CN100567188C - Crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics - Google Patents

Crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics Download PDF

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CN100567188C
CN100567188C CNB2006101220752A CN200610122075A CN100567188C CN 100567188 C CN100567188 C CN 100567188C CN B2006101220752 A CNB2006101220752 A CN B2006101220752A CN 200610122075 A CN200610122075 A CN 200610122075A CN 100567188 C CN100567188 C CN 100567188C
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crystallization
cooling
kiln
roller
combustion
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CN1919760A (en
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赵天佑
庄堆业
蔡来吉
庄伟兴
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GUANGDONG KEDI GLASS-CERAMIC INDUSTRIAL Co Ltd
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GUANGDONG KEDI GLASS-CERAMIC INDUSTRIAL Co Ltd
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    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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Abstract

The present invention relates to a kind of devitrified glass crystallization method, specifically is a kind of crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics and special-purpose crystallization roller kiln thereof.It is characterized in that and to cut into piece by the microcrystal glass plate that rolling process is produced, individual layer directly places devitrified glass crystallization roller kiln to carry out crystallization, its crystallization process condition comprises: preheating, intensification nucleus, thermostatic crystallization, rapid cooling, slow cooling, the crystallization cycle is 135-176 minute, and crystallization temperature is 870 ± 5 ℃.The present invention not only has advantages such as save energy, production efficiency height, product percent of pass height and comprehensive production cost are low, simultaneously, owing to exempt to be dustless operation with silicon carbide clamping plate and isolation oxidation magnesium powder, has both improved operator's Working environment, also helps environmental protection.

Description

Crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics
Technical field:
The present invention relates to a kind of devitrified glass crystallization method, specifically is a kind of crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics and special-purpose crystallization roller kiln thereof after improvement.
Background technology:
The existing lithium-aluminium-silicon system low-expansion glass-ceramics (being designated hereinafter simply as devitrified glass) as hot-plate such as electromagnetic oven, microwave oven, Yale cooker, gas furnace that is used for generally carries out crystallization at the crystallization roller kiln and handles.Traditional technology cuts into plate with devitrified glass usually, and is again that the devitrified glass plate is stacked together; For preventing its distortion, on the devitrified glass plate that stacks and below place respectively thickness than devitrified glass thick the carborundum plate of Duoing, usually silicon carbide is called clamping plate; For preventing to stick together between devitrified glass plate and the carborundum plate between devitrified glass plate and the devitrified glass plate, at interlayer sealing coat is set, sealing coat adopts magnesia powder usually; Because the devitrified glass plate that stacks is generally layer 2-4, adds bilevel carborundum plate, is total up to the 4-6 layer, places the crystallization roller kiln to carry out crystallization in the lump and handle.Because devitrified glass plate and the stacked crystallization roller kiln that are placed on of carborundum plate are carried out the crystallization processing, therefore the roller to roller kiln will require that enough physical strengths will be arranged, the diameter of the roller of existing roller kiln is all more than 50mm, because the diameter of roller is big, the wheelbase of roller and roller is also big, wheelbase is big more, requires more to adopt the silicon carbide clamping plate, could guarantee by the devitrified glass of crystallization indeformable.
In the crystallization roller kiln of above-described crystallization process and employing thereof, there is following shortcoming:
1, energy loss is big.Owing to adopt silicon carbide clamping plate and the microcrystal glass plate form of stacking to send in the crystallization roller kiln, except will making the required heat energy of devitrified glass crystallization, also will supply with the required heat energy of magnetization silicon clamping plate that volume and devitrified glass are more or less the same.
2, production efficiency is low.Because adopting silicon carbide clamping plate and the microcrystal glass plate form of stacking sends in the crystallization roller kiln, kiln body temperature degree is big with the core temperature deviation that is sandwiched in the devitrified glass in the layer, make devitrified glass reach crystallization temperature, requirement will have higher kiln body temperature degree and longer time.According to the patent specification introduction of the CN1161296C of approved mandate, sheet glass is stacked, under 900-1200 ℃ temperature, make glass crystallization, the crystallization cycle is 16-20 hour.
3, product breakage rate height.Because silicon carbide clamping plate and the microcrystal glass plate form of stacking are sent in the crystallization roller kiln, any moment of devitrified glass in roller kiln all is in strained condition, and the rotation of roller can make microcrystal glass plate be shaken and fragmentation; It is inhomogeneous to spread magnesia powder (sealing coat is set), also can make devitrified glass and devitrified glass, or sticks together between devitrified glass and the carborundum plate, and the devitrified glass of adhesion just becomes waste product; Operator's misoperation, devitrified glass and carborundum plate bump and fragmentation, also are one of reasons of product breakage.Product breakage rate 〉=10% of tradition crystallization process.
4, additional cost height.Because adopt silicon carbide as clamping plate, carborundum plate has certain access times, is subjected to the influence of all factors, carborundum plate is through a crystallization after the cycle, its breakage rate 〉=10%.The breakage of carborundum plate consumes the principal element that also constitutes production cost.
In a word, in the crystallization roller kiln of existing crystallization process and employing thereof, there are shortcomings such as complex process, comprehensive cost height, production cycle length.In addition, the district of coming out of the stove is the high-temperature zone, and the district of will coming out of the stove usually designs outdoor, operator's work under bad environment.
Summary of the invention:
The objective of the invention is to overcome the shortcoming of the crystallization roller kiln that have crystallization process and employing thereof now, a kind of crystallization method of the lithium-aluminium-silicon system low-expansion glass-ceramics after improvement and special-purpose crystallization roller kiln thereof of being exclusively used in are provided, make that its technology is simple, comprehensive cost is low, with short production cycle.
The present invention is that the microcrystal glass plate that will be produced by rolling process cuts into piece, and individual layer directly places devitrified glass crystallization roller kiln to carry out crystallization, and its crystallization process condition comprises:
A, preheating, in 18-23 minute, with microcrystal glass plate from room temperature heat temperature raising to 720 ℃;
B, intensification nucleus in 35-45 minute, are warming up to 870 ℃ with microcrystal glass plate from 720 ℃;
C, thermostatic crystallization are controlled at 870 ± 5 ℃ with microcrystal glass plate, keep 50-65 minute;
D, rapid cooling in 10-15 minute, are reduced to 370 ℃ with microcrystal glass plate from 870 ℃;
E, slow cooling, at 22-30 minute, or the time was long, and microcrystal glass plate is reduced to room temperature from 370 ℃, or than room temperature slightly height, kiln discharge then.
Devitrified glass crystallization roller kiln of the present invention, its structure will be described in an embodiment.
The present invention compares with traditional crystallization process, has following positively effect:
1, save energy.Owing to will cut caked microcrystal glass plate, individual layer directly places devitrified glass crystallization roller kiln to carry out crystallization, only provides crystallization required heat energy to devitrified glass, needn't provide heat energy for the silicon carbide clamping plate beyond the devitrified glass.The consumption combustion gas of unit surface devitrified glass can reduce by 50% than traditional technology.
2, production efficiency height.Owing to directly place devitrified glass crystallization roller kiln to carry out crystallization the microcrystal glass plate individual layer, the temperature of devitrified glass approaches kiln body temperature degree, and not only crystallization process is convenient to control, and can adopt rapid heating and quick cooling technology, to shorten the production cycle, enhance productivity.Whole crystallization process process just can be finished in the highest 870 ℃ temperature and 135-176 minute of only needing.
3, product percent of pass height.Owing to directly place devitrified glass crystallization roller kiln to carry out crystallization the microcrystal glass plate individual layer, the crystallization process devitrified glass is heated fast and does not break, and it is indeformable to cool, and reduces the possibility of devitrified glass thermal distortion widely, also reduce the breakage rate of product, product percent of pass is more than 98%.
4, comprehensive production cost is low.The present invention not only because of energy consumption reduces, efficient improves, the qualification rate raising reduces unit cost, also saves the expense of silicon carbide clamping plate simultaneously, saves the consumption expense of magnesia powder.
In a word, the present invention not only has advantages such as save energy, production efficiency height, product percent of pass height and comprehensive production cost are low, and improves workman's production environment, come out of the stove the temperature of product near room temperature, be the non high temperature operation, can improve operator's Working environment with the district's design of coming out of the stove indoor, simultaneously, owing to exempt to use magnesia powder, be dustless operation, also help environmental protection.
Description of drawings:
Fig. 1 is the crystallization process time temperature curve synoptic diagram of embodiment;
Fig. 2-Fig. 5 is the structure principle chart of the crystallization roller kiln of embodiment employing, wherein:
Fig. 2 is a preheating zone part-structure schematic diagram;
Fig. 3 is combustion gas heat tracing zone and chilling cooling area part-structure schematic diagram;
Fig. 4 and Fig. 5 take out waste heat wind district for the slow cooling district and come out of the stove district's part-structure schematic diagram.
Among the figure, 1, roller 2, microcrystal glass plate 3, kiln body 4, chimney 5, smoke evacuation motor 6, gas burner 7, combustion air variable valve 8, gas control valve 9, combustion gas solenoid valve 10, gas pipeline 11, combustion air pipeline 12, chilling wind variable valve 13, heat exchanger 14, chilling blower fan 15, combustion-supporting fan 16, take out waste heat fan 17, fan 18, viewing window 19, cooling air transfer lime 20, cooling air is carried arm 21, combustion air is carried arm 22, the hot chimney 23 of exhaust, waste heat is collected pipeline 24, heat extraction gas chimney A, inlet B, outlet C, combustion gas hot gas flow D, cooling air E, combustion air F, waste heat wind.
Embodiment:
Present embodiment provides a kind of crystallization method that is used for electromagnetic oven, microwave oven, Yale cooker, gas furnace etc. as the lithium-aluminium-silicon system low-expansion glass-ceramics after improvement of hot-plate.Present method is that the microcrystal glass plate that will be produced by rolling process cuts into piece, and individual layer directly places devitrified glass crystallization roller kiln to carry out crystallization, its process time-temperature curve as shown in Figure 1, its crystallization process condition comprises:
A, preheating, in 18-23 minute, with microcrystal glass plate from room temperature heat temperature raising to 720 ℃;
B, intensification nucleus in 35-45 minute, are warming up to 870 ℃ with microcrystal glass plate from 720 ℃;
C, thermostatic crystallization are controlled at 870 ± 5 ℃ with microcrystal glass plate, keep 50-65 minute;
D, rapid cooling in 10-15 minute, are reduced to 370 ℃ with microcrystal glass plate from 870 ℃;
E, slow cooling, at 22-30 minute, or the time was long, and microcrystal glass plate is reduced to room temperature from 370 ℃, or than room temperature slightly height, kiln discharge then.
With reference to Fig. 2-Fig. 5, the devitrified glass crystallization roller kiln that present embodiment adopted, its structure comprises tunnel oven body, transmission mechanism, heating unit, control device and refrigerating unit.The kiln body is divided into pre-heating temperature elevation district from the A end that enters the mouth to exporting the B end along the kiln length direction, and heat temperature raising nucleus district, heated constant temperature crystallization region, chilling cooling area, slow cooling cooling area are provided with the separation flashboard at least between heated constant temperature crystallization region and chilling cooling area; In each district, a temperature monitor is set at least.Transmission mechanism is made of the roller 1 and the driving mechanism thereof that are set up on the frame, and roller 1 is the alumina-ceramic roller, and its diameter is 27mm, and the roller spacing is 10mm.Heating unit comprises the be staggered gas burner 6 that is arranged at roller-way upper and lower part, kiln body both sides, the fuel gas supply device that is connected with gas burner and combustion air feedway, and the fuel gas supply device is the fuel gas transportation pipeline 10 that is provided with variable valve 8; Only gas burner 6 is set in intensification nucleus district and thermostatic crystallization district; Combustion gas smoke evacuation chimney 4 is arranged in the pre-heating temperature elevation district of kiln body inlet A; Control device comprises controlling box and connected temperature monitor and combustion gas solenoid valve 9, and the probe of temperature monitor is arranged at kiln body inside, and combustion gas solenoid valve 9 is arranged on the fuel gas transportation pipeline; Every 2-4 gas burner 6 is provided with a combustion gas solenoid valve 9, with simplified control system; The combustion air feedway comprises the combustion air conveying arm 21 that is provided with variable valve 7, and combustion air carries arm 21 to be connected with combustion air transport pipe 11; Combustion air E is provided by combustion-supporting fan 15, and combustion-supporting fan blast tube is connected with combustion air transport pipe 11 by heat exchanger 13, and heat exchanger 13 places quench zone.At the chilling cooling area chilling air-cooling device is set, the cold wind refrigerating unit is made of chilling blower fan 14 and cooling air transport pipe 19, the cooling air transport pipe sets up some cooling airs separately and carries arm 20, cooling air carries arm 20 to be communicated in the kiln body of quench zone, carry on the arm 20 at cooling air, chilling wind variable valve 12 is set.At the slow cooling cooling area exhaust thermic devices is set, the exhaust thermic devices by take out waste heat fan 16, waste heat collects pipeline 23 and the hot chimney 22 of exhaust constitutes, waste heat collects that pipeline 23 and kiln body are inner to link to each other.In the district of coming out of the stove, exhaust cigarette chimney 24 and fan 17 are set, with the temperature of further reduction devitrified glass, make temperature when coming out of the stove near room temperature.
Present embodiment, owing to adopt and to cut caked microcrystal glass plate, individual layer directly places devitrified glass crystallization roller kiln to carry out the method for crystallization, thereby little to the pressure of the roller of roller kiln, not really high to the requirement of physical strength, can reduce to diameter from the diameter 52mm of the roller of existing roller kiln is 27mm, the roller spacing can be reduced to 10mm, become roller-way and be transmitted as " chain " transmission, prevent the thermal distortion of microcrystal glass plate effectively, saving the silicon carbide clamping plate has become possibility.
Present embodiment is provided with the combustion air heat exchanger at quench zone, and its meaning is: 1, combustion air absorbs the heat energy of quench zone by after the heat exchanger, helps improving the cooling rate of quench zone; 2, combustion air absorbs after the heat energy, brings heat energy into combustion chamber, utilizes the energy, save energy; 3, combustion air absorbs after the heat energy, becomes hot blast, further improves combustion-supporting effect.
Present embodiment, owing to gas burner 6 is set in intensification nucleus district and thermostatic crystallization district, and combustion gas smoke evacuation chimney 4 is arranged at the front end in the pre-heating temperature elevation district of kiln body inlet A, nucleus district and crystallization region incendiary hot gas flow through the preheating zone time also to preheating zone body of heater and devitrified glass heating, the preheating zone body of heater needn't be installed gas burner, also can arrive the temperature condition of processing requirement, therefore, present embodiment only is provided with gas burner 6 in intensification nucleus district and thermostatic crystallization district, also utilize the energy, save energy in a sense.

Claims (4)

1, a kind of crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics after improvement, it is characterized by: will cut into piece by the microcrystal glass plate that rolling process is produced, individual layer directly places devitrified glass crystallization roller kiln to carry out crystallization, and its crystallization process condition comprises:
A, preheating, in 18-23 minute, with microcrystal glass plate from room temperature heat temperature raising to 720 ℃;
B, intensification nucleus in 35-45 minute, are warming up to 870 ℃ with microcrystal glass plate from 720 ℃;
C, thermostatic crystallization are controlled at 870 ± 5 ℃ with microcrystal glass plate, keep 50-65 minute;
D, rapid cooling in 10-15 minute, are reduced to 370 ℃ with microcrystal glass plate from 870 ℃;
E, slow cooling at 22-30 minute, are reduced to room temperature, kiln discharge then with microcrystal glass plate from 370 ℃;
Described devitrified glass crystallization roller kiln comprise tunnel oven body (3), transmission mechanism, heating unit, control device and refrigerating unit, and transmission mechanism is made of the roller (1) and the driving mechanism thereof that are set up on the frame; Heating unit comprises the be staggered gas burner (6) that is arranged at roller-way upper and lower, kiln body both sides, the fuel gas supply device that is connected with gas burner and combustion air feedway, and the fuel gas supply device is for being provided with the fuel gas transportation pipeline (10) of variable valve (8); The combustion air feedway comprises the combustion air conveying arm (21) that is provided with variable valve (7), and combustion air carries arm (21) to be connected with combustion air transport pipe (11); Control device comprises controlling box and connected temperature monitor and combustion gas solenoid valve (9), and the probe of temperature monitor is arranged at kiln body inside, and combustion gas solenoid valve (9) is arranged on the fuel gas transportation pipeline; The kiln body is divided into pre-heating temperature elevation district from inlet (A) end to outlet (B) end along the kiln length direction, and heat temperature raising nucleus district, heated constant temperature crystallization region, chilling cooling area, slow cooling cooling area are provided with the separation flashboard at least between heated constant temperature crystallization region and chilling cooling area; In each district, a temperature monitor is set at least; Smoke evacuation chimney (4) is arranged at the front end in the pre-heating temperature elevation district of kiln body inlet (A); Every 2-4 gas burner (6) is provided with a combustion gas solenoid valve (9); Only gas burner (6) is set in intensification nucleus district and thermostatic crystallization district; Described roller (1) is the alumina-ceramic roller, and its diameter is 25-30mm, and the roller spacing is 10-15mm.
2, crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics according to claim 1, it is characterized by: the combustion air (E) of described devitrified glass crystallization roller kiln is provided by combustion-supporting fan (15), combustion-supporting fan blast tube is connected with combustion air transport pipe (11) by heat exchanger (13), and heat exchanger (13) places quench zone.
3, crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics according to claim 1, it is characterized by: the chilling cooling area at described devitrified glass crystallization roller kiln is provided with the chilling air-cooling device, the cold wind refrigerating unit is made of chilling blower fan (14) and cooling air transport pipe (19), the cooling air transport pipe sets up some cooling airs separately and carries arm (20), cooling air carries arm (20) to be communicated in the kiln body of quench zone, carry on the arm (20) at cooling air, chilling wind variable valve (12) is set.
4, crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics according to claim 1, it is characterized by: at the slow cooling cooling area of described devitrified glass crystallization roller kiln, the exhaust thermic devices is set, waste heat fan (16), waste heat are collected pipeline (23) to the exhaust thermic devices and the hot chimney of exhaust (22) constitutes by taking out, and waste heat is collected pipeline (23) and linked to each other with the kiln body is inner.
CNB2006101220752A 2006-09-09 2006-09-09 Crystallization method of lithium-aluminium-silicon system low-expansion glass-ceramics Active CN100567188C (en)

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DE102009015089B4 (en) * 2009-03-31 2012-05-24 Schott Ag Method and device for ceramizing glasses, glass ceramic articles and its use
CN103086602B (en) * 2013-03-04 2014-11-26 内蒙古科技大学 Method for manufacturing low-swelling microcrystalline glass through microwave heat treatment of gold tailings
CN106977084A (en) * 2017-05-20 2017-07-25 广东科迪微晶玻璃实业有限公司 Devitrified glass hot bending crystallization continuous tunnel furnace and its method for producing crystallized glass article

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4851022A (en) * 1987-05-06 1989-07-25 Schott Glaswerke Method and oven for ceramising glass plates

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4851022A (en) * 1987-05-06 1989-07-25 Schott Glaswerke Method and oven for ceramising glass plates

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