CN106587637A - Preparation method of microcrystalline glass - Google Patents
Preparation method of microcrystalline glass Download PDFInfo
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- CN106587637A CN106587637A CN201611228013.XA CN201611228013A CN106587637A CN 106587637 A CN106587637 A CN 106587637A CN 201611228013 A CN201611228013 A CN 201611228013A CN 106587637 A CN106587637 A CN 106587637A
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- preparation
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- glass
- devitrified glass
- raw material
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
Abstract
The invention belongs to the technical field of glass and particularly relates to a preparation method of microcrystalline glass. The preparation method comprises the following preparation steps: 1) weighing raw materials in parts by weight and ball-milling the raw materials; 2) drying, screening and smelting the raw materials to prepare uniform molten glass; 3) moulding the molten glass by casting and performing annealing treatment to obtain a glass sheet; and 4) nucleating the glass sheet, and then enabling the crystal nucleus to grow to obtain the microcrystalline glass. The microcrystalline glass prepared by the preparation method of microcrystalline glass is low in coefficient of thermal expansion, wide in low expansion using temperature range, low in melting temperature, good in toughness, high in strength, low in water absorption and free of radiation.
Description
Technical field
The invention belongs to glass technology field, more particularly to a kind of preparation method of devitrified glass.
Background technology
With the stable sustainable development of Chinese national economy, people's living standard is improved therewith, the demand day to high-grade material
Benefit expands, particularly more urgent to the substitute products demand of radiationless high-grade stone, but the replacement of the high-grade stone of the country is produced
Product fragility is big, it is not easy to machine-shaping, causes many high-grade stone needs from external import, and cost is significantly increased.
Devitrified glass is also called glass-ceramic, and the double grading with glass and ceramics, devitrified glass is made up of crystal, its
Atomic arrangement is regular, therefore, devitrified glass is higher and stronger than glass toughness than the brightness of ceramics.Devitrified glass has concentrated glass
Triple advantages of glass, ceramics and lithotome, better than lithotome and ceramics, can be used for building curtain wall and indoor high-grade decoration,
Structural material mechanically, the insulant on electronics, electrician, the baseboard material of large scale integrated circuit, microwave oven can also be done
Heat-resisting row vessel, chemical industry and anti-corrosion material and mine high-abrasive material etc., become the substitute products of preferable high-grade stone.
But existing devitrified glass, the melting temperature of the glass precursor in its manufacture process is generally very high, be 1450 DEG C~
1600℃.These devitrified glasses in order to manufacture process melting when homogenize with it is fining, clarifier can be added, as front
Such high effective clarifier of temperature province is stated, always using arsenic composition, antimony composition.But, arsenic composition, antimony composition may
Deleterious effect can be brought to human body and environment, control as far as possible is improved using the requirement of these compositions.
Additionally, in the existing method for preparing devitrified glass, the devitrified glass thermal coefficient of expansion for preparing is relatively still
It is somewhat high, even if preparing low-expansion devitrified glass, but still Shortcomings:The fusion temperature of the glass is too high, reaches
More than 1600 DEG C, the high temperature resistant and hot erosion resistant to glass-melting furnace requires extremely harshness, and domestic refractory material is difficult to meet and wants
Ask, smelting furnace can only be built by import refractory material, improve cost;In system components, industrial chemicals Li2O large usage quantities, and
Li2O's is expensive, makes glass relatively costly;The low bulk of glass is narrower using temperature range, and maximum temperature is 800 DEG C.
The content of the invention
The technical problem to be solved is to provide without harmful components such as arsenic composition, antimony compositions, and thermal expansion system
The preparation method of the low devitrified glass of number.
For achieving the above object, the present invention is adopted the following technical scheme that:
The present invention provides a kind of preparation method of devitrified glass, including following preparation process:
1) raw material is weighed by weight, adds ball-milling medium 20~30h of ball milling;
2) dry, sieve, be incubated 30~60min at 1150 DEG C~1250 DEG C and be melting into uniform glass liquid;
3) the rapid moulding by casting of vitreous humour, then anneal 6~8h in 480 DEG C~510 DEG C of annealing furnace, obtains glass
Piece;
4) sheet glass is incubated into 2h at 590 DEG C~600 DEG C makes nucleation, and being then incubated 3h at 700 DEG C~730 DEG C makes nucleus long
Greatly, devitrified glass is obtained.
Preferably, step 1 of the present invention) in, raw material is made up of the raw material of following weight portion:Silicon dioxide 20~50
Part, 8~20 parts of Calcium Carbonate, 3~15 parts of aluminium oxide, 2~8 parts of strontium carbonate, 0.1~0.7 part of lithium carbonate, Disamarium trioxide 0.02~0.14
Part.
Preferably, step 1 of the present invention) in, ball-milling medium is dehydrated alcohol.
Preferably, step 1 of the present invention) in, zirconia ball ball milling is used, raw material can be made more uniform.
It is highly preferred that step 1 of the present invention) in, raw material is made up of the raw material of following weight portion:35 parts of silicon dioxide,
14 parts of Calcium Carbonate, 9 parts of aluminium oxide, 5 parts of strontium carbonate, 0.4 part of lithium carbonate, 0.08 part of Disamarium trioxide.
Preferably, step 2 of the present invention) in, with 19~25 DEG C/min ramps.It is rapidly heated in this speed,
The bulk density of devitrified glass is significantly improved, sintering activation energy, stomatal frequency and pore size is reduced, devitrified glass is significantly improved
Bending strength.It is rapidly heated with such speed, low viscosity glass is mutually conducive to the growth of bar-shaped and needle-like anorthite crystalline phase, rises
To the effect of reinforcing devitrified glass.
Preferably, step 2 of the present invention) in, 100 mesh sieves are crossed, this particle diameter contributes to reducing solution temperature.
Preferably, step 4 of the present invention) in, sheet glass is incubated nucleation at 595 DEG C.
Preferably, step 4 of the present invention) in, make nuclei growth in 715 DEG C of insulations.
The beneficial effects of the present invention is:
1st, the devitrified glass thermal coefficient of expansion that the preparation method of devitrified glass of the invention is prepared is low, and low bulk makes
Use temperature range width.
2nd, the preparation method melting temperature of devitrified glass of the invention is low, energy saving and cost.
3rd, the devitrified glass that the preparation method of devitrified glass of the invention is prepared have natural jade moisture and
Waxiness sense, good toughness, intensity are high, water absorption rate is low, radiationless, are easily processed further molding, and low cost, conforming product rate
Height, can be widely used in the fields such as the succedaneum of high-grade stone.
4th, the preparation method preparation method of devitrified glass of the invention is simple, it is easy to operate, pollution-free.
Specific embodiment
With reference to embodiments the invention will be further described, but the invention is not limited in these embodiments.
Embodiment 1
A kind of preparation method of devitrified glass, including following preparation process:
1) following raw material is weighed by weight:20 parts of silicon dioxide, 20 parts of Calcium Carbonate, 3 parts of aluminium oxide, 8 parts of strontium carbonate, carbon
0.1 part of sour lithium, 0.14 part of Disamarium trioxide;
2) dehydrated alcohol is added, with zirconia ball ball milling 20h;
3) dry, cross 100 mesh sieves, with 25 DEG C/min ramps to 1150 DEG C, insulation 60min is melting into uniform glass
Liquid;
4) the rapid moulding by casting of vitreous humour, then anneal 6h in 480 DEG C of annealing furnace, obtains sheet glass;
5) sheet glass is incubated into 2h at 590 DEG C makes nucleation, and being then incubated 3h at 730 DEG C makes nuclei growth, obtains crystallite glass
Glass.
Performance test:Thermal coefficient of expansion is 0.2 × 10-7/℃;The thermal coefficient of expansion is 290~890 using temperature range
℃;Water absorption rate is 1%;Impact flexibility is 5.9kJcm3;Mohs' hardness is 6.6;Rupture strength is 96MPa, and comprcssive strength is
890MPa。
Embodiment 2
A kind of preparation method of devitrified glass, including following preparation process:
1) following raw material is weighed by weight:25 parts of silicon dioxide, 18 parts of Calcium Carbonate, 5 parts of aluminium oxide, 7 parts of strontium carbonate, carbon
0.2 part of sour lithium, 0.12 part of Disamarium trioxide;
2) dehydrated alcohol is added, with zirconia ball ball milling 22h;
3) dry, cross 100 mesh sieves, with 24 DEG C/min ramps to 1170 DEG C, insulation 55min is melting into uniform glass
Liquid;
4) the rapid moulding by casting of vitreous humour, then anneal 8h in 485 DEG C of annealing furnace, obtains sheet glass;
5) sheet glass is incubated into 2h at 592 DEG C makes nucleation, and being then incubated 3h at 725 DEG C makes nuclei growth, obtains crystallite glass
Glass.
Performance test:Thermal coefficient of expansion is 0.3 × 10-7/℃;The thermal coefficient of expansion is 295~885 using temperature range
℃;Water absorption rate is 3%;Impact flexibility is 6.2kJcm3;Mohs' hardness is 6.6;Rupture strength is 95MPa, and comprcssive strength is
880MPa。
Embodiment 3
A kind of preparation method of devitrified glass, including following preparation process:
1) following raw material is weighed by weight:30 parts of silicon dioxide, 16 parts of Calcium Carbonate, 7 parts of aluminium oxide, 6 parts of strontium carbonate, carbon
0.3 part of sour lithium, 0.1 part of Disamarium trioxide;
2) dehydrated alcohol is added, with zirconia ball ball milling 24h;
3) dry, cross 100 mesh sieves, with 23 DEG C/min ramps to 1180 DEG C, insulation 50min is melting into uniform glass
Liquid;
4) the rapid moulding by casting of vitreous humour, then anneal 6h in 490 DEG C of annealing furnace, obtains sheet glass;
5) sheet glass is incubated into 2h at 594 DEG C makes nucleation, and being then incubated 3h at 720 DEG C makes nuclei growth, obtains crystallite glass
Glass.
Performance test:Thermal coefficient of expansion is 0.3 × 10-7/℃;The thermal coefficient of expansion is 300~880 using temperature range
℃;Water absorption rate is 2%;Impact flexibility is 6.3kJcm3;Mohs' hardness is 6.8;Rupture strength is 101MPa, and comprcssive strength is
850MPa。
Embodiment 4
A kind of preparation method of devitrified glass, including following preparation process:
1) following raw material is weighed by weight:35 parts of silicon dioxide, 14 parts of Calcium Carbonate, 9 parts of aluminium oxide, 5 parts of strontium carbonate, carbon
0.4 part of sour lithium, 0.08 part of Disamarium trioxide;
2) dehydrated alcohol is added, with zirconia ball ball milling 26h;
3) dry, cross 100 mesh sieves, with 22 DEG C/min ramps to 1200 DEG C, insulation 45min is melting into uniform glass
Liquid;
4) the rapid moulding by casting of vitreous humour, then anneal 7h in 495 DEG C of annealing furnace, obtains sheet glass;
5) sheet glass is incubated into 2h at 595 DEG C makes nucleation, and being then incubated 3h at 715 DEG C makes nuclei growth, obtains crystallite glass
Glass.
Performance test:Thermal coefficient of expansion is 0.4 × 10-7/℃;The thermal coefficient of expansion is 305~885 using temperature range
℃;Water absorption rate is 3%;Impact flexibility is 6.4kJcm3;Mohs' hardness is 6.7;Rupture strength is 105MPa, and comprcssive strength is
875MPa。
Embodiment 5
A kind of preparation method of devitrified glass, including following preparation process:
1) following raw material is weighed by weight:40 parts of silicon dioxide, 12 parts of Calcium Carbonate, 11 parts of aluminium oxide, 4 parts of strontium carbonate,
0.5 part of lithium carbonate, 0.06 part of Disamarium trioxide;
2) dehydrated alcohol is added, with zirconia ball ball milling 28h;
3) dry, cross 100 mesh sieves, with 21 DEG C/min ramps to 1230 DEG C, insulation 40min is melting into uniform glass
Liquid;
4) the rapid moulding by casting of vitreous humour, then anneal 8h in 450 DEG C of annealing furnace, obtains sheet glass;
5) sheet glass is incubated into 2h at 597 DEG C makes nucleation, and being then incubated 3h at 710 DEG C makes nuclei growth, obtains crystallite glass
Glass.
Performance test:Thermal coefficient of expansion is 0.3 × 10-7/℃;The thermal coefficient of expansion is 310~880 using temperature range
℃;Water absorption rate is 3%;Impact flexibility is 6.7kJcm3;Mohs' hardness is 7;Rupture strength is 108MPa, and comprcssive strength is
885MPa。
Embodiment 6
A kind of preparation method of devitrified glass, including following preparation process:
1) following raw material is weighed by weight:45 parts of silicon dioxide, 10 parts of Calcium Carbonate, 13 parts of aluminium oxide, 3 parts of strontium carbonate,
0.6 part of lithium carbonate, 0.04 part of Disamarium trioxide;
2) dehydrated alcohol is added, with zirconia ball ball milling 30h;
3) dry, cross 100 mesh sieves, with 20 DEG C/min ramps to 1240 DEG C, insulation 35min is melting into uniform glass
Liquid;
4) the rapid moulding by casting of vitreous humour, then anneal 7h in 505 DEG C of annealing furnace, obtains sheet glass;
5) sheet glass is incubated into 2h at 598 DEG C makes nucleation, and being then incubated 3h at 705 DEG C makes nuclei growth, obtains crystallite glass
Glass.
Performance test:Thermal coefficient of expansion is 0.3 × 10-7/℃;The thermal coefficient of expansion is 305~880 using temperature range
℃;Water absorption rate is 3%;Impact flexibility is 6.4kJcm3;Mohs' hardness is 6.6;Rupture strength is 101MPa, and comprcssive strength is
900MPa。
Embodiment 7
A kind of preparation method of devitrified glass, including following preparation process:
1) following raw material is weighed by weight:50 parts of silicon dioxide, 8 parts of Calcium Carbonate, 15 parts of aluminium oxide, 2 parts of strontium carbonate, carbon
0.7 part of sour lithium, 0.02 part of Disamarium trioxide;
2) dehydrated alcohol is added, with zirconia ball ball milling 24h;
3) dry, cross 100 mesh sieves, with 19 DEG C/min ramps to 1250 DEG C, insulation 30min is melting into uniform glass
Liquid;
4) the rapid moulding by casting of vitreous humour, then anneal 6h in 510 DEG C of annealing furnace, obtains sheet glass;
5) sheet glass is incubated into 2h at 600 DEG C makes nucleation, and being then incubated 3h at 700 DEG C makes nuclei growth, obtains crystallite glass
Glass.
Performance test:Thermal coefficient of expansion is 0.4 × 10-7/℃;The thermal coefficient of expansion is 300~880 using temperature range
℃;Water absorption rate is 1%;Impact flexibility is 6.3kJcm3;Mohs' hardness is 7;Rupture strength is 103MPa, and comprcssive strength is
895MPa。
Claims (8)
1. a kind of preparation method of devitrified glass, it is characterised in that including following preparation process:
1) raw material is weighed by weight, adds ball-milling medium 20~30h of ball milling;
2) dry, sieve, be incubated 30~60min at 1150 DEG C~1250 DEG C and be melting into uniform glass liquid;
3) the rapid moulding by casting of vitreous humour, then anneal 6~8h in 480 DEG C~510 DEG C of annealing furnace, obtains sheet glass;
4) sheet glass is incubated into 2h at 590 DEG C~600 DEG C makes nucleation, and being then incubated 3h at 700 DEG C~730 DEG C makes nuclei growth,
Obtain devitrified glass;
Described step 1) in, raw material is made up of the raw material of following weight portion:20~50 parts of silicon dioxide, 8~20 parts of Calcium Carbonate,
3~15 parts of aluminium oxide, 2~8 parts of strontium carbonate, 0.1~0.7 part of lithium carbonate, 0.02~0.14 part of Disamarium trioxide.
2. the preparation method of devitrified glass according to claim 1, it is characterised in that:The step 1) in, ball-milling medium
For dehydrated alcohol.
3. the preparation method of devitrified glass according to claim 1, it is characterised in that:The step 1) in, use zirconium oxide
Ball ball milling.
4. the preparation method of devitrified glass according to claim 1, it is characterised in that:The step 1) in, raw material by with
The raw material of lower weight portion is made:35 parts of silicon dioxide, 14 parts of Calcium Carbonate, 9 parts of aluminium oxide, 5 parts of strontium carbonate, 0.4 part of lithium carbonate, oxygen
Change 0.08 part of samarium.
5. the preparation method of devitrified glass according to claim 1, it is characterised in that:The step 2) in, with 19~25
DEG C/min ramps.
6. the preparation method of devitrified glass according to claim 1, it is characterised in that:The step 2) in, cross 100 mesh
Sieve.
7. the preparation method of devitrified glass according to claim 1, it is characterised in that:The step 4) in, sheet glass exists
595 DEG C of insulation nucleation.
8. the preparation method of devitrified glass according to claim 1, it is characterised in that:The step 4) in, in 715 DEG C of guarantors
Temperature makes nuclei growth.
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CN201611228013.XA CN106587637A (en) | 2016-12-27 | 2016-12-27 | Preparation method of microcrystalline glass |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107902910A (en) * | 2017-12-27 | 2018-04-13 | 安徽凤阳亚欧玻璃工艺品有限公司 | A kind of corrosion-resistant devitrified glass |
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2016
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CN1065646A (en) * | 1991-04-05 | 1992-10-28 | 湖北省化学研究所 | Slag microcrystalline glass directly made by industry furnace molten cinder |
CN1172778A (en) * | 1996-02-28 | 1998-02-11 | 日本电气硝子株式会社 | Nucleated glass with natural marble figue used as building material and its making method |
CN101186443A (en) * | 2007-12-07 | 2008-05-28 | 霍镰泉 | Building microcrystalline glass and producing method thereof |
CN101265027A (en) * | 2008-03-18 | 2008-09-17 | 深圳市和兴泰实业有限公司 | Formulation of imperforate micro-spar sheet material and manufacturing method thereof |
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CN107902910A (en) * | 2017-12-27 | 2018-04-13 | 安徽凤阳亚欧玻璃工艺品有限公司 | A kind of corrosion-resistant devitrified glass |
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Application publication date: 20170426 |