CN103496850B - Black micro-crystal glass plate and production method thereof - Google Patents
Black micro-crystal glass plate and production method thereof Download PDFInfo
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- CN103496850B CN103496850B CN201310441663.2A CN201310441663A CN103496850B CN 103496850 B CN103496850 B CN 103496850B CN 201310441663 A CN201310441663 A CN 201310441663A CN 103496850 B CN103496850 B CN 103496850B
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- 239000011521 glass Substances 0.000 title claims abstract description 63
- 239000013081 microcrystal Substances 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- 239000007858 starting material Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 241000276489 Merlangius merlangus Species 0.000 claims abstract description 6
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000001506 calcium phosphate Substances 0.000 claims abstract description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 6
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 6
- 235000014380 magnesium carbonate Nutrition 0.000 claims abstract description 6
- 229910000150 monocalcium phosphate Inorganic materials 0.000 claims abstract description 6
- 235000019691 monocalcium phosphate Nutrition 0.000 claims abstract description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 5
- 238000002425 crystallisation Methods 0.000 claims description 24
- 230000008025 crystallization Effects 0.000 claims description 24
- 238000005352 clarification Methods 0.000 claims description 12
- 238000000265 homogenisation Methods 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 8
- 238000005096 rolling process Methods 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 abstract description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010936 titanium Substances 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002667 nucleating agent Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 15
- 239000000203 mixture Substances 0.000 description 7
- 239000002241 glass-ceramic Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000010438 granite Substances 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000003490 calendering Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- Glass Compositions (AREA)
Abstract
The invention discloses a kind of black micro-crystal glass plate and production method thereof, described 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:3 ~ 4 part; CaO:4 ~ 8 part; Fe
2o
3: 5 ~ 10 parts; TiO
2: 1.5 ~ 2.5 parts.Described production method is by 9 ~ 20 parts, magnesite, 30 ~ 50 parts, grouan, monocalcium phosphate 0.5 ~ 3 part, coarse whiting 1 ~ 8 part, adopts all-electric melting to roll and produce after the mixing of 30 ~ 70 parts, basalt.The present invention, through the proportioning of the crystallizing glass sheet material that studies for a long period of time, obtains the formula of black micro-crystal glass plate, and obtains the production method of producing this black micro-crystal glass plate; Breach the situation that existing crystallizing glass sheet material color is single; With basalt waste residue, grouan for main raw material, containing a large amount of ferro elements and titanium elements in basalt waste residue, titanium as Nucleating Agent, can reduce P
2o
5amount, without the need to adding iron oxide red in starting material; Starting material are all easy to get, and cost is low.
Description
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, has again the polycrystalline feature of pottery, has concentrated the feature of glass and pottery, has become 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, obtain in the world in recent years and develop fast." 12 new material industry development program " that particularly in January, 2012, Ministry of Industry and Information of country announced, listing calendering devitrified glass in give priority to new inorganic non-metallic materials catalogue, having great importance to rolling the application of devitrified glass in fundamental new material field from now on.
The production of tradition devitrified glass adopts sintering process technique, and the energy consumption high problem that sintering process technique faces in devitrified glass is produced is the critical bottleneck of the fast development of restriction devitrified glass and large-scale production always.Sintering process explained hereafter devitrified glass and expensive non-ferrous metal zinc oxide starting material will be used, the production cost of a lot of devitrified glass enterprise is remained high always, simultaneously sintering process production technique efficiency is low, and product has that pore, planeness are poor, the devitrified glass enterprise management condition of sintering process technique is always had difficulty in taking a step.The all-electric melting rolling process that company initiates in the whole nation is produced 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), has filled up domestic blank.Adopt 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 will significantly reduce, and can also be that country saves a large amount of non-ferrous metal zinc oxide precious materials.The invention of this technology, has complied with the development trend of China's new material industry and the requirement in continuous broadened application field.
Current utilization is discarded granite and is adopted 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 meet the demand of market to multi items, multi-color devitrified glass, therefore need formula and the production technique of constantly studying the devitrified glass of different pattern.
Summary of the invention
The object 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 one: choose starting material according to following weight parts: 9 ~ 20 parts, magnesite, 30 ~ 50 parts, grouan, monocalcium phosphate 0.5 ~ 3 part, coarse whiting 1 ~ 8 part, 30 ~ 70 parts, basalt;
Step 2: above-mentioned starting material are mixed, and add the water of starting material gross weight 2%, mixing 3 ~ 5min, compound is sent into the melting pool of All Electric Melting Furnace, controlled melting temperature is 1350 ~ 1500 DEG C; Glass after fusing carries out clarification and homogenization, and the temperature of clarification and homogenization is 1400 ~ 1450 DEG C, and the time of clarification and homogenization is 7 ~ 8h;
Step 3: the glass clarified, homogenizing is good is entered material road through dog-hole, uptake, and temperature reduces to 1250 ~ 1300 DEG C, after the cooling of material road, enter rolling press and be molded into glass ribbon, mold temperature is 1150 ~ 1250 DEG C;
Step 4: the glass ribbon after shaping carries out anneal, kiln temperature degree brought into by glass is 650 ~ 800 DEG C, 680 ~ 750 DEG C of insulations after 10 ~ 20 minutes, 580 ~ 620 DEG C are cooled to by the speed of 3 DEG C/minute ~ 5 DEG C/minute, 300 DEG C are cooled to again by the speed of 7 DEG C/minute ~ 12 DEG C/minute, be cooled to 35 ~ 45 DEG C through 40 ~ 60 minutes again, kiln discharge, cut rear generation annealed sheet;
Step 5: annealed sheet is sent into crystallization kiln carries out coring, crystallization becomes crystallization plate, be specially: be warming up to 600 DEG C ~ 720 DEG C through 30 ~ 90 minutes, in 600 DEG C ~ 720 DEG C insulations coring in 30 ~ 90 minutes, 820 DEG C ~ 930 DEG C are warming up to again through 30 ~ 90 minutes, in 820 DEG C ~ 930 DEG C insulations, 30 ~ 120 minutes crystallization, be cooled to 35 ~ 45 DEG C of kiln discharges through 60 ~ 120 minutes;
Step 6: crystallization plate is carried out polish, polishing.
The present invention compared with prior art, has following beneficial effect:
(1) the present invention is through the proportioning of the crystallizing glass sheet material that studies for a long period of time, obtains the formula of black micro-crystal glass plate, and obtains the production method of producing this black micro-crystal glass plate, breaches the situation that existing crystallizing glass sheet material color is single.
(2) produce black micro-crystal glass plate and provide MgO with basalt waste residue, grouan for main raw material, magnesite, monocalcium phosphate provides P
2o
5and CaO, coarse whiting provides CaO, and containing a large amount of ferro elements and titanium elements in basalt waste residue, titanium as Nucleating Agent, can reduce P
2o
5amount, without the need to adding iron oxide red in starting material; Starting material are all easy to get, and cost is low.
(3) the product ultimate compression strength 200-300MPa of the present invention's production, 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 mixing, mixing time is 4min, and add 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)
2, sent into by above-mentioned compound in the melting pool of All Electric Melting Furnace, controlled melting temperature is 1350 DEG C, and the glass after fusing carries out clarification and homogenization, and the temperature of clarification and homogenization is 1400 DEG C, and the time of clarification and homogenization is 8h.
3, the glass clarified, homogenizing is good is entered material road through dog-hole, uptake, temperature reduces to 1280 DEG C, and after the cooling of material road, enter rolling press and be molded into glass ribbon, mold temperature is 1150 DEG C; Thickness, the width of formed glass band regulate according to the requirement of producing sheet.
4, the glass ribbon after shaping enters annealing furnace carry out anneal through transmitting roller tables, kiln temperature degree brought into by glass is 700 DEG C, 680 DEG C of insulations after 15 minutes, 580 DEG C are cooled to by the speed of 3 DEG C/minute, 300 DEG C are cooled to again by the speed of 9 DEG C/minute, be cooled to 40 DEG C through 60 minutes again, kiln discharge, then enter cold junction line of cut.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), delivers to nucleus crystallization in crystallization kiln through transition roller table.
5, annealed sheet is sent into crystallization kiln carries out coring, crystallization becomes crystallization plate, be specially: be warming up to 700 DEG C through 60 minutes, in 700 DEG C of insulations coring in 60 minutes, then be warming up to 900 DEG C through 45 minutes, in 900 DEG C of insulations, 100 minutes crystallization, be cooled to 40 DEG C of kiln discharges through 120 minutes.
6, crystallization plate is carried out polish, polishing.
The black glass ceramic of above-mentioned preparation is carried out composition detection, and the result of composition detection is as shown in table 2.
Table 2: the composition analysis of the black glass ceramic that embodiment 1 is produced
| 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 mixing, mixing time is 4min, and add water 10Kg.
| Material name | Magnesite | Granite | Monocalcium phosphate | Coarse whiting | Basalt |
| Weight (Kg) | 64 | 181 | 2.4 | 7.6 | 242 |
2, sent into by above-mentioned compound in the melting pool of All Electric Melting Furnace, controlled melting temperature is 1350 DEG C, and the glass after fusing carries out clarification and homogenization, and the temperature of clarification and homogenization is 1400 DEG C, and the time of clarification and homogenization is 8h.
3, the glass clarified, homogenizing is good is entered material road through dog-hole, uptake, temperature reduces to 1280 DEG C, and after the cooling of material road, enter rolling press and be molded into glass ribbon, mold temperature is 1150 DEG C; Thickness, the width of formed glass band regulate according to the requirement of producing sheet.
4, the glass ribbon after shaping enters annealing furnace carry out anneal through transmitting roller tables, kiln temperature degree brought into by glass is 700 DEG C, 680 DEG C of insulations after 15 minutes, 580 DEG C are cooled to by the speed of 3 DEG C/minute, 300 DEG C are cooled to again by the speed of 9 DEG C/minute, be cooled to 40 DEG C through 60 minutes again, kiln discharge, then enter cold junction line of cut.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), delivers to nucleus crystallization in crystallization kiln through transition roller table.
5, annealed sheet is sent into crystallization kiln carries out coring, crystallization becomes crystallization plate, be specially: be warming up to 720 DEG C through 60 minutes, in 720 DEG C of insulations coring in 60 minutes, then be warming up to 930 DEG C through 60 minutes, in 930 DEG C of insulations, 100 minutes crystallization, be cooled to 40 DEG C of kiln discharges through 120 minutes.
6, crystallization plate is carried out polish, polishing.
The black glass ceramic of above-mentioned preparation is carried out composition detection, and the result of composition detection is as shown in table 3.
Table 3: the composition analysis of the black glass ceramic that embodiment 2 is produced
| 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 the present invention's preferably embodiment, 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 amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (1)
1. a black micro-crystal glass plate, is characterized in that the component comprising 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; Described black micro-crystal glass plate adopts following preparation method to make:
Step one: choose starting material according to following weight parts: 9 ~ 20 parts, magnesite, 30 ~ 50 parts, grouan, monocalcium phosphate 0.5 ~ 3 part, coarse whiting 1 ~ 8 part, 30 ~ 70 parts, basalt;
Step 2: above-mentioned starting material are mixed, and add the water of starting material gross weight 2%, mixing 3 ~ 5min, compound is sent into the melting pool of All Electric Melting Furnace, controlled melting temperature is 1350 ~ 1500 DEG C; Glass after fusing carries out clarification and homogenization, and the temperature of clarification and homogenization is 1400 ~ 1450 DEG C, and the time of clarification and homogenization is 7 ~ 8h;
Step 3: the glass clarified, homogenizing is good is entered material road through dog-hole, uptake, and temperature reduces to 1250 ~ 1300 DEG C, after the cooling of material road, enter rolling press and be molded into glass ribbon, mold temperature is 1150 ~ 1250 DEG C;
Step 4: the glass ribbon after shaping carries out anneal, kiln temperature degree brought into by glass is 650 ~ 800 DEG C, 680 ~ 750 DEG C of insulations after 10 ~ 20 minutes, 580 ~ 620 DEG C are cooled to by the speed of 3 DEG C/minute ~ 5 DEG C/minute, 300 DEG C are cooled to again by the speed of 7 DEG C/minute ~ 12 DEG C/minute, be cooled to 35 ~ 45 DEG C through 40 ~ 60 minutes again, kiln discharge, cut rear generation annealed sheet;
Step 5: annealed sheet is sent into crystallization kiln carries out coring, crystallization becomes crystallization plate, be specially: be warming up to 600 DEG C ~ 720 DEG C through 30 ~ 90 minutes, in 600 DEG C ~ 720 DEG C insulations coring in 30 ~ 90 minutes, 820 DEG C ~ 930 DEG C are warming up to again through 30 ~ 90 minutes, in 820 DEG C ~ 930 DEG C insulations, 30 ~ 120 minutes crystallization, be cooled to 35 ~ 45 DEG C of kiln discharges through 60 ~ 120 minutes;
Step 6: crystallization plate is carried out polish, polishing.
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