CN103496850A - Black microcrystalline glass sheet material and production method thereof - Google Patents

Black microcrystalline glass sheet material and production method thereof Download PDF

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Publication number
CN103496850A
CN103496850A CN201310441663.2A CN201310441663A CN103496850A CN 103496850 A CN103496850 A CN 103496850A CN 201310441663 A CN201310441663 A CN 201310441663A CN 103496850 A CN103496850 A CN 103496850A
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glass
glass sheet
microcrystalline glass
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CN103496850B (en
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秦刚
秦小平
姜小元
王刚琳
王桃
徐国梁
熊冰峰
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SICHUAN YIMING MICROCRYSTALLINE TECHNOLOGY Co Ltd
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SICHUAN YIMING MICROCRYSTALLINE TECHNOLOGY Co Ltd
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Abstract

The invention discloses a black microcrystalline glass sheet material and a production method thereof. The black microcrystalline glass sheet material contains the following ingredients in parts by weight: 2-4 parts of Na2O, 6-10 parts of MgO, 8-13 parts of Al2O3, 55-65 parts of SiO2, 0.5-2 parts of P2O5, 3-4 parts of K2O, 4-8 parts of CaO, 5-10 parts of Fe2O3 and 1.5-2.5 parts of TiO2. The production method comprises the steps of mixing 9-20 parts by weight of magnesite, 30-50 parts by weight of granite, 0.5-3 parts by weight of calcium dihydrogen phosphate, 1-8 parts by weight of heavy calcium carbonate and 30-70 parts by weight of basalt and then producing by adopting all-electric melting calendering. According to the black microcrystalline glass sheet material and the production method thereof, through the long-term research on the proportioning ratio of microcrystalline glass sheet materials, a formula for the black microcrystalline glass sheet material is obtained, and the production method of the black microcrystalline glass sheet material is also obtained; the situation that the existing microcrystalline glass sheet materials are single in color is broken through; basalt waste residues and granite are taken as main raw materials, the basalt waste residues contain a large amount of iron and titanium, titanium can serve as a crystal nucleating agent, the content of P2O5 can be reduced, and iron oxide red is not required to be added into the raw materials; the raw materials are all easily obtained and are low in cost.

Description

Black micro-crystal glass plate and production method thereof
Technical field
The present invention relates to a kind of material of construction and production method thereof, be specifically related to a kind of black micro-crystal glass plate and production method thereof.
Background technology
The fundamental property of the existing glass of devitrified glass, have again ceramic polycrystalline feature, concentrated glass and ceramic characteristics, becomes the type material of a class uniqueness.High with its physical strength, hardness is large, wear resisting property good, erosion resistance is strong, has good chemical stability and thermostability, can adapt to rugged environment, has obtained in the world in recent years fast development." the 12 new material industry development program " that particularly in January, 2012, Ministry of Industry and Information of country announced, list the calendering devitrified glass in give priority to new inorganic non-metallic materials catalogue, to rolling from now on devitrified glass, in the application of basic field of new, great importance is arranged.
The production of tradition devitrified glass adopts sintering process technique more, and the high problem of the energy consumption that sintering process technique faces in devitrified glass production is the critical bottleneck of the fast development of restriction devitrified glass and large-scale production always.Sintering process explained hereafter devitrified glass and will use expensive non-ferrous metal zinc oxide starting material, make the production cost of a lot of devitrified glass enterprise always high, sintering process production technique efficiency is low simultaneously, and product has pore, planeness devitrified glass enterprise management condition poor, sintering process technique always to have difficulty in taking a step.The pioneering all-electric melting rolling process in the company whole nation is produced the devitrified glass novel process and has been obtained national inventing patent (patent name: utilize granite waste to produce the method for microcrystalline glass decorative plate, the patent No.: ZL200910216248.0), filled up domestic blank.Adopt the all-electric melting calendering to produce devitrified glass, the energy consumption of unit product of devitrified glass and ten thousand yuan of industrial added value energy consumptions, by decrease, can also be saved a large amount of non-ferrous metal zinc oxide precious materials for country.The invention of present technique, complied with the development trend of China's new material industry and the constantly requirement in broadened application field.
Utilize at present discarded granite to adopt all-electric melting rolling process explained hereafter to go out beige, coffee-like serial crystallizing glass sheet material, but beige, coffee-like crystallizing glass sheet material are difficult to the demand of satisfying the market to many kinds, multi-color devitrified glass, therefore need constantly formula and the production technique of the devitrified glass of the different patterns of research.
Summary of the invention
The purpose of this invention is to provide a kind of black micro-crystal glass plate and production method thereof, to meet the demand of multi-color devitrified glass.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
A kind of black micro-crystal glass plate comprises the component of following weight part:
Na 2o:2~4 part; MgO:6~10 part; Al 2o 3: 8~13 parts; SiO 2: 55~65 parts; P 2o 5: 0.5~2 part; K 2o:2~~5 part; CaO:4~8 part; Fe 2o 3: 5~10 parts; TiO 2: 1.5~2.5 parts.
The production method of described black micro-crystal glass plate comprises the following steps:
Step 1: according to following weight parts, choose starting material: 9~20 parts, magnesite, 30~50 parts, grouan, 0.5~3 part of monocalcium phosphate, 1~8 part of coarse whiting, 30~70 parts, basalt;
Step 2: above-mentioned starting material are mixed, and add the water of starting material gross weight 2%, mix 3~5min, compound is sent into to the melting pool of All Electric Melting Furnace, the controlled melting temperature is 1350~1500 ℃; Glass after fusing carries out clarification and homogenization, and the temperature of clarification and homogenization is 1400~1450 ℃, and the time of clarification and homogenization is 7~8h;
Step 3: the glass will clarify, homogenizing is good enters the material road through dog-hole, uptake, and temperature enters rolling press and is molded into glass ribbon after reducing to 1250~1300 ℃ of ,Jing Liao road coolings, and mold temperature is 1150~1250 ℃;
Step 4: the glass ribbon after moulding carries out anneal, it is 650~800 ℃ that glass is brought the kiln temperature degree into, 680~750 ℃ the insulation 10~20 minutes after, speed by 3 ℃/minutes~5 ℃/minutes is cooled to 580~620 ℃, be cooled to 300 ℃ by the speed of 7 ℃/minutes~12 ℃/minutes again, be cooled to 35~45 ℃ through 40~60 minutes again, kiln discharge, cut rear generation annealed sheet;
Step 5: annealed sheet is sent into to crystallization kiln carries out coring, crystallization becomes the crystallization plate, be specially: be warming up to 600 ℃~720 ℃ through 30~90 minutes, in 600 ℃~720 ℃ insulations coring in 30~90 minutes, be warming up to 820 ℃~930 ℃ through 30~90 minutes again, in 30~120 minutes crystallization of 820 ℃~930 ℃ insulations, be cooled to 35~45 ℃ of kiln discharges through 60~120 minutes;
Step 6: by the crystallization plate polished, polishing.
The present invention compared with prior art, has following beneficial effect:
(1) the present invention, through the proportioning of the crystallizing glass sheet material that studies for a long period of time, has obtained the formula of black micro-crystal glass plate, and has obtained producing the production method of this black micro-crystal glass plate, has broken through the single situation of existing crystallizing glass sheet material color.
(2) produce black micro-crystal glass plate and take basalt waste residue, grouan and provide MgO as main raw material, magnesite, monocalcium phosphate provides P 2o 5and CaO, coarse whiting provides CaO, contains a large amount of ferro elements and titanium elements in the basalt waste residue, and titanium can be used as Nucleating Agent, can reduce P 2o 5amount, in starting material without adding iron oxide red; Starting material all are easy to get, and cost is low.
(3) the product ultimate compression strength 200-300MPa that the present invention produces, bending strength 40-80MPa, density 2.6-2.7g/cm3, Mohs' hardness 5-6 level, water-intake rate<0.01%, smooth finish 90-98, acidproof soda acid, radioassay meets national category-A examination criteria.
Embodiment
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
According to one embodiment of present invention, the production method of black glass ceramic comprises the following steps:
1, choose starting material according to following weight parts, send into mixer and mix, mixing time is 4min, adds water 10Kg.
Material name Magnesite Granite Monocalcium phosphate Coarse whiting Basalt
Weight (Kg) 70 190 2.4 7.6 230
Table 1: raw-material Chemical Composition (weight percent)
Figure BDA0000387569290000041
2, above-mentioned compound is sent in the melting pool of All Electric Melting Furnace, the controlled melting temperature is 1350 ℃, and the glass after fusing carries out clarification and homogenization, and the temperature of clarification and homogenization is 1400 ℃, and the time of clarification and homogenization is 8h.
3, the glass will clarify, homogenizing is good enters the material road through dog-hole, uptake, and temperature enters rolling press and is molded into glass ribbon after reducing to 1280 ℃ of ,Jing Liao road coolings, and mold temperature is 1150 ℃; The thickness of formed glass band, width are regulated according to the requirement of producing sheet.
4, the glass ribbon after moulding enters annealing furnace through the transfer roller platform and carries out anneal, it is 700 ℃ that glass is brought the kiln temperature degree into, 680 ℃ the insulation 15 minutes after, speed by 3 ℃/minutes is cooled to 580 ℃, again by 9 ℃/minute speed be cooled to 300 ℃, be cooled to 40 ℃ through 60 minutes again, kiln discharge, then enter the cold junction line of cut.The cold junction line of cut cuts glass ribbon by the length of setting requirement or customer requirement, cuts rear generation work in-process (annealed sheet), through transition roller table, delivers to nucleus crystallization in crystallization kiln.
5, annealed sheet is sent into to crystallization kiln carries out coring, crystallization becomes the crystallization plate, be specially: be warming up to 700 ℃ through 60 minutes, in 700 ℃ of insulations coring in 60 minutes, then be warming up to 900 ℃ through 45 minutes, in 100 minutes crystallization of 900 ℃ of insulations, be cooled to 40 ℃ of kiln discharges through 120 minutes.
6, the crystallization plate is polished, polishing.
The black glass ceramic of above-mentioned preparation is carried out to composition detection, and the result of composition detection is as shown in table 2.
The composition analysis of the black glass ceramic that table 2: embodiment 1 produces
Na 2O MgO Al 2O 3 SiO 2 P 2O 5 K 2O CaO TiO 2 MnO 2 Fe 2O 3
3.49 8.50 11.20 59.07 0.50 2.17 5.00 2.00 0.14 7.89
Embodiment 1:
According to one embodiment of present invention, the production method of black glass ceramic comprises the following steps:
1, choose starting material according to following weight parts, send into mixer and mix, mixing time is 4min, adds water 10Kg.
Material name Magnesite Granite Monocalcium phosphate Coarse whiting Basalt
Weight (Kg) 64 181 2.4 7.6 242
2, above-mentioned compound is sent in the melting pool of All Electric Melting Furnace, the controlled melting temperature is 1350 ℃, and the glass after fusing carries out clarification and homogenization, and the temperature of clarification and homogenization is 1400 ℃, and the time of clarification and homogenization is 8h.
3, the glass will clarify, homogenizing is good enters the material road through dog-hole, uptake, and temperature enters rolling press and is molded into glass ribbon after reducing to 1280 ℃ of ,Jing Liao road coolings, and mold temperature is 1150 ℃; The thickness of formed glass band, width are regulated according to the requirement of producing sheet.
4, the glass ribbon after moulding enters annealing furnace through the transfer roller platform and carries out anneal, it is 700 ℃ that glass is brought the kiln temperature degree into, 680 ℃ the insulation 15 minutes after, speed by 3 ℃/minutes is cooled to 580 ℃, again by 9 ℃/minute speed be cooled to 300 ℃, be cooled to 40 ℃ through 60 minutes again, kiln discharge, then enter the cold junction line of cut.The cold junction line of cut cuts glass ribbon by the length of setting requirement or customer requirement, cuts rear generation work in-process (annealed sheet), through transition roller table, delivers to nucleus crystallization in crystallization kiln.
5, annealed sheet is sent into to crystallization kiln carries out coring, crystallization becomes the crystallization plate, be specially: be warming up to 720 ℃ through 60 minutes, in 720 ℃ of insulations coring in 60 minutes, then be warming up to 930 ℃ through 60 minutes, in 100 minutes crystallization of 930 ℃ of insulations, be cooled to 40 ℃ of kiln discharges through 120 minutes.
6, the crystallization plate is polished, polishing.
The black glass ceramic of above-mentioned preparation is carried out to composition detection, and the result of composition detection is as shown in table 3.
The composition analysis of the black glass ceramic that table 3: embodiment 2 produces
Na 2O MgO Al 2O 3 SiO 2 P 2O 5 K 2O CaO TiO 2 MnO 2 Fe 2O 3
3.52 8.00 11.31 59.04 0.50 2.09 5.00 2.10 0.14 8.25
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only preferably embodiment of the present invention, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and within embodiment will drop on the disclosed principle scope and spirit of the application.

Claims (2)

1. a black micro-crystal glass plate is characterized in that comprising the component of following weight part:
Na 2o:2~4 part;
MgO:6~10 part;
Al 2o 3: 8~13 parts;
SiO 2: 55~65 parts;
P 2o 5: 0.5~2 part;
K 2o:2~5 part;
CaO:4~8 part;
Fe 2o 3: 5~10 parts;
TiO 2: 1.5~2.5 parts.
2. the production method of black micro-crystal glass plate claimed in claim 1 is characterized in that comprising the following steps:
Step 1: according to following weight parts, choose starting material: 9~20 parts, magnesite, 30~50 parts, grouan, 0.5~3 part of monocalcium phosphate, 1~8 part of coarse whiting, 30~70 parts, basalt;
Step 2: above-mentioned starting material are mixed, and add the water of starting material gross weight 2%, mix 3~5min, compound is sent into to the melting pool of All Electric Melting Furnace, the controlled melting temperature is 1350~1500 ℃; Glass after fusing carries out clarification and homogenization, and the temperature of clarification and homogenization is 1400~1450 ℃, and the time of clarification and homogenization is 7~8h;
Step 3: the glass will clarify, homogenizing is good enters the material road through dog-hole, uptake, and temperature enters rolling press and is molded into glass ribbon after reducing to 1250~1300 ℃ of ,Jing Liao road coolings, and mold temperature is 1150~1250 ℃;
Step 4: the glass ribbon after moulding carries out anneal, it is 650~800 ℃ that glass is brought the kiln temperature degree into, 680~750 ℃ the insulation 10~20 minutes after, speed by 3 ℃/minutes~5 ℃/minutes is cooled to 580~620 ℃, be cooled to 300 ℃ by the speed of 7 ℃/minutes~12 ℃/minutes again, be cooled to 35~45 ℃ through 40~60 minutes again, kiln discharge, cut rear generation annealed sheet;
Step 5: annealed sheet is sent into to crystallization kiln carries out coring, crystallization becomes the crystallization plate, be specially: be warming up to 600 ℃~720 ℃ through 30~90 minutes, in 600 ℃~720 ℃ insulations coring in 30~90 minutes, be warming up to 820 ℃~930 ℃ through 30~90 minutes again, in 30~120 minutes crystallization of 820 ℃~930 ℃ insulations, be cooled to 35~45 ℃ of kiln discharges through 60~120 minutes;
Step 6: by the crystallization plate polished, polishing.
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Cited By (12)

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CN103951188A (en) * 2014-04-22 2014-07-30 武汉理工大学 Black decorative glass taking gold-copper tailing as main raw material and preparation 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
CN104973878A (en) * 2015-06-01 2015-10-14 安徽省益民工贸集团有限公司 Hydroxyapatite whisker reinforced glass ceramic dish and preparation method thereof
CN105884200A (en) * 2016-04-11 2016-08-24 大连理工大学 Method for producing microcrystalline glass-ceramic composite material from industrial fly ash and vitrification slag
CN105948508A (en) * 2016-04-25 2016-09-21 四川名微晶科技股份有限公司 Glass-ceramic prepared from ferronickel waste residue by using all-electric melting rolling method and preparation 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
CN106810076A (en) * 2017-01-05 2017-06-09 四川名微晶科技股份有限公司 The production method of crystallizing glass sheet material
CN107129156A (en) * 2017-06-06 2017-09-05 广东环境保护工程职业学院 A kind of graphene devitrified glass and preparation method thereof
CN108751720A (en) * 2018-07-03 2018-11-06 四川名微晶科技股份有限公司 A kind of method that the utilization of granite Making Use of Tailings prepares devitrified glass
CN109369026A (en) * 2018-10-31 2019-02-22 昆明理工大学 The method that producing yellow Phosphorus by electric oven prepares high calcium heterogeneous devitrified glass simultaneously
CN110818266A (en) * 2019-11-26 2020-02-21 西南科技大学 Preparation method of basalt microcrystalline glass
CN111847871A (en) * 2019-04-30 2020-10-30 桂林理工大学 Method for preparing high-physical-property glass by using dilong granite as auxiliary agent

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103951188A (en) * 2014-04-22 2014-07-30 武汉理工大学 Black decorative glass taking gold-copper tailing as main raw material and preparation 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
CN104973878A (en) * 2015-06-01 2015-10-14 安徽省益民工贸集团有限公司 Hydroxyapatite whisker reinforced glass ceramic dish and preparation method thereof
CN105884200B (en) * 2016-04-11 2018-08-21 大连理工大学 A method of manufacturing devitrified glass ceramics composite material using industrial fly ash and vitrifying slag
CN105884200A (en) * 2016-04-11 2016-08-24 大连理工大学 Method for producing microcrystalline glass-ceramic composite material from industrial fly ash and vitrification slag
CN105948508A (en) * 2016-04-25 2016-09-21 四川名微晶科技股份有限公司 Glass-ceramic prepared from ferronickel waste residue by using all-electric melting rolling method and preparation method thereof
CN105948508B (en) * 2016-04-25 2018-05-01 四川一名微晶科技股份有限公司 It is devitrified glass that raw material is produced using all-electric melting rolling process and preparation method thereof using ferronickel waste residue
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
CN106810076A (en) * 2017-01-05 2017-06-09 四川名微晶科技股份有限公司 The production method of crystallizing glass sheet material
CN107129156A (en) * 2017-06-06 2017-09-05 广东环境保护工程职业学院 A kind of graphene devitrified glass and preparation method thereof
CN108751720A (en) * 2018-07-03 2018-11-06 四川名微晶科技股份有限公司 A kind of method that the utilization of granite Making Use of Tailings prepares devitrified glass
CN109369026A (en) * 2018-10-31 2019-02-22 昆明理工大学 The method that producing yellow Phosphorus by electric oven prepares high calcium heterogeneous devitrified glass simultaneously
CN111847871A (en) * 2019-04-30 2020-10-30 桂林理工大学 Method for preparing high-physical-property glass by using dilong granite as auxiliary agent
CN110818266A (en) * 2019-11-26 2020-02-21 西南科技大学 Preparation method of basalt microcrystalline glass

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