CN101591144B - Thin-type CaO-Al2O3-SiO2 system glass ceramics and preparation - Google Patents
Thin-type CaO-Al2O3-SiO2 system glass ceramics and preparation Download PDFInfo
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- CN101591144B CN101591144B CN 200910062856 CN200910062856A CN101591144B CN 101591144 B CN101591144 B CN 101591144B CN 200910062856 CN200910062856 CN 200910062856 CN 200910062856 A CN200910062856 A CN 200910062856A CN 101591144 B CN101591144 B CN 101591144B
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Abstract
The invention relates to CaO-Al2O3-SiO2 system glass ceramics, which comprises the following chemical compositions in percentage by weight: 60.0 to 70.0 percent of SiO2, 5.0 to 10.0 percent of Al2O3, 16.5 to 18.0 percent of CaO, 0 to 2.5 percent of ZnO, 4.0 to 6.0 percent of BaO, 5.0 to 6.0 percent of Na2O, 0.5 to 2.0 percent of K2O, 1.0 to 3.0 percent of B2O3, 0.5 to 1.0 percent of Sb2O3 and 1.0 to 3.0 percent of MgO. The preparation method of the system glass ceramics comprises the following steps: stirring the compositions evenly; putting the compositions in a ceramic crucible and then putting in a MoSi2 furnace for heating and heat preservation; forming 0.5 to 6mm glass granules by water quenching and then drying the granules; spreading the granules in a die made of fireproof material, and putting the die in a high-temperature furnace for heating and heat preservation to crystallize and flatten the glass granules; and finally, annealing and cooling to room temperature. The thin-type CaO-Al2O3-SiO2 system glass ceramics has the advantages of low cost, ideal performance, thin type and wide application.
Description
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, the advantages such as protection against corrosion day by day are familiar with and are approved by people.Devitrified glass has had multiple utilization in building trade, is used for the high-grade house places such as the 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 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, protection of the 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, such as flyash, coal gangue, blast furnace slag, various mining mine tailings etc.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 namely the solid waste consumption is larger, and the performance loss of product is just larger.Meanwhile, the major equipment of producing at present the Sintering of Glass-Ceramics decorative sheet is tunnel like and shuttle-type sintering crystallization kiln, and the thickness of the crystallizing glass decoration board of producing is (thick template) in the scope of 18～30mm.Cause thus its weight per unit area large, yield poorly, the raw material consumption of product is large, energy consumption is high.
Therefore, be necessary the low-cost glass ingredient of development of new, increase crystallizing glass sheet material assortment, improve the quality of products and labour productivity, will become the from now on main development 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 from making the used raw material of devitrified glass, adjust the chemical constitution of described 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 composition 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 composition batching, this batching is placed in the ceramic crucible through fully mixing, put into again silicon molybdenum stove 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 frit of drying is laid in the refractory-material dies, upper strata glass particle granularity is 2～3mm, layer thickness is 10～20mm, insert high-temperature experimental furnace and be raised to 1050～1100 ℃ with 3～5 ℃/minute temperature rise rate from room temperature, soaking time 〉=1.5 hour, the glass particle crystallization is shakeout, be cooled to room temperature through annealing, obtain described devitrified glass.
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: 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 Industry Core Competitive support that provides the necessary technical.
They are five years old. and development prospect is wide: because quality product improves, cost is conducive to utilize 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%, calcium 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 is conducive to 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, then dries classification.The glass particle material of drying is tiled on the refractory-material dies, and the upper strata grain graininess is 2～3mm, and layer thickness is 20mm.Stone and strike off after, be placed on 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 processing through crystallization sinters an integral body into, and separates out a large amount of wollastonite crystal.Be annealed at last room temperature, make the devitrified glass sample.
The composition of the devitrified glass that obtains (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%, calcium 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, then dries classification.The glass particle material of drying is tiled on the refractory-material dies, and the upper strata grain graininess is 2～3mm, and layer thickness is 20mm.Stone and strike off after, be placed on 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 processing through crystallization sinters an integral body into, and separates out a large amount of wollastonite crystal.Be annealed at last room temperature, 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%, calcium 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 MgO 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, then dries classification.The glass particle material of drying is tiled on the refractory-material dies, and the upper strata grain graininess is 2～3mm, and layer thickness is 20mm.Stone and strike off after, be placed on 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 processing through crystallization sinters an integral body into, and separates out a large amount of wollastonite crystal.Be annealed at last room temperature, 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%, calcium 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 finally improves the overall mechanical properties of finished product to improve the network connection degree of glassy phase.
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, then dries classification.The glass particle material of drying is tiled on the refractory-material dies, and the upper strata grain graininess is 2～3mm, and layer thickness is 20mm.Stone and strike off after, be placed on 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 processing through crystallization sinters an integral body into, and separates out a large amount of wollastonite crystal.Be annealed at last room temperature, 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 composition of this devitrified glass is: 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%, above each component sum is 100%.
2. the preparation method of a devitrified glass claimed in claim 1 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 composition batching, this batching is placed in the ceramic crucible through fully mixing, put into again silicon molybdenum stove 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 frit of drying is laid in the refractory-material dies, upper strata glass particle granularity is 2～3mm, layer thickness is 10～20mm, insert high-temperature experimental furnace and be raised to 1050～1100 ℃ with 3～5 ℃/minute temperature rise rate from room temperature, 1050～1100 ℃ of soaking time 〉=1.5 hour, the glass particle crystallization is shakeout, be cooled to room temperature through annealing, obtain described devitrified glass.
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, it is characterized in that: the thickness of prepared devitrified glass is 8～15mm.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN101787786B (en) * | 2010-02-10 | 2012-07-18 | 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 |
| 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 |
| 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 |
| CN112679224B (en) * | 2021-01-27 | 2022-09-16 | 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 |
| CN115745380A (en) * | 2022-10-31 | 2023-03-07 | 苏州大学 | Light sintered microcrystal plate and sintering process thereof |
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Inventor after: Cheng Jinshu Inventor after: He Feng Inventor after: Xie Jun Inventor after: Lu Ping Inventor after: Zheng Weihong Inventor after: Quan Jian Inventor after: Xiao Zifan Inventor before: Xie Jun Inventor before: Cheng Jinshu Inventor before: He Feng Inventor before: Lu Ping Inventor before: Zheng Weihong Inventor before: Quan Jian Inventor before: Xiao Zifan |
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