CN103030290B - Devitrified glass that a kind of fold resistance is strong and preparation method thereof - Google Patents

Devitrified glass that a kind of fold resistance is strong and preparation method thereof Download PDF

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CN103030290B
CN103030290B CN201210515378.6A CN201210515378A CN103030290B CN 103030290 B CN103030290 B CN 103030290B CN 201210515378 A CN201210515378 A CN 201210515378A CN 103030290 B CN103030290 B CN 103030290B
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glass
oxide
weight portion
temperature
devitrified glass
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CN103030290A (en
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毛庆云
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Zhongshan New Feeling Glass Co ltd
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Abstract

The invention discloses the devitrified glass that a kind of fold resistance is strong, it is made up of the raw material of following weight parts: gangue 25-30, quartz sand 20-30, flyash 15-20, silica 1 0-15, calcium carbonate 10-15, alabaster 10-15, zinc oxide 6-8, aluminium oxide 5-7, barium monoxide 5-7, potassium oxide 3-4, salt 3-4, magnesium fluoride 2-4, calcirm-fluoride 2-3, charcoal 2.5-3, clay 3-4, boron oxide 2-3, lithia 2-3, trees ash 2.5-3, plant ash 2-3, sodium oxide molybdena 2-3, potassic feldspar 0.25-0.4, sodium tetraborate 0.15-0.3, vanadic anhydride 0.15-0.3, zirconium dioxide 0.15-0.2. the present invention produce devitrified glass flatness good, mechanical strength is high, hardness is large, have good heat resistance, flexural strength, corrosion resistance and wearability, product can be made into all kinds of tubing, sheet material, can be widely used in architectural abrasion-proof corrosion-proof corrosion material, building and ornament materials.

Description

Devitrified glass that a kind of fold resistance is strong and preparation method thereof
Technical field
The present invention relates generally to a kind of devitrified glass and preparation method thereof, relates in particular to devitrified glass that a kind of fold resistance is strong and preparation method thereof.
Background technology
Devitrified glass, claim again glass ceramics, it is a kind of new material that comprehensive glass and ceramic technology grow up, it is the equally distributed material of microcrystal and glassy phase, its physicochemical property has been concentrated glass, triple advantages of pottery and lithotome, as high in mechanical strength, corrosion-resistant, heat-resisting, wear-resisting, antioxygenic property is good, electrical property is good, the coefficient of expansion is adjustable, Heat stability is good etc., and be better than lithotome and pottery, can be used for building curtain wall and indoor high-grade decoration, also can do structural material mechanically, electronics, insulating materials on electrician, the baseboard material of large scale integrated circuit, the heat-resisting serial vessel of micro-wave oven, chemical industry and anti-corrosion material and mine high-abrasive material etc., it is the new material with the 21 century of development prospect. thereby be widely used in the fields such as electronics, chemical industry, military affairs, space flight, nuclear industry and building. because devitrified glass can use ore, industrial tailings, metallurgical slag, flyash, gangue etc. as main production raw material, and produced in process pollution-free, the no radioactivity pollute of product own, environment-friendly products or green material therefore be otherwise known as, often there are a large amount of manufacturability pores in the top layer of the devitrified glass of traditional mode of production and internal layer thereof, and the performance such as rupture strength and resistance to water is not strong, limit the application of devitrified glass.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, and devitrified glass of the fine and close pore-free of a kind of any surface finish, water-fast, High anti bending strength and preparation method thereof is provided.
The present invention is achieved by the following technical solutions:
The devitrified glass that fold resistance is strong, it is made up of the raw material of following weight parts:
Gangue 25-30, quartz sand 20-30, flyash 15-20, silica 1 0-15, calcium carbonate 10-15, alabaster 10-15, zinc oxide 6-8, aluminium oxide 5-7, barium monoxide 5-7, potassium oxide 3-4, salt 3-4, magnesium fluoride 2-4, calcirm-fluoride 2-3, charcoal 2.5-3, clay 3-4, boron oxide 2-3, lithia 2-3, trees ash 2.5-3, plant ash 2-3, sodium oxide molybdena 2-3, potassic feldspar 0.25-0.4, sodium tetraborate 0.15-0.3, vanadic anhydride 0.15-0.3, zirconium dioxide 0.15-0.2.
A preparation method for the devitrified glass that fold resistance is strong, comprises the following steps:
(1) raw material of above-mentioned weight portion is mixed to join in glass-melting furnace, under the high temperature of 1520-1620 DEG C, is melt into uniform vitreum;
(2) above-mentioned vitreum is directly dropped in water, cold quenching becomes glass particle, is then ground into 20-25 μ m powder, add the modified glass body powder of its weight 1-3%, mix oven dry, and be laid on the horizontal plane with the refractory material of trees ashes separation layer, laid thickness is 20-24mm;
The preparation method of described modified glass body powder is: the plant ash that is 10-12 by weight portion, weight portion are the calcium oxide of 3-5 part, the quartz sand that weight portion is 52-56, the attapulgite that weight portion is 18-20, the Cab-O-sil that weight portion is 30-32, mix and add in glass-melting furnace, be heated under the high temperature of 1560-1650 DEG C, melting 2-3 hour, be down to again at 1400-1450 DEG C and clarify 1.5-2 hour, make glass metal, then quench in cold water and obtain cullet body, then grind to form 3-5 μ m modified glass body powder;
(3) above-mentioned laid good glass particle is placed in to resistance furnace together with refractory material, temperature schedule: normal temperature is heated to 340-360 DEG C, 6 DEG C/min of heating rate; 340-360 DEG C is heated to 750-850 DEG C, 7 DEG C/min of heating rate; At 750-900 DEG C, be incubated 1.8-2h; Then be heated to 1350 DEG C, 8 DEG C/min of heating rate from 900 DEG C; At 1350 DEG C, be incubated 2.5-3h, complete coring and crystallization process;
(4) annealing: the glass after above-mentioned crystallization is carried out to annealing in process with the annealing cooling rate of 4-5 DEG C/min, in the time that temperature is down in 580-620 DEG C, keep constant temperature 30-40 minute, and then 5-6 DEG C/min speed is warmed up to 850-900 DEG C, and then continue cooling with 6-7 DEG C/min speed, in the time that temperature is down in 280-320 DEG C, then naturally cool to room temperature;
(5) size as requested cuts into plate, grinding and polishing, deburring.
Advantage of the present invention is:
The present invention produce devitrified glass flatness good, mechanical strength is high, hardness is large, have good heat resistance, flexural strength, corrosion resistance and wearability, product can be made into all kinds of tubing, sheet material, can be widely used in architectural abrasion-proof corrosion-proof corrosion material, building and ornament materials, use for laboratory heating appliances, high-temperature heat exchanger, for quartz glass, window pyrometer, radome etc.
Detailed description of the invention
Embodiment 1
The devitrified glass that fold resistance is strong, it by following weight parts (kilogram) raw material form:
Gangue 30, quartz sand 30, flyash 20, silica 15, calcium carbonate 15, alabaster 15, zinc oxide 8, aluminium oxide 7, barium monoxide 7, potassium oxide 3, salt 4, magnesium fluoride 4, calcirm-fluoride 3, charcoal 2.5, clay 4, boron oxide 3, lithia 3, trees ash 2.5, plant ash 3, sodium oxide molybdena 3, potassic feldspar 0.4, sodium tetraborate 0.3, vanadic anhydride 0.15, zirconium dioxide 0.2.
A preparation method for the devitrified glass that fold resistance is strong, comprises the following steps:
(1) raw material of above-mentioned weight portion is mixed to join in glass-melting furnace, under the high temperature of 1620 DEG C, is melt into uniform vitreum;
(2) above-mentioned vitreum is directly dropped in water, cold quenching becomes glass particle, is then ground into 25 μ m powder, add the modified glass body powder of its weight 3%, mix oven dry, and be laid on the horizontal plane with the refractory material of trees ashes separation layer, laid thickness is 24mm;
The preparation method of described modified glass body powder is: the plant ash that is 12 by weight portion, weight portion are the calcium oxide of 5 parts, the quartz sand that weight portion is 56, the attapulgite that weight portion is 20, the Cab-O-sil that weight portion is 32, mix and add in glass-melting furnace, be heated under the high temperature of 1650 DEG C, melting 3 hours, be down to again at 1450 DEG C and clarify 1.5 hours, make glass metal, in the cold water of then quenching, obtain cullet body, then grind to form 3-5 μ m modified glass body powder;
(3) above-mentioned laid good glass particle is placed in to resistance furnace together with refractory material, temperature schedule: normal temperature is heated to 360 DEG C, 6 DEG C/min of heating rate; 360 DEG C are heated to 850 DEG C, 7 DEG C/min of heating rate; At 900 DEG C, be incubated 2h; Then be heated to 1350 DEG C, 8 DEG C/min of heating rate from 900 DEG C; At 1350 DEG C, be incubated 2.5h, complete coring and crystallization process;
(4) annealing: the glass after above-mentioned crystallization is carried out to annealing in process with the annealing cooling rate of 5 DEG C/min, in the time that temperature is down in 620 DEG C, keep constant temperature 40 minutes, and then 6 DEG C/min speed is warmed up to 900 DEG C, and then continue cooling with 7 DEG C/min speed, in the time that temperature is down in 320 DEG C, then naturally cool to room temperature;
(5) size as requested cuts into plate, grinding and polishing, deburring.
Performance test:
Rupture strength test: adopt MC009-wds10M type electronic universal material property testing machine to utilize the rupture strength of three-point bending method working sample, getting 6 strip samples (9mm × 7mm × 85mm) tests, calculate rupture strength, finally average.
Microsclerometry: by the hardness of HXD-1000 digital micro-analysis hardness-testing device working sample, each sample is surveyed three points, represents its microhardness with mean value, surveys altogether three samples, finally calculates the mean value of the microhardness of three samples.
Water resistance test: adopt powder to soak weight-loss method and measure (DTN12116), sample is pulverized, get 40 now, 2 grams of microcrystalline glass powders on 60 orders, in 50ml volumetric flask, add water to scale, at 98 ± 0.5 DEG C of temperature, be incubated 60 minutes, measure its 100cm2Weight-loss ratio (mg/100cm2)。
Test result:
1, sample appearance quality: surface compact, the defects such as pore-free, surface of polished light.
2, mechanical performance: average rupture strength 89.7MPa, average microhardness 893.3kgf/mm2
3, hydrolysis grade: 1 grade, weight-loss ratio is: 0.282mg/100cm2

Claims (2)

1. the devitrified glass that fold resistance is strong, it is characterized in that it is made up of the raw material of following weight parts: gangue 25-30, quartz sand 20-30, flyash 15-20, silica 1 0-15, calcium carbonate 10-15, alabaster 10-15, zinc oxide 6-8, aluminium oxide 5-7, barium monoxide 5-7, potassium oxide 3-4, salt 3-4, magnesium fluoride 2-4, calcirm-fluoride 2-3, charcoal 2.5-3, clay 3-4, boron oxide 2-3, lithia 2-3, trees ash 2.5-3, plant ash 2-3, sodium oxide molybdena 2-3, potassic feldspar 0.25-0.4, sodium tetraborate 0.15-0.3, vanadic anhydride 0.15-0.3, zirconium dioxide 0.15-0.2.
2. a preparation method for the devitrified glass that fold resistance as claimed in claim 1 is strong, is characterized in that comprising the following steps:
(1) raw material of above-mentioned weight portion is mixed to join in glass-melting furnace, under the high temperature of 1520-1620 DEG C, is melt into uniform vitreum;
(2) above-mentioned vitreum is directly dropped in water, cold quenching becomes glass particle, is then ground into 20-25 μ m powder, add the modified glass body powder of its weight 1-3%, mix oven dry, and be laid on the horizontal plane with the refractory material of trees ashes separation layer, laid thickness is 20-24mm; The preparation method of described modified glass body powder is: the plant ash that is 10-12 by weight portion, weight portion are the calcium oxide of 3-5 part, the quartz sand that weight portion is 52-56, the attapulgite that weight portion is 18-20, the Cab-O-sil that weight portion is 30-32, mix and add in glass-melting furnace, be heated under the high temperature of 1560-1650 DEG C, melting 2-3 hour, be down to again at 1400-1450 DEG C and clarify 1.5-2 hour, make glass metal, then quench in cold water and obtain cullet body, then grind to form 3-5 μ m modified glass body powder;
(3) above-mentioned laid good glass particle is placed in to resistance furnace together with refractory material, temperature schedule: normal temperature is heated to 340-360 DEG C, 6 DEG C/min of heating rate; 340-360 DEG C is heated to 750-850 DEG C, 7 DEG C/min of heating rate; At 750-900 DEG C, be incubated 1.8-2h; Then be heated to 1350 DEG C, 8 DEG C/min of heating rate from 900 DEG C; At 1350 DEG C, be incubated 2.5-3h, complete coring and crystallization process;
(4) annealing: the glass after above-mentioned crystallization is carried out to annealing in process with the annealing cooling rate of 4-5 DEG C/min, in the time that temperature is down in 580-620 DEG C, keep constant temperature 30-40 minute, and then 5-6 DEG C/min speed is warmed up to 850-900 DEG C, and then continue cooling with 6-7 DEG C/min speed, in the time that temperature is down in 280-320 DEG C, then naturally cool to room temperature;
(5) size as requested cuts into plate, grinding and polishing, deburring.
CN201210515378.6A 2012-12-05 2012-12-05 Devitrified glass that a kind of fold resistance is strong and preparation method thereof Active CN103030290B (en)

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CN106277801A (en) * 2016-08-31 2017-01-04 望江宇花玻璃有限公司 A kind of homoiothermic devitrified glass containing modified coal ash and preparation technology thereof
CN106380079A (en) * 2016-08-31 2017-02-08 望江宇花玻璃有限公司 High-strength microcrystalline glass containing modified coal ash and preparation technology of high-strength microcrystalline glass

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101306920A (en) * 2008-06-30 2008-11-19 浙江振申绝热科技有限公司 Production raw material of foamed glass and process for producing foamed glass
CN101767933A (en) * 2009-12-30 2010-07-07 陕西乾盛环保建材工程有限公司 Method utilizing coal gangue to manufacture microcrystalline glass plate material
CN102795772A (en) * 2012-07-23 2012-11-28 北京大有盛和科技有限公司 Method for preparing microcrystalline glass from kaolin-type coal gangue or fly ash and carbide slag

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004107183A (en) * 2002-09-20 2004-04-08 Rikogaku Shinkokai Crystallized material and method of manufacturing it

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101306920A (en) * 2008-06-30 2008-11-19 浙江振申绝热科技有限公司 Production raw material of foamed glass and process for producing foamed glass
CN101767933A (en) * 2009-12-30 2010-07-07 陕西乾盛环保建材工程有限公司 Method utilizing coal gangue to manufacture microcrystalline glass plate material
CN102795772A (en) * 2012-07-23 2012-11-28 北京大有盛和科技有限公司 Method for preparing microcrystalline glass from kaolin-type coal gangue or fly ash and carbide slag

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Address after: 541002 No. two, No. 5, West Road, Xiangshan District, Guilin, the Guangxi Zhuang Autonomous Region

Patentee after: Qiu Mingjin

Address before: 230000 Changan industrial agglomeration area, Shunchang Town, Feixi, Anhui, China,

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Address after: 528447 B building 47, Sha Gang Middle Road, port town, Zhongshan, Guangdong

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Denomination of invention: A microcrystalline glass with strong bending resistance and its preparation method

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