CN101898867B - Pyroceram-ceramic composite plate and preparation method thereof - Google Patents

Pyroceram-ceramic composite plate and preparation method thereof Download PDF

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Publication number
CN101898867B
CN101898867B CN2010102302811A CN201010230281A CN101898867B CN 101898867 B CN101898867 B CN 101898867B CN 2010102302811 A CN2010102302811 A CN 2010102302811A CN 201010230281 A CN201010230281 A CN 201010230281A CN 101898867 B CN101898867 B CN 101898867B
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glass
percent
ceramic
pyroceram
major ingredient
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CN101898867A (en
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郭兴忠
杨辉
杨广跃
李文彦
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a pyroceram-ceramic composite plate. The pyroceram in the composite plate consists of main materials and antimony trioxide (Sb2O3), wherein the Sb2O3 accounts for 0.8 to 1.2 percent of the total weight of the main materials; and the main materials consist of the following components in percentage by weight: 45 to 55 percent of silicon dioxide (SiO2), 4 to 10 percent of magnesium oxide (MgO), 15 to 20 percent of calcium oxide (CaO), 10 to 14 percent of aluminum oxide (Al2O3), 3 to 6 percent of sodium oxide (Na2O) or potassium oxide (K2O) and 6 to 10 percent of calcium fluoride (CaF2). The invention also discloses a method for preparing the pyroceram-ceramic composite plate. The method comprises the following steps of: 1) mixing the main materials and the Sb2O3 uniformly and heating the mixture; 2) pouring the obtained glass liquid into an iron mould to form and cool, then annealing, and preparing the obtained mother glass into glass powder and glass particles respectively; and 3) paving and scattering the glass powder and the glass particles on the conventional ceramic plate sequentially and then performing heat treatment. The pyroceram-ceramic composite plate has the characteristics of lower cost and high glossiness.

Description

A kind of microcrystal glass-ceramic compounded plate and preparation method thereof
Technical field
The present invention relates to a kind of microcrystal glass-ceramic compounded plate and preparation method thereof.
Background technology
Than traditional decorative ceramic board, advantage such as that microcrystalline glass decorative plate has is corrosion-resistant, wear-resistant, water-intake rate is low, but there are problems such as production cost height, complicated process of preparation, kind are single in present crystallizing glass decoration board, is difficult to popularization on a large scale.
Crystallizing glass decoration board commonly used is generally selected CaO-Al for use 2O 3-SiO 2System, CaO-MgO-SiO 2System or CaO-MgO-Al 2O 3-SiO 2The sytull of system, and, usually need in glass, add valuable ZnO, BaO and and Na in order to reach good sintering character and flowing property 2O (or K 2O) be mixed into ZnO+Na 2O, BaO+Na 2O or ZnO+BaO+Na 2Mixtures such as O are as fusing assistant.As being among CN00136831.1, CN1974455A, the CN1433985A at publication number, the add-on of its ZnO, BaO even reach about 10wt% makes that the production cost of sytull is higher.At publication number is among CN101186129A and the CN101186443A, and the artificial sytull production cost that reduces of invention adopts Li 2O replaces fusing assistant ZnO and BaO, but still needs to use the higher Li of price 2O, and its usage quantity is also bigger.Valuable raw material ZnO, BaO, Li 2The effect of fusing assistant has not only been played in the adding of O, thereby and the flowability that can improve glass reduce the thermal treatment temp of glass.
In addition, sintering process at present commonly used prepare sytull generally be with the direct lay of coarse particles frit that obtains after the shrend on ceramic bases, thermal treatment then.It utilize the coarse particles frit to be because still can maintain gloss after bakingout process; But because particle size is bigger, occur the space each other easily, in order to make final sytull densification, thermal treatment temp generally reaches 1100~1200 ℃.Like publication number is that treatment temp all reaches 1200 ℃ among CN101186129A and the CN101186443A.This certainly will improve the production cost of sytull again, and is totally unfavorable for producing in enormous quantities, promoting on a large scale.
Summary of the invention
The technical problem that the present invention will solve provides microcrystal glass-ceramic compounded plate that a kind of cost is lower, glossiness is good and preparation method thereof.
In order to solve the problems of the technologies described above, the present invention provides a kind of microcrystal glass-ceramic compounded plate, and the sytull in this composition board is by major ingredient with as the Sb of finings 2O 3Form Sb 2O 3Account for 0.8~1.2% of major ingredient gross weight; Said major ingredient is grouped into by the one-tenth of following percentage composition: the SiO of 45~55wt% 2, the MgO of 4~10wt%, the CaO of 15~20wt%, the Al of 10~14wt% 2O 3, 3~6wt% Na 2O or K 2The CaF of O and 6~10wt% 2
The present invention also provides the preparation method of above-mentioned microcrystal glass-ceramic compounded plate simultaneously, may further comprise the steps:
1), with major ingredient and Sb 2O 3Thorough mixing is even, places stove to be heated to 1450~1500 ℃ and be incubated 3.5~4.5h then, obtains clarifying uniform glass metal;
2), glass metal is poured in the swage into moulding and cooled off 1~2min, in 480~520 ℃ of annealing 0.5~1h down, obtain blocky mother glass afterwards; After half of mother glass pulverized glass powder, second half of mother glass is broken into the glass particle that particle diameter is 0.1~0.3mm;
3), get glass powder and evenly be laid on the conventional ceramic plate, becoming thickness is the glass frit layer of 1~2mm; And then with the glass particle of individual layer (being that glass particle does not produce superposition phenomenon up and down each other) evenly spreading on glass frit layer,, obtain microcrystal glass-ceramic compounded plate through 950~1000 ℃ of thermal treatment 2~3h.
Improvement as the preparation method of microcrystal glass-ceramic compounded plate of the present invention: the glass powder step 2) needed 200 mesh sieves.
The present invention be the contriver on the basis of sytull that studies for a long period of time, obtain through exploring technological process repeatedly.The present invention only adopts Na 2O and K 2O utilizes glass powder to replace coarse particles as fusing assistant, has not only removed valuable oxide compound ZnO, BaO, Li from 2The adding of O, and remedied because of lacking ZnO, BaO, Li 2O and the glass flow property variation that causes have also reduced the thermal treatment temp of glass simultaneously.In addition, the present invention lays glass particle on glass powder, relies on glass particle to handle the glossiness characteristics in back, has guaranteed the surface gloss after the sytull thermal treatment.
In sum, the present invention has following advantage:
The first, preparation sytull desired raw material is cheap raw material, does not contain Li 2The more expensive fusing assistants of price such as O, ZnO, BaO have effectively reduced the production cost of crystallizing glass sheet material, help it and produce and promote on a large scale.
The second, the present invention has combined the glass powder low-temperature heat treatment to be prone to after densification and the glass particle thermal treatment glossiness two specific characters are preferably arranged; The mother glass material is prepared into powder and particle respectively; And be layed in thermal treatment again on the ceramic plate successively; So both effectively reduce thermal treatment temp (minimum only need get final product for 950 ℃), guaranteed the glossiness on sytull surface simultaneously again.
Therefore, the present invention overcome existing microcrystal glass-ceramic compounded plate production cost higher, need to use the heat treated shortcoming of comparatively high temps.
Adopt the microcrystal glass-ceramic plate that the present invention produced, can be widely used in the family decorations such as exterior wall finish and high-grade public place such as airport, hotel, office building.
Embodiment
The preparation method of embodiment 1, a kind of microcrystal glass-ceramic compounded plate, its process step is following:
1), with the SiO of 45wt% 2, the MgO of 10wt%, the CaO of 20wt%, the Al of 14wt% 2O 3, 5wt% Na 2The CaF of O, 6wt% 2Form major ingredient, adding accounts for major ingredient gross weight 1wt%Sb 2O 3As finings, thorough mixing is even; Place stove to be heated to 1450 ℃ and be incubated 4h then, obtain clarifying uniform glass metal;
2), glass metal is poured in the swage into moulding and cooled off 2min, in 480 ℃ of annealing 0.5h down, obtain blocky mother glass afterwards.Half was ground into the glass powder of 200 mesh sieves with mother glass, and second half then is broken into the glass particle that particle diameter is 0.1~0.15mm, as the raw material of preparation glass-ceramic layer;
3), get glass powder and evenly be laid on the conventional ceramic plate, forming thickness is the glass frit layer of 1.5mm; And then the even spreading of the glass particle of individual layer (is the thickness≤0.15mm) of glass particle layer, through 950 ℃ of thermal treatment 2h, obtains microcrystal glass-ceramic compounded plate on glass frit layer.
Through range estimation, this microcrystal glass-ceramic compounded plate has surface gloss preferably.
The preparation method of embodiment 2, a kind of microcrystal glass-ceramic compounded plate, its process step is following:
1), with the SiO of 47wt% 2, the MgO of 10wt%, the CaO of 20wt%, the Al of 10wt% 2O 3, 3wt% K 2The CaF of O, 10wt% 2Form major ingredient, adding accounts for major ingredient gross weight 1wt%Sb 2O 3As finings, thorough mixing is even; Place stove to be heated to 1470 ℃ and be incubated 4h then, obtain clarifying uniform glass metal;
2), glass metal is poured in the swage into moulding and cooled off 1min, in 500 ℃ of annealing 0.5h down, obtain blocky mother glass afterwards.Half was ground into the glass powder of 200 mesh sieves with mother glass, and second half then is broken into the glass particle that particle diameter is 0.15~0.2mm, as the raw material of preparation glass-ceramic layer;
3), get glass powder and evenly be laid on the conventional ceramic plate, forming thickness is the glass frit layer of 2mm; And then the even spreading of the glass particle of individual layer (is the thickness≤0.2mm) of glass particle layer, through 980 ℃ of thermal treatment 3h, obtains microcrystal glass-ceramic compounded plate on glass frit layer.
Through range estimation, this microcrystal glass-ceramic compounded plate has surface gloss preferably.
The preparation method of embodiment 3, a kind of microcrystal glass-ceramic compounded plate, its process step is following:
1), with the SiO of 50wt% 2, the MgO of 9wt%, the CaO of 15wt%, the Al of 11wt% 2O 3, 6wt% Na 2The CaF of O, 9wt% 2Form major ingredient, adding accounts for major ingredient gross weight 1wt%Sb 2O 3As finings, thorough mixing is even; Place stove to be heated to 1480 ℃ and be incubated 4h then, obtain clarifying uniform glass metal;
2), glass metal is poured in the swage into moulding and cooled off 2min, in 510 ℃ of annealing 1h down, obtain blocky mother glass afterwards.Half was ground into the glass powder of 200 mesh sieves with mother glass, and second half then is broken into the glass particle that particle diameter is 0.2~0.3mm, as the raw material of preparation glass-ceramic layer;
3), get glass powder and evenly be laid on the conventional ceramic plate, forming thickness is the glass frit layer of 1mm; And then the even spreading of the glass particle of individual layer (is the thickness≤0.3mm) of glass particle layer, through 1000 ℃ of thermal treatment 2h, obtains microcrystal glass-ceramic compounded plate on glass frit layer.
Through range estimation, this microcrystal glass-ceramic compounded plate has surface gloss preferably.
The preparation method of embodiment 4, a kind of microcrystal glass-ceramic compounded plate, its process step is following:
1), with the SiO of 52wt% 2, the MgO of 4wt%, the CaO of 17wt%, the Al of 13wt% 2O 3, 4wt% Na 2The CaF of O, 10wt% 2Form major ingredient, adding accounts for major ingredient gross weight 1wt%Sb 2O 3As finings, thorough mixing is even; Place stove to be heated to 1490 ℃ and be incubated 4h then, obtain clarifying uniform glass metal;
2), glass metal is poured in the swage into moulding and cooled off 1min, in 520 ℃ of annealing 0.5h down, obtain blocky mother glass afterwards.Half was ground into the glass powder of 200 mesh sieves with mother glass, and second half then is broken into the glass particle that particle diameter is 0.2~0.3mm, as the raw material of preparation glass-ceramic layer;
3), get glass powder and evenly be laid on the conventional ceramic plate, forming thickness is the glass frit layer of 1.5mm; And then the even spreading of the glass particle of individual layer (is the thickness≤0.3mm) of glass particle layer, through 980 ℃ of thermal treatment 2.5h, obtains microcrystal glass-ceramic compounded plate on glass frit layer.
Through range estimation, this microcrystal glass-ceramic compounded plate has surface gloss preferably.
The preparation method of embodiment 5, a kind of microcrystal glass-ceramic compounded plate, its process step is following:
1), with the SiO of 55wt% 2, the MgO of 5wt%, the CaO of 16wt%, the Al of 14wt% 2O 3, 4wt% K 2The CaF of O, 6wt% 2Form major ingredient, adding accounts for major ingredient gross weight 1wt%Sb 2O 3As finings, thorough mixing is even; Place stove to be heated to 1500 ℃ and be incubated 4h then, obtain clarifying uniform glass metal;
2), glass metal is poured in the swage into moulding and cooled off 2min, in 520 ℃ of annealing 1h down, obtain blocky mother glass afterwards.Half was ground into the glass powder of 200 mesh sieves with mother glass, and second half then is broken into the glass particle that particle diameter is 0.2~0.3mm, as the raw material of preparation glass-ceramic layer;
3), get glass powder and evenly be laid on the conventional ceramic plate, forming thickness is the glass frit layer of 2mm; And then the even spreading of the glass particle of individual layer (is the thickness≤0.3mm) of glass particle layer, through 990 ℃ of thermal treatment 3h, obtains microcrystal glass-ceramic compounded plate on glass frit layer.
Through range estimation, this microcrystal glass-ceramic compounded plate has surface gloss preferably.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.

Claims (2)

1. the preparation method of a microcrystal glass-ceramic compounded plate is characterized in that: the sytull in this composition board is by major ingredient with as the Sb of finings 2O 3Form Sb 2O 3Account for 0.8~1.2% of major ingredient gross weight; Said major ingredient is grouped into by the one-tenth of following percentage composition: the SiO of 45~55wt% 2, the MgO of 4~10wt%, the CaO of 15~20wt%, the Al of 10~14wt% 2O 3, 3~6wt% Na 2O or K 2The CaF of O and 6~10wt% 2May further comprise the steps
1), with major ingredient and Sb 2O 3Thorough mixing is even, places stove to be heated to 1450~1500 ℃ and be incubated 3.5~4.5h then, obtains clarifying uniform glass metal;
2), glass metal is poured in the swage into moulding and cooled off 1~2min, in 480~520 ℃ of annealing 0.5~1h down, obtain blocky mother glass afterwards; After half of mother glass pulverized glass powder, second half of mother glass is broken into the glass particle that particle diameter is 0.1~0.3mm;
3), get glass powder and evenly be laid on the conventional ceramic plate, becoming thickness is the glass frit layer of 1~2mm; And then with the even spreading of the glass particle of individual layer on glass frit layer, through 950~1000 ℃ of thermal treatment 2~3h, obtain microcrystal glass-ceramic compounded plate.
2. the preparation method of microcrystal glass-ceramic compounded plate according to claim 1, it is characterized in that: the glass powder said step 2) is crossed 200 mesh sieves.
CN2010102302811A 2010-07-19 2010-07-19 Pyroceram-ceramic composite plate and preparation method thereof Expired - Fee Related CN101898867B (en)

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CN102643024B (en) * 2012-04-10 2014-04-02 中原工学院 Magnesium oxide (MgO)-silicon dioxide (SiO2)-aluminum oxide (Al2O3)-boron trioxide (B2O3)-potassium fluoride (KF) glass ceramic composite material adopting silicon carbide (SiC) as enhanced-phase and preparation method thereof

Citations (3)

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Publication number Priority date Publication date Assignee Title
CN1884206A (en) * 2006-07-10 2006-12-27 中国地质大学(武汉) Process for preparing microcrystal glass-ceramic compounded plate
CN1974456A (en) * 2006-12-11 2007-06-06 巫汉生 Etched microcrystalline glass plate and its production process
CN1974455A (en) * 2006-12-11 2007-06-06 佛山欧神诺陶瓷有限公司 Integrally crystallization process microcrystaline glass-ceramic composite brick and its production process

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1884206A (en) * 2006-07-10 2006-12-27 中国地质大学(武汉) Process for preparing microcrystal glass-ceramic compounded plate
CN1974456A (en) * 2006-12-11 2007-06-06 巫汉生 Etched microcrystalline glass plate and its production process
CN1974455A (en) * 2006-12-11 2007-06-06 佛山欧神诺陶瓷有限公司 Integrally crystallization process microcrystaline glass-ceramic composite brick and its production process

Non-Patent Citations (1)

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