CN106517776B - A kind of preparation method of red copper star scintillation glass - Google Patents

A kind of preparation method of red copper star scintillation glass Download PDF

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CN106517776B
CN106517776B CN201610919779.6A CN201610919779A CN106517776B CN 106517776 B CN106517776 B CN 106517776B CN 201610919779 A CN201610919779 A CN 201610919779A CN 106517776 B CN106517776 B CN 106517776B
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temperature
star
red copper
rate
preparation
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CN106517776A (en
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郭宏伟
宋建波
白胜利
罗亚丽
宁峰鸣
吴明
杨晨
杨龙康
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Shaanxi University of Science and Technology
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    • 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
    • C03C1/04—Opacifiers, e.g. fluorides or phosphates; Pigments
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00—Annealing glass products
    • 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
    • C03C4/00—Compositions for glass with special properties
    • C03C4/02—Compositions for glass with special properties for coloured glass

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

A kind of preparation method of red copper star scintillation glass, by sodium carbonate, cuprous oxide, quartz sand, potassium carbonate, Pb3O4, borax, sodium nitrate, iron powder, stannous oxide, aluminium powder, high temperature sintering is after fluorite mixing up to red copper star scintillation glass；The disadvantages such as the method that the present invention uses multilevel reduction agent to be used in mixed way, avoids traditional preparation methods, and specimen surface oxide layer is blocked up, and sample section Venus is uneven, and product utilization is low, and production efficiency is low；Meanwhile this method is using the crystallization process that cools down step by step, thoroughly solves that color difference in the crystallization process that heated up after traditional aventurine glass cooling again is big and the non-uniform disadvantage of grain growth；Copper star source is added using multiple, has fully ensured that the formation of sample intermediate cam shape copper simple substance, has shown star excellent effect；The color method of the application is conducive to large-scale production, and the preparation process time is short, high efficiency, and the aobvious star effect of sample is good, and color is uniform.

Description

A kind of preparation method of red copper star scintillation glass
Technical field
The present invention relates to a kind of preparation method of scintillation glass, in particular to a kind of preparation side of red copper star scintillation glass Method.
Background technique
Copper aventurine glass is integrally in the brown, yellowish-brown, puce of milkiness, is uniform-distribution with the triangle of 0.5~1mm size The flaky crystal of shape or hexagonal metallic copper, or the grain crystalline less than 130 μm, reflect bright golden yellow, it appears rich It is beautiful luxurious, it is similar to aventurine.Copper aventurine glass can be engraved as the arts work such as scenery with hills and waters, personage, flowers and decoration as jade Product can also fuse in various coloured glasss, and the different art work and craftwork are configured to through jacking, like gold inlays it In, a kind of dazzling golden colour lustre is generated after light irradiates, and gives people a kind of special aesthetic feeling.Copper aventurine glass is also preparation The main material of decorative board for building, mosaic and goldstone glaze with flashing Venus.
Physics that red copper star scintillation glass not only has general glass excellent, chemistry, mechanical property, and it is internal with dodging Bright charming point point Venus has high decorative effect.
CN1084834A discloses the manufacturing method of gold star glass making method from tail sand of gold mine, using gold ore tailing as main former The additive of material and the common cheap raw material of glass industry and a small amount of formation Venus pedestal is melted through sufficiently mixing after, at It is made after type, annealing, using gold ore tailing, cost is greatly lowered, but the Venus grain diameter formed is smaller, is not achieved very well Decorative effect.CN1100388A discloses a kind of preparation method of copper aventurine glass mosaic, in parent glass liquid, uniformly Put into copper aventurine glass particle, it is repressed after molding, but it needs to prepare aventurine glass in advance, complex procedures, and in finished product Venus granule content is less.CN2139579Y discloses the preparation method of composite coloured golden star ornamental glass, it is characterized in that anti- It penetrates the high flasher of rate to be added in glue mucus, then is coated on glass plate, just can form flashing bright spot on a glass, have fabulous Decorative effect, but its only Venus is contained on surface, intolerant to abrasion, and use environment is limited by temperature.
Summary of the invention
It is an object of the invention to overcome the above-mentioned prior art, it is simple to provide a kind of preparation process, shows star effect Fruit is excellent, and Venus color is uniform, sample high yield rate, the preparation method of low-cost red copper star scintillation glass.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) quartz sand 55~65%, sodium carbonate 12~18%, potassium carbonate 1~5%, Pb are taken by mass fraction3O46~ 10%, borax 3~9%, sodium nitrate 0.5~3%, cuprous oxide 3~7%, iron powder 1~4%, stannous oxide 1~3%, aluminium powder 0.1~0.5%, fluorite 0.2~5%；
2) sodium carbonate and cuprous oxide are uniformly mixed, and take out after the mixture 30% is used as and adds mixture；
3) the remaining mixture of step 2) and other surplus stocks are uniformly mixed, and by 30 mesh standard sieves, are formed Batch；
4) batch addition has been warming up in 1350~1450 DEG C of silica crucible, after keeping the temperature 30min, by step 2) It is primary that stirring in crucible is added in the half of the mixture of taking-up；
5) after keeping the temperature 30min again, remaining mixture is added again in crucible and is stirred primary；
6) furnace temperature is down to 1330~1430 DEG C, keeps the temperature 30~120min；
7) furnace temperature is down to 950 DEG C according to the rate of temperature fall of 8~10 DEG C/min, keeps the temperature 5~10min；
8) furnace temperature is down to 780 DEG C according to the rate of temperature fall of 2~4 DEG C/min, and in 780 DEG C of 35~120min of heat preservation；
9) furnace temperature is down to 500 DEG C according to the rate of temperature fall of 3~5 DEG C/min, and in 500 DEG C of 10~30min of heat preservation；
10) furnace temperature is down to room temperature up to red copper star scintillation glass according to the rate of temperature fall of 10~15 DEG C/min.
Iron content is less than 100ppm in the quartz sand, and granularity is 100 mesh.
The granularity of the cuprous oxide, iron powder, stannous oxide, aluminium powder is greater than 200 mesh.
The method that the present invention uses multilevel reduction agent to be used in mixed way, avoids traditional preparation methods, specimen surface oxide layer The disadvantages such as blocked up, sample section Venus is uneven, and product utilization is low, and production efficiency is low.Meanwhile this method is using step by step cooling down Crystallization process, thoroughly solves that color difference is big in the crystallization process that heated up after the cooling of traditional aventurine glass again and grain growth is uneven Even disadvantage.Copper star source is added using multiple, has fully ensured that the formation of sample intermediate cam shape copper simple substance, has shown star excellent effect. The color method of the application is conducive to large-scale production, and the preparation process time is short, high efficiency, and the aobvious star effect of sample is good, and color is equal It is even.Prepared red copper star scintillation glass can be used as the ornament materials of high-grade glass, ceramics, metal etc., decorative effect pole It is good.
Specific embodiment
Embodiment 1:
1) quartz sand 55%, sodium carbonate 18%, potassium carbonate 1%, Pb are taken by mass fraction3O47%, borax 8%, sodium nitrate 3%, cuprous oxide 3%, iron powder 3%, stannous oxide 1.3%, aluminium powder 0.5%, fluorite 0.2%；
2) sodium carbonate and cuprous oxide are uniformly mixed, and take out after the mixture 30% is used as and adds mixture；
3) the remaining mixture of step 2) and other surplus stocks are uniformly mixed, and by 30 mesh standard sieves, are formed Batch；
4) batch addition has been warming up in 1350 DEG C of silica crucible, after keeping the temperature 30min, step 2) has been taken out It is primary that stirring in crucible is added in the half of mixture；
5) after keeping the temperature 30min again, remaining mixture is added again in crucible and is stirred primary；
6) furnace temperature is down to 1330 DEG C, keeps the temperature 120min；
7) furnace temperature is down to 950 DEG C according to the rate of temperature fall of 8 DEG C/min, keeps the temperature 5min；
8) furnace temperature is down to 780 DEG C according to the rate of temperature fall of 4 DEG C/min, and in 780 DEG C of heat preservation 120min；
9) furnace temperature is down to 500 DEG C according to the rate of temperature fall of 5 DEG C/min, and in 500 DEG C of heat preservation 30min；
10) furnace temperature is down to room temperature up to red copper star scintillation glass according to the rate of temperature fall of 10 DEG C/min.
Embodiment 2:
1) quartz sand 65%, sodium carbonate 12%, potassium carbonate 2%, Pb are taken by mass fraction3O46%, borax 3%, sodium nitrate 0.5%, cuprous oxide 7%, iron powder 1%, stannous oxide 2.5%, aluminium powder 0.1%, fluorite 0.9%；
2) sodium carbonate and cuprous oxide are uniformly mixed, and take out after the mixture 30% is used as and adds mixture；
3) the remaining mixture of step 2) and other surplus stocks are uniformly mixed, and by 30 mesh standard sieves, are formed Batch；
4) batch addition has been warming up in 1450 DEG C of silica crucible, after keeping the temperature 30min, step 2) has been taken out It is primary that stirring in crucible is added in the half of mixture；
5) after keeping the temperature 30min again, remaining mixture is added again in crucible and is stirred primary；
6) furnace temperature is down to 1430 DEG C, keeps the temperature 30min；
7) furnace temperature is down to 950 DEG C according to the rate of temperature fall of 10 DEG C/min, keeps the temperature 10min；
8) furnace temperature is down to 780 DEG C according to the rate of temperature fall of 2 DEG C/min, and in 780 DEG C of heat preservation 35min；
9) furnace temperature is down to 500 DEG C according to the rate of temperature fall of 3 DEG C/min, and in 500 DEG C of heat preservation 10min；
10) furnace temperature is down to room temperature up to red copper star scintillation glass according to the rate of temperature fall of 15 DEG C/min.
Embodiment 3:
1) quartz sand 57%, sodium carbonate 13%, potassium carbonate 2%, Pb are taken by mass fraction3O46%, borax 4%, sodium nitrate 2.8%, cuprous oxide 3%, iron powder 4%, stannous oxide 3%, aluminium powder 0.2%, fluorite 5%；
2) sodium carbonate and cuprous oxide are uniformly mixed, and take out after the mixture 30% is used as and adds mixture；
3) the remaining mixture of step 2) and other surplus stocks are uniformly mixed, and by 30 mesh standard sieves, are formed Batch；
4) batch addition has been warming up in 1400 DEG C of silica crucible, after keeping the temperature 30min, step 2) has been taken out It is primary that stirring in crucible is added in the half of mixture；
5) after keeping the temperature 30min again, remaining mixture is added again in crucible and is stirred primary；
6) furnace temperature is down to 1380 DEG C, keeps the temperature 75min；
7) furnace temperature is down to 950 DEG C according to the rate of temperature fall of 9 DEG C/min, keeps the temperature 7min；
8) furnace temperature is down to 780 DEG C according to the rate of temperature fall of 3 DEG C/min, and in 780 DEG C of heat preservation 75min；
9) furnace temperature is down to 500 DEG C according to the rate of temperature fall of 4 DEG C/min, and in 500 DEG C of heat preservation 20min；
10) furnace temperature is down to room temperature up to red copper star scintillation glass according to the rate of temperature fall of 12 DEG C/min.
Embodiment 4:
1) quartz sand 62%, sodium carbonate 12%, potassium carbonate 3%, Pb are taken by mass fraction3O48%, borax 6%, sodium nitrate 1%, cuprous oxide 4%, iron powder 1.7%, stannous oxide 1%, aluminium powder 0.3%, fluorite 1%；
2) sodium carbonate and cuprous oxide are uniformly mixed, and take out after the mixture 30% is used as and adds mixture；
3) the remaining mixture of step 2) and other surplus stocks are uniformly mixed, and by 30 mesh standard sieves, are formed Batch；
4) batch addition has been warming up in 1380 DEG C of silica crucible, after keeping the temperature 30min, step 2) has been taken out It is primary that stirring in crucible is added in the half of mixture；
5) after keeping the temperature 30min again, remaining mixture is added again in crucible and is stirred primary；
6) furnace temperature is down to 1350 DEG C, keeps the temperature 60min；
7) furnace temperature is down to 950 DEG C according to the rate of temperature fall of 8.5 DEG C/min, keeps the temperature 9min；
8) furnace temperature is down to 780 DEG C according to the rate of temperature fall of 3.5 DEG C/min, and in 780 DEG C of heat preservation 60min；
9) furnace temperature is down to 500 DEG C according to the rate of temperature fall of 5 DEG C/min, and in 500 DEG C of heat preservation 25min；
10) furnace temperature is down to room temperature up to red copper star scintillation glass according to the rate of temperature fall of 13 DEG C/min.
Embodiment 5:
1) quartz sand 56%, sodium carbonate 13%, potassium carbonate 1%, Pb are taken by mass fraction3O410%, borax 9%, sodium nitrate 1.6%, cuprous oxide 3%, iron powder 2%, stannous oxide 2%, aluminium powder 0.4%, fluorite 2%；
2) sodium carbonate and cuprous oxide are uniformly mixed, and take out after the mixture 30% is used as and adds mixture；
3) the remaining mixture of step 2) and other surplus stocks are uniformly mixed, and by 30 mesh standard sieves, are formed Batch；
4) batch addition has been warming up in 1430 DEG C of silica crucible, after keeping the temperature 30min, step 2) has been taken out It is primary that stirring in crucible is added in the half of mixture；
5) after keeping the temperature 30min again, remaining mixture is added again in crucible and is stirred primary；
6) furnace temperature is down to 1400 DEG C, keeps the temperature 70min；
7) furnace temperature is down to 950 DEG C according to the rate of temperature fall of 9 DEG C/min, keeps the temperature 6min；
8) furnace temperature is down to 780 DEG C according to the rate of temperature fall of 4 DEG C/min, and in 780 DEG C of heat preservation 80min；
9) furnace temperature is down to 500 DEG C according to the rate of temperature fall of 3 DEG C/min, and in 500 DEG C of heat preservation 12min；
10) furnace temperature is down to room temperature up to red copper star scintillation glass according to the rate of temperature fall of 11 DEG C/min.
Embodiment 6:
1) quartz sand 55%, sodium carbonate 14%, potassium carbonate 5%, Pb are taken by mass fraction3O48%, borax 7%, sodium nitrate 0.5%, cuprous oxide 5%, iron powder 1.2%, stannous oxide 1%, aluminium powder 0.3%, fluorite 3%；
2) sodium carbonate and cuprous oxide are uniformly mixed, and take out after the mixture 30% is used as and adds mixture；
3) the remaining mixture of step 2) and other surplus stocks are uniformly mixed, and by 30 mesh standard sieves, are formed Batch；
4) batch addition has been warming up in 1410 DEG C of silica crucible, after keeping the temperature 30min, step 2) has been taken out It is primary that stirring in crucible is added in the half of mixture；
5) after keeping the temperature 30min again, remaining mixture is added again in crucible and is stirred primary；
6) furnace temperature is down to 1370 DEG C, keeps the temperature 100min；
7) furnace temperature is down to 950 DEG C according to the rate of temperature fall of 10 DEG C/min, keeps the temperature 9min；
8) furnace temperature is down to 780 DEG C according to the rate of temperature fall of 3 DEG C/min, and in 780 DEG C of heat preservation 95min；
9) furnace temperature is down to 500 DEG C according to the rate of temperature fall of 4 DEG C/min, and in 500 DEG C of heat preservation 17min；
10) furnace temperature is down to room temperature up to red copper star scintillation glass according to the rate of temperature fall of 14 DEG C/min.
The method that the present invention uses multilevel reduction agent to be used in mixed way, avoids traditional preparation methods, specimen surface oxide layer The disadvantages such as blocked up, sample section Venus is uneven, and product utilization is low, and production efficiency is low.Meanwhile this method is using step by step cooling down Crystallization process, thoroughly solves that color difference is big in the crystallization process that heated up after the cooling of traditional aventurine glass again and grain growth is uneven Even disadvantage.Copper star source is added using multiple, has fully ensured that the formation of sample intermediate cam shape copper simple substance, has shown star excellent effect. The color method of the application is conducive to large-scale production, and the preparation process time is short, high efficiency, and the aobvious star effect of sample is good, and color is equal It is even.Prepared red copper star scintillation glass can be used as the ornament materials of high-grade glass, ceramics, metal etc., decorative effect pole It is good.

Claims (3)

1. a kind of preparation method of red copper star scintillation glass, it is characterised in that:
1) quartz sand 55~65%, sodium carbonate 12~18%, potassium carbonate 1~5%, Pb are taken by mass fraction3O46~10%, boron Sand 3~9%, sodium nitrate 0.5~3%, cuprous oxide 3~7%, iron powder 1~4%, stannous oxide 1~3%, aluminium powder 0.1~ 0.5%, fluorite 0.2~5%；
2) sodium carbonate and cuprous oxide are uniformly mixed, and take out after mixture 30% is used as and adds mixture；
3) the remaining mixture of step 2) and other surplus stocks are uniformly mixed, and by 30 mesh standard sieves, form cooperation Material；
4) batch addition has been warming up in 1350~1450 DEG C of silica crucible, after keeping the temperature 30min, step 2) has been taken out The half of mixture that stirring in crucible is added is primary；
5) after keeping the temperature 30min again, remaining mixture is added again in crucible and is stirred primary；
6) furnace temperature is down to 1330~1430 DEG C, keeps the temperature 30~120min；
7) furnace temperature is down to 950 DEG C according to the rate of temperature fall of 8~10 DEG C/min, keeps the temperature 5~10min；
8) furnace temperature is down to 780 DEG C according to the rate of temperature fall of 2~4 DEG C/min, and in 780 DEG C of 35~120min of heat preservation；
9) furnace temperature is down to 500 DEG C according to the rate of temperature fall of 3~5 DEG C/min, and in 500 DEG C of 10~30min of heat preservation；
10) furnace temperature is down to room temperature up to red copper star scintillation glass according to the rate of temperature fall of 10~15 DEG C/min.
2. a kind of preparation method of red copper star scintillation glass according to claim 1, it is characterised in that: the quartz sand Middle iron content is less than 100ppm, and granularity is 100 mesh.
3. a kind of preparation method of red copper star scintillation glass according to claim 1, it is characterised in that: the oxidation is sub- The granularity of copper, iron powder, stannous oxide, aluminium powder is greater than 200 mesh.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4816687B1 (en) * 1969-08-09 1973-05-24
JPS4822971B1 (en) * 1968-06-18 1973-07-10
SU1452802A1 (en) * 1987-06-24 1989-01-23 Московский химико-технологический институт им.Д.И.Менделеева Avanturine glass
CN102249539A (en) * 2011-04-19 2011-11-23 武汉理工大学 Method for preparing aventurine fluoride-free opal glass

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4822971B1 (en) * 1968-06-18 1973-07-10
JPS4816687B1 (en) * 1969-08-09 1973-05-24
SU1452802A1 (en) * 1987-06-24 1989-01-23 Московский химико-технологический институт им.Д.И.Менделеева Avanturine glass
CN102249539A (en) * 2011-04-19 2011-11-23 武汉理工大学 Method for preparing aventurine fluoride-free opal glass

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
艺术玻璃和装饰玻璃(七) ———金星玻璃;王承遇等;《玻璃与搪瓷》;20080429;第36卷(第2期);第48页表8、第3段

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