CN105859112B - A kind for the treatment of process of photosensitive quartz ampoule - Google Patents
A kind for the treatment of process of photosensitive quartz ampoule Download PDFInfo
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- CN105859112B CN105859112B CN201610189555.4A CN201610189555A CN105859112B CN 105859112 B CN105859112 B CN 105859112B CN 201610189555 A CN201610189555 A CN 201610189555A CN 105859112 B CN105859112 B CN 105859112B
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- quartz ampoule
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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
Abstract
The present invention relates to production of quartz tubes technical fields, and in particular to a kind for the treatment of process of photosensitive quartz ampoule.Including five sabot, heating, cooling, heat treatment and annealing steps;The present invention is excessive for quartz ampoule hydroxyl rise amount during following process in the prior art, and oxidizing electrode is understood when oxygen atom release and causes quartz ampoule crystallization devitrification, luminous flux reduces and shortens the deficiency of product service life, a kind of hydroxy radical content and rise amount that can effectively reduce in quartz ampoule is provided, the deshydroxy technique of the photosensitive quartz ampoule of service life to extend photosensitive quartz ampoule.
Description
Technical field
The present invention relates to production of quartz tubes technical fields, and in particular to a kind for the treatment of process of photosensitive quartz ampoule.
Background technology
Quartz ampoule glass is made of pure transparent silicon dioxide, have coefficient of thermal expansion is small, high temperature resistant, electrical insulation capability it is good with
And a series of excellent physical and chemical properties such as radiance is superior thoroughly, it is a kind of very excellent resistance to height of electric light source industry
Warm lamp basic material.Country's quartz glass industry development quickly, mainly produces quartz ampoule using electric furnace continuous smelting method at present, this
Tungsten net heater aoxidizes method at high temperature in order to prevent, using hydrogen as protective gas, while small using hydrogen molecule diameter,
The strong feature of penetration, generated bubble is taken out of in vitro when raw material glass sand is melted, to improve the appearance of product
Quality.But introduce hydrogen easily react with the oxygen in silica generate hydroxyl, hydroxy radical content number be directly related to
The service life and quality of the fluorescent tubes such as halogen tungsten lamp.This is because lamp, when lighting, high temperature makes hydroxyl escape into lamp from tube wall
Halogen cycle agent chemically reactive in interior and light bulb, generates water, and water resolves into rapidly hydrogen and oxygen at high temperature, oxygen after
And reacted with tungsten and generate tungsten oxide, it evaporates immediately at high temperature, and deposited in colder steep that wall, steep that wall is made to black, contract
The service life of short light bulb.The especially prevalent presence in the gas-discharge lamp of high temperature modification of this phenomenon, and be to influence discharge lamp to open
One of the key factor of dynamic performance, influences more very Metal halogen lamp.Because there is hydrogen in hydroxyl, hydrogen is more in discharge tube, restarts voltage
Spike is high, the easy blow-out of lamp.Therefore, in the processing technology of quartz ampoule, it is necessary to carry out deshydroxy processing to quartz glass.
In the prior art, it is de- to disclose a kind of heavy caliber quartz ampoule by Chinese invention patent mandate publication number CN103771692B
Hydroxyalkyl meth, by having the function that deshydroxy provided with certain heating curve and soaking time, but its parameter setting is not to the utmost
Rationally, even if causing the hydroxy radical content in quartzy tubing that can decline, but during subsequent heat treatment, hydroxyl rise amount
Greatly, the service life of quartz ampoule and finished product is shortened.
In addition, the majority that existing heat processing technique uses is single coal oxygen flame either oxyhydrogen flame, in process
Middle quartz ampoule causes the rise of quartz ampoule hydroxyl because the c h bond that deshydroxy is broken can recombine-OH keys.
Invention content
For quartz ampoule in the prior art, hydroxyl rise amount is excessive during following process, meeting when oxygen atom being caused to discharge
Oxidizing electrode simultaneously causes quartz ampoule crystallization devitrification, and luminous flux reduces and shorten the deficiency of product service life, the present invention provides
A kind of deshydroxy technique of photosensitive quartz ampoule effectively reduces hydroxy radical content and rise amount in quartz ampoule, to extend light
The service life of quick quartz ampoule.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind for the treatment of process of photosensitive quartz ampoule, includes the following steps:
S1. sabot:By quartz ampoule block pattern row pattern at least two layers of graphite charging tray, the stone stacked on every layer of graphite charging tray
English tube layer number is 8-12 layers;
S2. it heats up:Under room temperature, the graphite charging tray piled up is put into deshydroxy stove, is at the uniform velocity warming up to 600 DEG C, heating speed
Degree is 4-6 DEG C/min, keeps the temperature 20-50min;Then 800 DEG C are warming up to by the heating rate of 3-5 DEG C/min, 20-50 points of heat preservation
Clock;1050 DEG C are warming up to by the heating rate of 2-4 DEG C/min again, keeps the temperature 210-250min;
S3. it cools down:650 DEG C are naturally cooling to, nitrogen is then passed to, is cooled to 300 DEG C;It is air-cooled to 60 DEG C hereinafter, going out again
Stove;
S4. it is heat-treated:The surfaces externally and internally of quartz ampoule is carried out at fiery throwing with the mixed gas of coal gas, methane gas and oxygen
Reason;
S5. it anneals:Quartz ampoule is put into annealing furnace, 1150 DEG C is warming up to by the speed of 300 DEG C/h, keeps the temperature 30 minutes,
Furnace cooling obtains product.
Further, the treatment process of the photosensitive quartz ampoule, includes the following steps:
S1. sabot:By quartz ampoule block pattern row pattern at least two layers of graphite charging tray, the stone stacked on every layer of graphite charging tray
English tube layer number is 10 layers;
S2. it heats up:Under room temperature, the graphite charging tray piled up is put into deshydroxy stove, is at the uniform velocity warming up to 600 DEG C, heating speed
Degree is 5 DEG C/min, keeps the temperature 30min;Then 800 DEG C are warming up to by the heating rate of 4 DEG C/min, keep the temperature 30 minutes;Again press 3 DEG C/
The heating rate of min is warming up to 1050 DEG C, keeps the temperature 240min;
S3. it cools down:650 DEG C are naturally cooling to, nitrogen is then passed to, is cooled to 300 DEG C;Open cycle wind turbine is cooled to 60 again
DEG C hereinafter, coming out of the stove;
S4. it is heat-treated:The surfaces externally and internally of quartz ampoule is carried out at fiery throwing with the mixed gas of coal gas, methane gas and oxygen
Reason;
S5. it anneals:Quartz ampoule is put into annealing furnace, 1150 DEG C is warming up to by the speed of 300 DEG C/h, keeps the temperature 30 minutes,
Furnace cooling obtains product.
Further, quartz ampoule is cut after the step S3, back cover, crimping, special bent pipe and sealing
Process.
Further, the use ratio of the mixed gas of coal gas, methane gas and oxygen is in the step S4:Coal gas:First
Alkane:Oxygen=2:1:5.
Further, the raw material that the photosensitive quartz ampoule uses is SiO2Content 99.98% or more quartz, oxidation
Aluminium and bismuth silicate.
Further, when the photosensitive quartz ampoule is in deshydroxy stove, it is 9 × 10 to keep relative pressure in deshydroxy stove-5MPa。
Further, the photosensitive quartz ampoule is after deshydroxy and heat treatment, hydroxy radical content≤1ppm in tube body.
Compared with prior art, the invention has the advantages that:
1, quartz ampoule is banked up using Multi-layer graphite charging tray, improves yield and working efficiency;
2, pass through optimize deshydroxy technique every heating and heat preservation parameter so that photosensitive quartz ampoule after deshydroxy hydroxy radical content≤
1ppm;Hydroxyl rise amount≤20ppm;
3, the service life of product is improved, the service life of photosensitive quartz ampoule can extend to 15000 hours;
4, using the mixed gas of coal gas, methane and oxygen as heat source when heat treatment, the hydroxyl of quartz ampoule is reduced
Rise rate, and heating efficiency is improved, it can effectively reduce by 20% energy consumption.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the implementation of the present invention
Example, technical scheme in the embodiment of the invention is clearly and completely described.Based on the embodiments of the present invention, this field
The every other embodiment that those of ordinary skill is obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment 1:
A kind for the treatment of process of photosensitive quartz ampoule, includes the following steps:
S1. sabot:It will be by SiO2The quartz of content >=99.98%, the neat code of quartz ampoule of aluminium oxide and bismuth silicate composition
It is placed at least two layers of graphite charging tray, the quartz ampoule number of plies stacked on every layer of graphite charging tray is 8 layers;
S2. it heats up:Under room temperature, the graphite charging tray piled up is put into deshydroxy stove, it is 9 to keep relative pressure in deshydroxy stove
×10 -5MPa is at the uniform velocity warming up to 600 DEG C, and heating rate is 4 DEG C/min, keeps the temperature 20min;Then the heating rate of 3 DEG C/min is pressed
800 DEG C are warming up to, keeps the temperature 20 minutes;1050 DEG C are warming up to by the heating rate of 2 DEG C/min again, keeps the temperature 210min;
S3. it cools down:650 DEG C are naturally cooling to, nitrogen is then passed to, is cooled to 300 DEG C;Open cycle wind turbine is cooled to 60 again
DEG C hereinafter, cooling of coming out of the stove, quartz ampoule is cut, back cover, crimping, special bent pipe and sealing process;
S4. it is heat-treated:It is 2 with volume ratio:1:The mixed gas of 5 coal gas, methane gas and oxygen is in quartz ampoule
Outer surface carries out fiery throwing processing;
S5. it anneals:Quartz ampoule is put into annealing furnace, 1150 DEG C is warming up to by the speed of 300 DEG C/h, keeps the temperature 30 minutes,
Furnace cooling obtains product.
Embodiment 2:
A kind for the treatment of process of photosensitive quartz ampoule, includes the following steps:
S1. sabot:It will be by SiO2The quartz of content >=99.98%, the neat code of quartz ampoule of aluminium oxide and bismuth silicate composition
It is placed at least two layers of graphite charging tray, the quartz ampoule number of plies stacked on every layer of graphite charging tray is 10 layers;
S2. it heats up:Under room temperature, the graphite charging tray piled up is put into deshydroxy stove, it is 9 to keep relative pressure in deshydroxy stove
×10 -5MPa is at the uniform velocity warming up to 600 DEG C, and heating rate is 5 DEG C/min, keeps the temperature 30min;Then the heating rate of 4 DEG C/min is pressed
800 DEG C are warming up to, keeps the temperature 30 minutes;1050 DEG C are warming up to by the heating rate of 3 DEG C/min again, keeps the temperature 240min;
S3. it cools down:650 DEG C are naturally cooling to, nitrogen is then passed to, is cooled to 300 DEG C;Open cycle wind turbine is cooled to 60 again
DEG C hereinafter, cooling of coming out of the stove, quartz ampoule is cut, back cover, crimping, special bent pipe and sealing process;
S4. it is heat-treated:It is 2 with use ratio:1:5 coal gas, methane gas and oxygen mixed gas to quartz ampoule inside and outside
Surface carries out fiery throwing processing.
S5. it anneals:Quartz ampoule is put into annealing furnace, 1150 DEG C is warming up to by the speed of 300 DEG C/h, keeps the temperature 30 minutes,
Furnace cooling obtains product.
Embodiment 3:
A kind for the treatment of process of photosensitive quartz ampoule, includes the following steps:
S1. sabot:It will be by SiO2The quartz of content >=99.98%, the neat code of quartz ampoule of aluminium oxide and bismuth silicate composition
It is placed at least two layers of graphite charging tray, the quartz ampoule number of plies stacked on every layer of graphite charging tray is 11 layers;
S2. it heats up:Under room temperature, the graphite charging tray piled up is put into deshydroxy stove, it is 9 to keep relative pressure in deshydroxy stove
×10 -5MPa is at the uniform velocity warming up to 600 DEG C, and heating rate is 5 DEG C/min, keeps the temperature 40min;Then the heating rate of 4 DEG C/min is pressed
800 DEG C are warming up to, keeps the temperature 40 minutes;1050 DEG C are warming up to by the heating rate of 3 DEG C/min again, keeps the temperature 220min;
S3. it cools down:650 DEG C are naturally cooling to, nitrogen is then passed to, is cooled to 300 DEG C;Open cycle wind turbine is cooled to 60 again
DEG C hereinafter, cooling of coming out of the stove, quartz ampoule is cut, back cover, crimping, special bent pipe and sealing process;
S4. it is heat-treated:It is 2 with use ratio:1:5 coal gas, methane gas and oxygen mixed gas to quartz ampoule inside and outside
Surface carries out fiery throwing processing.
S5. it anneals:Quartz ampoule is put into annealing furnace, 1150 DEG C is warming up to by the speed of 300 DEG C/h, keeps the temperature 30 minutes,
Furnace cooling obtains product.
Embodiment 4:
A kind for the treatment of process of photosensitive quartz ampoule, includes the following steps:
S1. sabot:It will be by SiO2The quartz of content >=99.98%, the neat code of quartz ampoule of aluminium oxide and bismuth silicate composition
It is placed at least two layers of graphite charging tray, the quartz ampoule number of plies stacked on every layer of graphite charging tray is 12 layers;
S2. it heats up:Under room temperature, the graphite charging tray piled up is put into deshydroxy stove, it is 9 to keep relative pressure in deshydroxy stove
×10 -5MPa is at the uniform velocity warming up to 600 DEG C, and heating rate is 6 DEG C/min, keeps the temperature 50min;Then the heating rate of 5 DEG C/min is pressed
800 DEG C are warming up to, keeps the temperature 50 minutes;1050 DEG C are warming up to by the heating rate of 4 DEG C/min again, keeps the temperature 250min;
S3. it cools down:650 DEG C are naturally cooling to, nitrogen is then passed to, is cooled to 300 DEG C;Open cycle wind turbine is cooled to 60 again
DEG C hereinafter, cooling of coming out of the stove, quartz ampoule is cut, back cover, crimping, special bent pipe and sealing process;
S4. it is heat-treated:It is 2 with use ratio:1:5 coal gas, methane gas and oxygen mixed gas to quartz ampoule inside and outside
Surface carries out fiery throwing processing.
S5. it anneals:Quartz ampoule is put into annealing furnace, 1150 DEG C is warming up to by the speed of 300 DEG C/h, keeps the temperature 30 minutes,
Furnace cooling obtains product.
Compared with prior art, the invention has the advantages that:
1, quartz ampoule is banked up using Multi-layer graphite charging tray, improves yield and working efficiency;
2, pass through optimize deshydroxy technique every heating and heat preservation parameter so that photosensitive quartz ampoule after deshydroxy hydroxy radical content≤
1ppm;Hydroxyl rise amount≤20ppm;
3, the service life of product is improved, the service life of photosensitive quartz ampoule can extend to 15000 hours;
4, using the mixed gas of coal gas, methane and oxygen as heat source when heat treatment, the hydroxyl of quartz ampoule is reduced
Rise rate, and heating efficiency is improved, it can effectively reduce by 20% energy consumption.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although with reference to the foregoing embodiments
Invention is explained in detail, it will be understood by those of ordinary skill in the art that:It still can be to aforementioned each implementation
Technical solution recorded in example is modified or equivalent replacement of some of the technical features;And these modification or
It replaces, the spirit and scope for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution.
Claims (7)
1. a kind for the treatment of process of photosensitive quartz ampoule, which is characterized in that include the following steps:
S1. sabot:By quartz ampoule block pattern row pattern at least two layers of graphite charging tray, the quartz ampoule stacked on every layer of graphite charging tray
The number of plies is 8-12 layers;
S2. it heats up:Under room temperature, the graphite charging tray piled up is put into deshydroxy stove, is at the uniform velocity warming up to 600 DEG C, heating rate is
4-6 DEG C/min, keep the temperature 20-50min;Then 800 DEG C are warming up to by the heating rate of 3-5 DEG C/min, keep the temperature 20-50 minutes;Again
1050 DEG C are warming up to by the heating rate of 2-4 DEG C/min, keeps the temperature 210-250min;
S3. it cools down:650 DEG C are naturally cooling to, nitrogen is then passed to, is cooled to 300 DEG C;It is air-cooled to 60 DEG C hereinafter, coming out of the stove again;
S4. it is heat-treated:Fiery throwing processing is carried out to the surfaces externally and internally of quartz ampoule with the mixed gas of coal gas, methane gas and oxygen;
S5. it anneals:Quartz ampoule is put into annealing furnace, 1150 DEG C is warming up to by the speed of 300 DEG C/h, 30 minutes is kept the temperature, with stove
It is cooling, obtain product.
2. the treatment process of photosensitive quartz ampoule as described in claim 1, which is characterized in that include the following steps:
S1. sabot:By quartz ampoule block pattern row pattern at least two layers of graphite charging tray, the quartz ampoule stacked on every layer of graphite charging tray
The number of plies is 10 layers;
S2. it heats up:Under room temperature, the graphite charging tray piled up is put into deshydroxy stove, is at the uniform velocity warming up to 600 DEG C, heating rate 5
DEG C/min, keep the temperature 30min;Then 800 DEG C are warming up to by the heating rate of 4 DEG C/min, keep the temperature 30 minutes;Press 3 DEG C/min's again
Heating rate is warming up to 1050 DEG C, keeps the temperature 240min;
S3. it cools down:650 DEG C are naturally cooling to, nitrogen is then passed to, is cooled to 300 DEG C;Again open cycle wind turbine be cooled to 60 DEG C with
Under, it comes out of the stove;
S4. it is heat-treated:Fiery throwing processing is carried out to the surfaces externally and internally of quartz ampoule with the mixed gas of coal gas, methane gas and oxygen;
S5. it anneals:Quartz ampoule is put into annealing furnace, 1150 DEG C is warming up to by the speed of 300 DEG C/h, 30 minutes is kept the temperature, with stove
It is cooling, obtain product.
3. the treatment process of photosensitive quartz ampoule as claimed in claim 1 or 2, which is characterized in that after the step S3
Quartz ampoule is cut, back cover, crimping, special bent pipe and sealing process.
4. the treatment process of photosensitive quartz ampoule as claimed in claim 1 or 2, which is characterized in that coal gas, first in the step S4
The mixed gas of alkane gas and oxygen is using volume ratio:Coal gas:Methane:Oxygen=2:1:5.
5. the treatment process of photosensitive quartz ampoule as claimed in claim 1 or 2, which is characterized in that the photosensitive quartz ampoule uses
Raw material be SiO2Quartz, aluminium oxide and bismuth silicate of the content 99.98% or more.
6. the treatment process of photosensitive quartz ampoule as claimed in claim 1 or 2, which is characterized in that the photosensitive quartz ampoule is de-
When in hydroxyl stove, it is 9 × 10 to keep relative pressure in deshydroxy stove-5MPa。
7. the treatment process of photosensitive quartz ampoule as claimed in claim 1 or 2, which is characterized in that the photosensitive quartz ampoule is through de-
After hydroxyl and heat treatment, hydroxy radical content≤1ppm in tube body.
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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 |
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