CN101591144A - Slim CaO-Al 2O 3-SiO 2System glass ceramics and preparation - Google Patents

Slim CaO-Al 2O 3-SiO 2System glass ceramics and preparation Download PDF

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Publication number
CN101591144A
CN101591144A CNA2009100628560A CN200910062856A CN101591144A CN 101591144 A CN101591144 A CN 101591144A CN A2009100628560 A CNA2009100628560 A CN A2009100628560A CN 200910062856 A CN200910062856 A CN 200910062856A CN 101591144 A CN101591144 A CN 101591144A
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glass
cao
sio
preparation
devitrified glass
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CN101591144B (en
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谢俊
程金树
何峰
陆平
郑伟宏
全健
肖子凡
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

A kind of CaO-Al 2O 3-SiO 2System glass ceramics, its chemical ingredients comprises (weight %): SiO 260.0~70.0, Al 2O 35.0~10.0, CaO 16.5~18.0, ZnO 0~2.5, and BaO 4.0~6.0, Na 2O 5.0~6.0, K 2O 0.5~2.0, B 2O 31.0~3.0, Sb 2O 30.5~1.0, MgO 1.0~3.0.Its preparation method is: batching is stirred evenly be placed in the ceramic crucible, and put into silicon molybdenum stove heating and insulation, shrend is carried out drying after becoming the glass particle of 0.5~6mm, again it is laid in the refractory-material dies, and insert and heat in the High Temperature Furnaces Heating Apparatus and insulation, the glass particle crystallization is shakeout, and annealing is cooled to room temperature then.Cost of the present invention is low, and is functional, slim, uses wide.

Description

Slim CaO-Al 2O 3-SiO 2System glass ceramics and preparation
Technical field
The present invention relates to glass, particularly relate to a kind of low cost for building and slim CaO-Al 2O 3-SiO 2System glass ceramics and preparation method thereof.
Background technology
In recent years, because crystallizing glass decoration board is beautiful in colour, aberration is little and will never fade; Compact structure, clean mark; Hard wear resistant, weather resistance, advantages such as protection against corrosion are familiar with and are approved by people day by day.Devitrified glass has had multiple utilization in building trade, has been used for high-grade house places such as high-grade utilities building such as airport, station, office block, subway, hotel, hotel and villa.Crystallizing glass sheet material is high-grade high consumption product, and the existing market valency is higher.Expensive high price has become the key obstacle that opens up a market.In production cost was formed, fuel cost accounted for four/the last one, secondly is expense of raw materials, and the binomial total accounts for about half of cost, and how to reduce production costs is one of major subjects in recent years.
For economizing on resources, the protection environment reduces cost in recent years, and Chinese scholars adopts solid waste to reach the purpose that reduces cost as the devitrified glass raw material, as flyash, coal gangue, blast furnace slag, various mining mine tailings or the like.This respect has many patent reports: number of patent application is 200510003205.6 to disclose the method for producing microcrystalline glass plaque with phosphorus slag; Number of patent application is 200410058045.0 to disclose devitrified glass and the method that high iron tailings is made; The patent No. is that 85100521A discloses microcrystal glass from fine coal ash and waste residue; But the devitrified glass product that solid waste is produced usually can be paid the cost of performance, and promptly the solid waste consumption is big more, and the performance loss of product is just big more.Meanwhile, the major equipment of production sintering process crystallizing glass decoration board is tunnel like and shuttle-type sintering crystallization kiln at present, and the thickness of the crystallizing glass decoration board of being produced is (thick template) in the scope of 18~30mm.Cause thus its weight per unit area big, yield poorly, the raw material consumption of product is big, energy consumption is high.
Therefore, be necessary to develop the novel low-cost glass ingredient, increase crystallizing glass sheet material assortment, improve the quality of products and labour productivity, will become the main from now on developing direction of crystallizing glass sheet material.
Summary of the invention
Technical problem to be solved by this invention is: a kind of low cost, slim and well behaved CaO-Al are provided 2O 3-SiO 2System glass ceramics, and, adjust the chemical constitution of described devitrified glass from making the used raw material of devitrified glass, reduce the preparation method that the high zinc oxide content of raw materials cost obtains this glass.
The present invention solves its technical problem and adopts following technical scheme:
The present invention is to provide the slim CaO-Al of a kind of low cost 2O 3-SiO 2System glass ceramics (abbreviation devitrified glass), by weight, the chemical ingredients of this devitrified glass comprises: SiO 260.0~70.0%, Al 2O 35.0~10.0%, CaO 16.5~18.0%, ZnO 0~2.5%, and BaO 4.0~6.0%, Na 2O 5.0~6.0%, K 2O 0.5~2.0%, B 2O 31.0~3.0%, Sb 2O 30.5~1.0%, MgO 1.0~3.0%.
The present invention is from reducing ZnO content and introducing MgO and K 2O content is set about, prepare above-mentioned devitrified glass, its preparation process comprises: press devitrified glass chemical ingredients batching, this batching is placed in the ceramic crucible through fully mixing, put into silicon molybdenum stove again and be raised to 1450 ℃~1480 ℃ with 1~3 ℃/minute, behind soaking time 〉=45min, shrend becomes the glass particle of 0.5~6mm, dry for standby; The exsiccant frit is laid in the refractory-material dies, upper strata glass particle granularity is 2~3mm, layer thickness is 10~20mm, insert the high temperature experimental furnace and be raised to 1050~1100 ℃ from room temperature with 3~5 ℃/minute temperature rise rate, soaking time 〉=1.5 hour, the glass particle crystallization is shakeout, be cooled to room temperature, obtain described devitrified glass through annealing.
When batching, raw materials used is silica sand, albite, rhombspar, calcite, zinc oxide, barium carbonate, soda ash, borax, weisspiessglanz and salt of wormwood.
The thickness of the prepared devitrified glass of the present invention is 8~30mm.Enriched the description of microcrystal glass plate section product, made the thickness range of sheet material expand to 8~30mm by 18 original~30mm, the adaptability of product is enhanced.
Devitrified glass provided by the invention and preparation method thereof compared with prior art has following major advantage:
One. cost reduces: from reducing ZnO content and introducing MgO and K 2O sets about, and manufacturing cost is reduced.
They are two years old. and functional: devitrified glass is not easy to crack in process of production, and void content reduces, thereby has guaranteed the quality of devitrified glass, and its intensity, whiteness and glossiness comply with the national standard requirements.
They are three years old. have slim characteristics: the thin type nucleated glass dalle that can prepare 8~15mm.
They are four years old. and enriched the description of microcrystal glass plate section product, made the thickness range of sheet material expand to 8~30mm by 18 original~30mm.To promoting the related industries technical progress, promoting the support that provides the necessary technical of industry core competitiveness.
They are five years old. and development prospect is wide: because quality product improves, cost reduces, and helps utilizing the lever of high-grade low price to pry open the gate, market like this, is done sth. on a larger scale in devitrified glass market.If these high-grade green decoration materials are entered common people house, the development prospect of crystallizing glass sheet material will be more wide.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of devitrified glass of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment, but do not limit the present invention.
The preparation of embodiment 1. devitrified glasses:
Batching (mass percent): press quartz sand 52.4%, aluminum oxide 4.9%, lime carbonate 24.7%, zinc oxide 1.7%, barium carbonate 4.2%, yellow soda ash 7.7%, salt of wormwood 1.8%, borax 2.3%, antimonous oxide 0.4% batching.This prescription is characterised in that uses K 2O partly substitutes ZnO, K 2O not only plays the effect that reduces glass viscosity, and glass surface tension is along with K simultaneously 2O substitutes the increase of ZnO content and reduces, and helps the discharge of bubble in the sintering process and shakeouing of surface.
The preparation of devitrified glass: load weighted raw material is mixed, be prepared into glass batch.This admixtion melts and clarifies at 1450 ± 10 ℃, and the glass metal shrend that fusing is good becomes the glass particle of 0.5~6mm, dries classification then.Exsiccant glass particle material is tiled on the refractory-material dies, and the upper strata grain graininess is 2~3mm, and layer thickness is 20mm.After stone and the strickling, be placed on the high temperature experimental furnace and carry out the crystallization processing, temperature increasing schedule is: room temperature~750 ℃, 5 ℃/min of temperature rise rate, 750~910 ℃, 3 ℃/min of temperature rise rate, 910~1100 ℃, 4 ℃/min of temperature rise rate 1050~1100 ℃ of soaking time 〉=1.5 hour, shakeouts the glass particle surface.The glass pellet of handling through crystallization sinters an integral body into, and separates out a large amount of wollastonite crystal.Be annealed to room temperature at last, make the devitrified glass sample.
The composition of the devitrified glass that is obtained (mass percent) is: SiO 262.6%, Al 2O 35.9%, CaO 16.7%, ZnO2%, BaO 3.9%, Na 2O 5.9%, K 2O 1.5%, B 2O 31%, Sb 2O 30.5%.
The preparation of embodiment 2. devitrified glasses:
Batching (mass percent): press quartz sand 51.6%, aluminum oxide 4.2%, lime carbonate 25.2%, zinc oxide 1.7%, barium carbonate 4.3%, yellow soda ash 7.9%, magnesium oxide 2.5%, borax 2.3%, antimonous oxide 0.4% batching.This prescription is characterised in that with MgO and partly substitutes ZnO, introduces MgO and can promote separating out of wollastonite crystalline phase in the glass, compactness that can reinforcing glass and improve physical strength.
The preparation of devitrified glass: load weighted raw material is mixed, be prepared into glass batch.This admixtion melts and clarifies at 1450 ± 10 ℃, and the glass metal shrend that fusing is good becomes the glass particle of 0.5~6mm, dries classification then.Exsiccant glass particle material is tiled on the refractory-material dies, and the upper strata grain graininess is 2~3mm, and layer thickness is 20mm.After stone and the strickling, be placed on the high temperature experimental furnace and carry out the crystallization processing, temperature increasing schedule is: room temperature~750 ℃, 5 ℃/min of temperature rise rate, 750~910 ℃, 3 ℃/min of temperature rise rate, 910~1100 ℃, 4 ℃/min of temperature rise rate 1050~1100 ℃ of soaking time 〉=1.5 hour, shakeouts the glass particle surface.The glass pellet of handling through crystallization sinters an integral body into, and separates out a large amount of wollastonite crystal.Be annealed to room temperature at last, make the devitrified glass sample.
The composition (mass percent) of the devitrified glass that obtains is: SiO 261.5%, Al 2O 35%, CaO 17%, ZnO 2%, BaO 4%, Na 2O 6%, MgO 3%, B 2O 31%, Sb 2O 30.5%.
The preparation of embodiment 3. devitrified glasses:
Batching (mass percent): press quartz sand 51.3%, aluminum oxide 4.1%, lime carbonate 25.1%, zinc oxide 0.4%, barium carbonate 4.3%, yellow soda ash 7.8%, salt of wormwood 1.8%, magnesium oxide 2.5%, borax 2.3%, antimonous oxide 0.4% batching.This prescription is characterised in that with Mg0 and K 2O mixes introducing and substitutes ZnO, and the content of ZnO is further reduced, and cost economizes in raw materials.
The preparation of devitrified glass: load weighted raw material is mixed, be prepared into glass batch.This admixtion melts and clarifies at 1450 ± 10 ℃, and the glass metal shrend that fusing is good becomes the glass particle of 0.5~6mm, dries classification then.Exsiccant glass particle material is tiled on the refractory-material dies, and the upper strata grain graininess is 2~3mm, and layer thickness is 20mm.After stone and the strickling, be placed on the high temperature experimental furnace and carry out the crystallization processing, temperature increasing schedule is: room temperature~750 ℃, 5 ℃/min of temperature rise rate, 750~910 ℃, 3 ℃/min of temperature rise rate, 910~1100 ℃, 4 ℃/min of temperature rise rate 1050~1100 ℃ of soaking time 〉=1.5 hour, shakeouts the glass particle surface.The glass pellet of handling through crystallization sinters an integral body into, and separates out a large amount of wollastonite crystal.Be annealed to room temperature at last, make the devitrified glass sample.
The composition (mass percent) of the devitrified glass that obtains is: SiO 261.5%, Al 2O 35%, CaO 17%, ZnO 0.5%, BaO 4%, Na 2O 6%, MgO 3%, K 2O 1.5%, B 2O 31%, Sb 2O 30.5%.
The preparation of embodiment 4. devitrified glasses:
Batching (mass percent): press quartz sand 51.2%, aluminum oxide 5.8%, lime carbonate 25.2%, zinc oxide 0%, barium carbonate 4.3%, yellow soda ash 6.5%, salt of wormwood 1.8%, magnesium oxide 2.5%, borax 2.3%, antimonous oxide 0.4% batching.This prescription is characterised in that with not using ZnO as raw material fully, and suitably increases Al 2O 3Content connects degree with the network that improves glassy phase, finally improves the overall mechanical properties of finished product.
The preparation of devitrified glass: load weighted raw material is mixed, be prepared into glass batch.This admixtion melts and clarifies at 1450 ± 10 ℃, and the glass metal shrend that fusing is good becomes the glass particle of 0.5~6mm, dries classification then.Exsiccant glass particle material is tiled on the refractory-material dies, and the upper strata grain graininess is 2~3mm, and layer thickness is 20mm.After stone and the strickling, be placed on the high temperature experimental furnace and carry out the crystallization processing, temperature increasing schedule is: room temperature~750 ℃, 5 ℃/min of temperature rise rate, 750~910 ℃, 3 ℃/min of temperature rise rate, 910~1100 ℃, 4 ℃/min of temperature rise rate 1050~1100 ℃ of soaking time 〉=1.5 hour, shakeouts the glass particle surface.The glass pellet of handling through crystallization sinters an integral body into, and separates out a large amount of wollastonite crystal.Be annealed to room temperature at last, make the devitrified glass sample.Made devitrified glass sample is through X-ray diffraction analysis as can be known: its principal crystalline phase is β-wollastonite, and characteristic peak is sharp-pointed, and crystal structure is all right, and the XRD figure spectrum is seen Fig. 1.
The composition (mass percent) of the devitrified glass that obtains is: SiO 261%, Al 2O 37%, CaO 17%, BaO 4%, Na 2O 5%, MgO 3%, K 2O 1.5%, B 2O 31%, Sb 2O 30.5%.

Claims (4)

1. a devitrified glass is characterized in that the slim CaO-Al of sintering process 2O 3-SiO 2System glass ceramics, by weight, the chemical ingredients of this devitrified glass comprises: SiO 260.0~70.0%, Al 2O 35.0~10.0%, CaO 16.5~18.0%, ZnO 0~2.5%, and BaO 4.0~6.0%, Na 2O 5.0~6.0%, K 2O 0.5~2.0%, B 2O 31.0~3.0%, Sb 2O 30.5~1.0%, MgO 1.0~3.0%.
2. the preparation method of a devitrified glass is characterized in that from reducing ZnO content and introducing MgO and K 2O content is set about, and prepares slim CaO-Al 2O 3-SiO 2System glass ceramics, its step comprises: press devitrified glass chemical ingredients batching, this batching is placed in the ceramic crucible through fully mixing, put into silicon molybdenum stove again and be raised to 1450 ℃~1480 ℃ with 1~3 ℃/minute, behind soaking time 〉=45min, shrend becomes the glass particle of 0.5~6mm, dry for standby; The exsiccant frit is laid in the refractory-material dies, upper strata glass particle granularity is 2~3mm, layer thickness is 10~20mm, insert the high temperature experimental furnace and be raised to 1050~1100 ℃ from room temperature with 3~5 ℃/minute temperature rise rate, soaking time 〉=1.5 hour, the glass particle crystallization is shakeout, be cooled to room temperature, obtain described devitrified glass through annealing.
3. preparation method as claimed in claim 2, when it is characterized in that preparing burden, raw materials used is silica sand, albite, rhombspar, calcite, zinc oxide, barium carbonate, soda ash, borax, weisspiessglanz and salt of wormwood.
4. preparation method as claimed in claim 2 is characterized in that: the thickness of prepared devitrified glass is 8~15mm.
CN 200910062856 2009-06-26 2009-06-26 Thin-type CaO-Al2O3-SiO2 system glass ceramics and preparation Expired - Fee Related CN101591144B (en)

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CN101787786A (en) * 2010-02-10 2010-07-28 姚桂龙 Preparation method of non-porous nano crystalline glass ground decoration tile
CN101792264A (en) * 2010-04-20 2010-08-04 香港福山实业有限公司 Microcrystalline jade and preparation method thereof
CN101767933B (en) * 2009-12-30 2012-05-30 陕西乾盛环保建材工程有限公司 Method utilizing coal gangue to manufacture microcrystalline glass plate material
CN103663967A (en) * 2013-12-06 2014-03-26 辽宁红山玉科技有限公司 Preparation method for jade-like microcrystalline glass
CN105060717A (en) * 2015-08-10 2015-11-18 武汉理工大学 Architectural decoration microcrystalline glass taking molybdic tailings as raw materials and preparation method therefor
CN105314851A (en) * 2015-12-14 2016-02-10 重庆大学 Long-acting antibacterial microcrystalline glass with blast furnace slag-doped transition metal oxides and preparation method of long-acting antibacterial microcrystalline glass
CN105330146A (en) * 2015-10-27 2016-02-17 武汉理工大学 Method for utilizing blast furnace slag to prepare engravable glass ceramics
CN112679224A (en) * 2021-01-27 2021-04-20 辽宁罕王绿色建材有限公司 Micro-crystallized porous ceramic plate and preparation method thereof
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CN1828282B (en) * 2006-03-30 2010-11-03 武汉理工大学 Neutron diffraction measure method for CaO-Al2O3-SiO2 system microcrystalline glass residue stress
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CN101767933B (en) * 2009-12-30 2012-05-30 陕西乾盛环保建材工程有限公司 Method utilizing coal gangue to manufacture microcrystalline glass plate material
CN101787786A (en) * 2010-02-10 2010-07-28 姚桂龙 Preparation method of non-porous nano crystalline glass ground decoration tile
CN101792264A (en) * 2010-04-20 2010-08-04 香港福山实业有限公司 Microcrystalline jade and preparation method thereof
CN103663967B (en) * 2013-12-06 2016-06-08 辽宁红山玉科技有限公司 A kind of preparation method of Jade-like microcrystalline glass
CN103663967A (en) * 2013-12-06 2014-03-26 辽宁红山玉科技有限公司 Preparation method for jade-like microcrystalline glass
CN105060717A (en) * 2015-08-10 2015-11-18 武汉理工大学 Architectural decoration microcrystalline glass taking molybdic tailings as raw materials and preparation method therefor
CN105060717B (en) * 2015-08-10 2018-06-26 武汉理工大学 It is a kind of using molybdic tailing as building decorative glass ceramics of main material and preparation method thereof
CN105330146A (en) * 2015-10-27 2016-02-17 武汉理工大学 Method for utilizing blast furnace slag to prepare engravable glass ceramics
CN105330146B (en) * 2015-10-27 2017-11-21 武汉理工大学 The method that can carve devitrified glass is prepared using blast furnace slag
CN105314851B (en) * 2015-12-14 2018-02-09 重庆大学 Long acting antibiotic devitrified glass of blast furnace slag containing transition metal oxide and preparation method thereof
CN105314851A (en) * 2015-12-14 2016-02-10 重庆大学 Long-acting antibacterial microcrystalline glass with blast furnace slag-doped transition metal oxides and preparation method of long-acting antibacterial microcrystalline glass
CN112679224A (en) * 2021-01-27 2021-04-20 辽宁罕王绿色建材有限公司 Micro-crystallized porous ceramic plate and preparation method thereof
CN113582549A (en) * 2021-08-11 2021-11-02 苏州大学 Microcrystalline glass and preparation method thereof

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