CN108483923A - A kind of preparation method of blue glass ceramics new material - Google Patents

A kind of preparation method of blue glass ceramics new material Download PDF

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Publication number
CN108483923A
CN108483923A CN201810322199.8A CN201810322199A CN108483923A CN 108483923 A CN108483923 A CN 108483923A CN 201810322199 A CN201810322199 A CN 201810322199A CN 108483923 A CN108483923 A CN 108483923A
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China
Prior art keywords
crystallization
temperature
minutes
kiln
minute
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CN201810322199.8A
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Chinese (zh)
Inventor
秦刚
秦小平
徐国梁
楼贤春
姜小元
王刚琳
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SICHUAN YIMING MICROCRYSTALLINE TECHNOLOGY Co Ltd
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SICHUAN YIMING MICROCRYSTALLINE TECHNOLOGY Co Ltd
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Priority to CN201810322199.8A priority Critical patent/CN108483923A/en
Publication of CN108483923A publication Critical patent/CN108483923A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified 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
    • C03C10/0063Devitrified 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 waste materials, e.g. slags
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B1/00Preparing the batches
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B13/00Rolling molten glass, i.e. where the molten glass is shaped by rolling
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/02Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/16Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified 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
    • C03C10/0018Devitrified 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 monovalent metal oxide as main constituents
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

Abstract

The invention discloses a kind of preparation methods of blue glass ceramics new material, include the following steps:Step 1: raw material selects;Step 2: raw material mixes;Step 3: the fusing of mixture;Step 4: calendaring molding;Step 5: annealing;Step 6: crystallization.The present invention is arranged by the way that copper oxide and corresponding system is added, it can make final devitrified glass product that blue be presented, and compression strength and bending strength are superior to Ordinary microcrystalline glass board material, the present invention also has energy-saving, raising plank yield rate, while reducing production cost, granite waste is utilized again.

Description

A kind of preparation method of blue glass ceramics new material
Technical field
The present invention relates to a kind of preparation methods of devitrified glass, and in particular to a kind of preparation of blue glass ceramics new material Method.
Background technology
The basic performance of the existing glass of devitrified glass, and with the polycrystalline feature of ceramics, concentrated the spy of glass and ceramics Point becomes a kind of unique new material.With its high mechanical strength, hardness is big, wear-resisting property is good, corrosion resistance is strong, has good Good chemical stability and thermal stability, adapts to rugged environment, has obtained quick development in the world in recent years.
Existing formula can not produce blue glass ceramics, to diversify, expand the scale of production, and meet different Gus Objective demand further increases occupation rate of market, and then realizes the combination of economic benefit and technological innovation.Just there is exploitation The plan of " blue glass ceramics " project, and find that its performance is better than Ordinary microcrystalline glass after actual production goes out blue glass ceramics Glass plate material.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of blue glass ceramics new material.
The invention is realized in this way:
A kind of preparation method of blue glass ceramics new material, includes the following steps:
Step 1: raw material selects
Raw material is selected according to following weight ratio:
Wherein, using discarded granite as primary raw material, granite (provides Al2O3), quartz sand (provide SiO2), magnesia unslacked (providing MgO), potassium carbonate (provide K2O), prodan (providing F), sodium carbonate (provide Na2O), copper oxide (provide CuO), again Calcium (providing CaO) can be purchased on periphery, and chemical composition is relatively stable, and production cost is relatively low.
Step 2: raw material mixes
It is mixed after being sent to mixing machine after above-mentioned raw materials are weighed well in proportion, and the water for accounting for raw material gross weight 2% is added, mixed Conjunction 3~after five minutes, it send to All Electric Melting Furnace feeding chamber.
Step 3: the fusing of mixture
(1) it feeds:It is fed using automatic charging equipment, is controlled and fed by blue outside line liquid level indicator.
(2) fusing of mixture is carried out using All Electric Melting Furnace
All Electric Melting Furnace is divided into main melting tank, dog-hole, increased channel and several parts of material path, the fusing (fusion temperature of mixture 1350 DEG C~1450 DEG C), 8 hours or so (1300~1350 DEG C of the clarification and homogenization temperature) time of clarification and homogenization, in main molten Change pond to carry out, clarification, the glass being homogenized enter material path through dog-hole, increased channel, and temperature is controlled at 1250 DEG C~1300 DEG C, warp After material path cooling, calendaring molding (1150 DEG C~1200 DEG C of forming temperature) is carried out into calender.
Step 4: calendaring molding
Every production line uses two table glass calender (the using and the reserved) calendaring moldings, and plate thickness, width can be according to lifes Production requires to be adjusted, and the communicated roller of glass tape of forming enters annealing kiln annealing.
Step 5: annealing
Glass tape enter annealing kiln temperature be 650~750 DEG C, at 680~750 DEG C keep the temperature 10~after twenty minutes, by 3 DEG C/ Divide~5 DEG C/minute of speed to be cooled to 580~620 DEG C, then 300 DEG C are cooled to by 7 DEG C/minute~12 DEG C/minute of speed, using 40 DEG C of kiln discharges are cooled within 40~60 minutes, subsequently into cold end cutting action.Cold end cutting action is wanted by sets requirement or client The length asked cuts glass tape, forms semi-finished product (annealed sheet) after cutting, is sent to crystallization kiln crystallization through transition roller table.
Step 6: crystallization
The qualified annealed sheet of detection enters crystallization kiln, and 600 DEG C~720 DEG C were warming up to through 30~90 minutes, 600 DEG C~ 720 DEG C of heat preservations coring in 30~90 minutes, had been warming up to 820 DEG C~920 DEG C through 30~90 minutes, 30 is kept the temperature at 820 DEG C~920 DEG C ~120 minutes crystallization were cooled to 40 DEG C of kiln discharges through 60~120 minutes, complete crystallization process.As hair plates (crystallization plate), send to Mill cuts workshop finishing.
Step 7: grinding and polishing
Detection qualified crystallization plate such as is polished through ZDML-16 full-automatic mills, is polished at the surfaces processing, and then storage is protected It deposits.
It should be further noted that after using composition of raw materials provided by the invention, finally to ensure in formula Main component meet following table formula design:
The invention has the advantages that:
1, product colour is that (addition copper oxide only just will present blue in this system cannot after system changes for blue Blue is presented), 350~400MPa of compression strength (is better than common 200~300Mpa of plank), 80~100MPa of bending strength (being better than common 40~80Mpa of plank) (after plank is by crystallization, forms two kinds of indenting crystalline phases, such as A crystalline phases in laterally Growth, B crystalline phases are in longitudinal growth, therefore it is with good mechanical performance), blue glass ceramics have the microcosmic of indenting shape Structure makes it have higher mechanical strength.
2, glass melting temperature (1350 DEG C~1450 DEG C), blue glass ceramics have lower glass melting temperature, general that temperature is melted Between degree is 1550 DEG C~1580 DEG C, energy consumption is saved.
3, blue glass ceramics have lower recrystallization temperature, so that it is not easy crystallization in forming temperature scope, are molded Plank flatness is high in journey, is conducive to improve plank yield rate.
4, blue glass ceramics have filled up the market vacancy.
5, granite solid waste is handled to a certain extent, and granite dosage accounts for 40% or so in formula, can provide The required alkali metal oxide of glass melting and glass skeleton structure, while reducing production cost, granite waste obtains To utilizing again.
Specific implementation mode
With reference to specific embodiment, the present invention is further illustrated.
Embodiment one
1, by following raw material precises, it is sent into batch mixer mixing (incorporation time 4 minutes)
2, above-mentioned mixture is sent into All Electric Melting Furnace fusing, 1400 DEG C of fusion temperature, the glass melted is clarified and equal After change, material path is entered by dog-hole, increased channel, temperature is down to 1300 DEG C, enters back into calendering work pool, is rolled into through calender Shape (1150 DEG C of forming temperature) enters annealing kiln afterwards.
3, the glass board material annealing kiln after rolling is annealed, and is 700 DEG C into kiln temperature degree, is cooled to by 3 DEG C/minute of speed 540 DEG C, then 300 DEG C are cooled to by 9 DEG C/minute of speed, 40 DEG C of kiln discharges were cooled to using 60 minutes, are cut subsequently into cold end Line.Cold end cutting line cuts glass tape by the length of sets requirement or customer requirement, and semi-finished product (annealed sheet), warp are generated after cutting Transition roller table is sent to crystallization kiln crystallization.
4, the qualified annealed sheet of detection enters crystallization kiln, was warming up to 710 DEG C through 60 minutes, 30 minutes core is kept the temperature at 710 DEG C Change, be warming up to 880 DEG C through 45 minutes, 45 minutes crystallization are kept the temperature at 880 DEG C, 40 DEG C of kiln discharges were cooled to through 120 minutes, completes brilliant Change process.As hair plates (crystallization plate), send to mill and cut workshop finishing.
In the present embodiment, end formulation composition detection such as following table:
Embodiment two
1, by following raw material precises, it is sent into batch mixer mixing (incorporation time 4 minutes).
2, above-mentioned mixture is sent into All Electric Melting Furnace fusing, 1400 DEG C of fusion temperature, the glass melted is clarified and equal After change, material path is entered by dog-hole, increased channel, temperature is down to 1300 DEG C, enters back into calendering work pool, is rolled into through calender Shape (1150 DEG C of forming temperature) enters annealing kiln afterwards.
3, the glass board material annealing kiln after rolling is annealed, and is 700 DEG C into kiln temperature degree, is cooled to by 3 DEG C/minute of speed 540 DEG C, then 300 DEG C are cooled to by 9 DEG C/minute of speed, 40 DEG C of kiln discharges were cooled to using 60 minutes, are cut subsequently into cold end Line.Cold end cutting line cuts glass tape by the length of sets requirement or customer requirement, and semi-finished product (annealed sheet), warp are generated after cutting Transition roller table is sent to crystallization kiln crystallization.
4, the qualified annealed sheet of detection enters crystallization kiln, was warming up to 680 DEG C through 60 minutes, 60 minutes core is kept the temperature at 680 DEG C Change, be warming up to 900 DEG C through 60 minutes, 60 minutes crystallization are kept the temperature at 880 DEG C, 40 DEG C of kiln discharges were cooled to through 120 minutes, completes brilliant Change process.As hair plates (crystallization plate), send to mill and cut workshop finishing.
In the present embodiment, end formulation composition detection such as following table:
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that people in the art Member can be designed that a lot of other modification and implementations, these modifications and implementations will be fallen in principle disclosed in the present application Within scope and spirit.

Claims (4)

1. a kind of preparation method of blue glass ceramics new material, it is characterised in that include the following steps:
Step 1: raw material selects
Raw material is selected according to following weight ratio:
Step 2: raw material mixes
It is mixed after being sent to mixing machine after above-mentioned raw materials are weighed well in proportion, and the water for accounting for raw material gross weight 2% is added, mixing 3 ~after five minutes, it send to All Electric Melting Furnace feeding chamber;
Step 3: the fusing of mixture
(1) it feeds:It is fed using automatic charging equipment, is controlled and fed by blue outside line liquid level indicator;
(2) fusing of mixture is carried out using All Electric Melting Furnace
All Electric Melting Furnace is divided into main melting tank, dog-hole, increased channel and several parts of material path, when the fusing of mixture, clarification and homogenization Between 8 hours or so, carried out in main melting tank, clarification, the glass that has been homogenized enter material path, temperature control through dog-hole, increased channel System is at 1250 DEG C~1300 DEG C, and after material path cools down, calendaring molding, forming temperature 1150 DEG C~1200 are carried out into calender ℃;
Step 4: calendaring molding
Every production line uses two table glass calender calendaring moldings, plate thickness, width to be adjusted according to production requirement, at The communicated roller of glass tape of shape enters annealing kiln annealing;
Step 5: annealing
Glass tape enter annealing kiln temperature be 650~750 DEG C, at 680~750 DEG C keep the temperature 10~after twenty minutes, by 3 DEG C/minute~5 DEG C/minute speed be cooled to 580~620 DEG C, then 300 DEG C are cooled to by 7 DEG C/minute~12 DEG C/minute of speed, using 40~60 Minute is cooled to 40 DEG C of kiln discharges, subsequently into cold end cutting action;Cold end cutting action is by sets requirement or the length of customer requirement Degree cuts glass tape, forms semi-finished product annealed sheet after cutting, is sent to crystallization kiln crystallization through transition roller table;
Step 6: crystallization
The qualified annealed sheet of detection enters crystallization kiln, 600 DEG C~720 DEG C is warming up to through 30~90 minutes, at 600 DEG C~720 DEG C Coring in 30~90 minutes is kept the temperature, 820 DEG C~920 DEG C had been warming up to through 30~90 minutes, 30~120 are kept the temperature at 820 DEG C~920 DEG C Minute crystallization was cooled to 40 DEG C of kiln discharges through 60~120 minutes, completes crystallization process, become crystallization plate.
2. the preparation method of blue glass ceramics new material according to claim 1, it is characterised in that:
In step 1, after raw material selection, finally to ensure that the main component in formula meets the formula design of following table:
3. the preparation method of blue glass ceramics new material according to claim 1 or claim 2, it is characterised in that:
In the main melting tank of All Electric Melting Furnace, 1350 DEG C~1450 DEG C of the fusion temperature of mixture, clarification and homogenization temperature 1300~ 1350℃。
4. the preparation method of blue glass ceramics new material according to claim 1 or claim 2, it is characterised in that:
In step 6, become crystallization plate after the completion of crystallization, is polished through ZDML-16 full-automatic mills, polished surface processing, so Storage preserves afterwards.
CN201810322199.8A 2018-04-11 2018-04-11 A kind of preparation method of blue glass ceramics new material Pending CN108483923A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116119929A (en) * 2022-11-22 2023-05-16 安徽火凤凰新材料科技有限公司 Colored microcrystalline glass and preparation method and application thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1072398A (en) * 1992-09-28 1993-05-26 唐山市古冶玻璃制品厂 Nucleated glass granite dalle and production technique
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
CN102942303A (en) * 2012-10-29 2013-02-27 中国科学院过程工程研究所 High-strength wear-resistant engineering microcrystalline glass prepared by using granite waste materials and preparation method thereof
CN103496851A (en) * 2013-09-25 2014-01-08 四川一名微晶科技股份有限公司 Black microcrystalline glass sheet material and production method thereof
CN104045237A (en) * 2014-06-30 2014-09-17 四川一名微晶科技股份有限公司 Red microcrystalline glass plate and production method thereof
CN106810079A (en) * 2016-12-23 2017-06-09 四川名微晶科技股份有限公司 The method that mica glass ceramic is prepared using granite waste residues

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1072398A (en) * 1992-09-28 1993-05-26 唐山市古冶玻璃制品厂 Nucleated glass granite dalle and production technique
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
CN102942303A (en) * 2012-10-29 2013-02-27 中国科学院过程工程研究所 High-strength wear-resistant engineering microcrystalline glass prepared by using granite waste materials and preparation method thereof
CN103496851A (en) * 2013-09-25 2014-01-08 四川一名微晶科技股份有限公司 Black microcrystalline glass sheet material and production method thereof
CN104045237A (en) * 2014-06-30 2014-09-17 四川一名微晶科技股份有限公司 Red microcrystalline glass plate and production method thereof
CN106810079A (en) * 2016-12-23 2017-06-09 四川名微晶科技股份有限公司 The method that mica glass ceramic is prepared using granite waste residues

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116119929A (en) * 2022-11-22 2023-05-16 安徽火凤凰新材料科技有限公司 Colored microcrystalline glass and preparation method and application thereof

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