed gas of coal gas, methane gas and oxygen is: coal gas: methane: oxygen=2:1:5.
The process technique of photosensitive quartz ampoule the most as claimed in claim 1 or 2, it is characterised in that the raw material that described photosensitive quartz ampoule uses is SiO2Content quartz, aluminium oxide and bismuth silicate more than 99.98%.
The process technique of photosensitive quartz ampoule the most as claimed in claim 1 or 2, it is characterised in that when described photosensitive quartz ampoule is in deshydroxy stove, in holding deshydroxy stove, relative pressure is 9 × 10-5MPa。
The process technique of photosensitive quartz ampoule the most as claimed in claim 1 or 2, it is characterised in that described photosensitive quartz ampoule after deshydroxy and heat treatment, hydroxy radical content≤1ppm in body.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610189555.4A CN105859112B (en) | 2016-03-30 | 2016-03-30 | A kind for the treatment of process of photosensitive quartz ampoule |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610189555.4A CN105859112B (en) | 2016-03-30 | 2016-03-30 | A kind for the treatment of process of photosensitive quartz ampoule |
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| CN105859112A true CN105859112A (en) | 2016-08-17 |
| CN105859112B CN105859112B (en) | 2018-10-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362565A (en) * | 2020-02-24 | 2020-07-03 | 东海县奥博石英制品有限公司 | Large-diameter quartz tube expanding and shrinking method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1119300C (en) * | 2000-05-25 | 2003-08-27 | 江苏省东海石英制品总厂 | Process for preparing low-hydroxyl quartz tube |
| WO2007073031A1 (en) * | 2005-12-19 | 2007-06-28 | Ls Cable Ltd. | Method for fabricating optical fiber preform with low oh concentration using mcvd process |
| CN101050054A (en) * | 2007-03-28 | 2007-10-10 | 徐胜利 | Vacuum deshydroxy method for quartz glass cell |
| CN203683355U (en) * | 2013-12-09 | 2014-07-02 | 江苏太平洋石英股份有限公司 | Feeding device for vacuum dehydroxylation of semiconductor quartz glass tube |
-
2016
- 2016-03-30 CN CN201610189555.4A patent/CN105859112B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1119300C (en) * | 2000-05-25 | 2003-08-27 | 江苏省东海石英制品总厂 | Process for preparing low-hydroxyl quartz tube |
| WO2007073031A1 (en) * | 2005-12-19 | 2007-06-28 | Ls Cable Ltd. | Method for fabricating optical fiber preform with low oh concentration using mcvd process |
| CN101050054A (en) * | 2007-03-28 | 2007-10-10 | 徐胜利 | Vacuum deshydroxy method for quartz glass cell |
| CN203683355U (en) * | 2013-12-09 | 2014-07-02 | 江苏太平洋石英股份有限公司 | Feeding device for vacuum dehydroxylation of semiconductor quartz glass tube |
Non-Patent Citations (1)
| Title |
|---|
| 王承遇等主编: "《玻璃材料手册》", 31 January 2008 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362565A (en) * | 2020-02-24 | 2020-07-03 | 东海县奥博石英制品有限公司 | Large-diameter quartz tube expanding and shrinking method |
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| CN105859112B (en) | 2018-10-23 |
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