CN101462820B - Low-expansion glass-ceramics moulding method for lithium-aluminum-silicon system - Google Patents
Low-expansion glass-ceramics moulding method for lithium-aluminum-silicon system Download PDFInfo
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- CN101462820B CN101462820B CN200910036518XA CN200910036518A CN101462820B CN 101462820 B CN101462820 B CN 101462820B CN 200910036518X A CN200910036518X A CN 200910036518XA CN 200910036518 A CN200910036518 A CN 200910036518A CN 101462820 B CN101462820 B CN 101462820B
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- glass
- temperature
- forming
- fire door
- stove
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- 238000000034 method Methods 0.000 title claims abstract description 22
- -1 lithium-aluminum-silicon Chemical compound 0.000 title claims abstract description 6
- 239000002241 glass-ceramic Substances 0.000 title claims description 9
- 238000000465 moulding Methods 0.000 title description 8
- 239000011521 glass Substances 0.000 claims abstract description 34
- 239000005357 flat glass Substances 0.000 claims abstract description 20
- 238000002425 crystallisation Methods 0.000 claims abstract description 3
- 230000008025 crystallization Effects 0.000 claims abstract description 3
- 239000013081 microcrystal Substances 0.000 claims description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000007496 glass forming Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims 2
- 230000006835 compression Effects 0.000 abstract 4
- 238000007906 compression Methods 0.000 abstract 4
- 238000003490 calendering Methods 0.000 abstract 1
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000003973 paint Substances 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- 238000005498 polishing Methods 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
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Abstract
The invention relates to a forming method for lithium-aluminum-silicon system low expansion microcrystalline glass. The process comprises the following steps: A, spreading upper paint on a working surface of a forming die comprising a lower die and a compression upper die, and drying the working surface of the forming die for standby; B, cutting microcrystalline sheet glass produced through a calendering method into pieces, and putting the microcrystalline sheet glass pieces into the lower die; C, preheating the compression upper die on a fire hole to more than or equal to 400 DEG C; D, picking the lower die containing the microcrystalline sheet glass into an electric furnace for preheating; E, picking the compression upper die into the furnace and placing the compression upper die above the microcrystalline sheet glass; and F, closing a furnace door, increasing, keeping and decreasing the temperature according to a temperature time curve, and after the softening and crystallization forming of the microcrystalline glass, opening the furnace door to cool down the glass below a softening point and taking the glass out of the furnace.
Description
Technical field:
The present invention relates to a kind of devitrified glass forming method, specifically is the roasting bent forming method that bends of a kind of lithium-aluminium-silicon system low-expansion glass-ceramics.
Background technology:
In simple glass curved technology, it is that sheet glass with definite shape places mould, under the effect of temperature, sheet glass is reached or be higher than the above temperature of softening temperature, deadweight that promptly can glass, crooked gradually, and depend on die surface and moulding (as shown in Figure 1).But in devitrified glass curved process, though and the simple glass curved common feature is arranged---devitrified glass is heated to softening temperature or is higher than the temperature of softening temperature.But the particularly black Jinping of devitrified glass sheet glass is more than annealing temperature, it until about 760 ℃ the nucleus growth process, a large amount of generations along with nucleus, its bending strength is constantly strengthened because of crystal, the softening temperature of black Jinping sheet glass if do not add any extraneous factor this moment, is can not natural moulding in 780 ℃~800 ℃ scopes, along with the rising of furnace temperature, black brilliant plate can only be a more shallow camber line (as shown in Figure 2).
Summary of the invention:
The object of the present invention is to provide a kind of devitrified glass forming method, specifically is the roasting bent method that becomes spherical cambered surface of bending of a kind of lithium-aluminium-silicon system low-expansion glass-ceramics, makes the spherical cambered surface devitrified glass of the machine-shaping high-power matrix electromagnetic stove that can be used for forming a complete production network.
The present invention, its technology comprises:
A, on the working face of forming mould, coat, dry for standby, forming mould comprise counterdie and the pressurization patrix;
B, will cut into piece, be positioned in the counterdie by the crystallite sheet glass that rolling process is produced;
C, the pressurization patrix place fire door be preheated to 〉=400 ℃;
D, then the counterdie that crystallite sheet glass is housed is chosen in the electric furnace preheating;
E, the patrix that will pressurize are chosen the top that stove into is built in crystallite sheet glass;
F, fire door is closed, press temperature time curve intensification, constant temperature and cooling, make that devitrified glass is softening, after the crystallization forming, open when fire door is cooled to the following temperature of softening temperature and come out of the stove.
The present invention, the weight of described pressurization patrix is pressed the big subtotal of crystallite sheet glass, is advisable with every square centimeter of 10-18g.
The present invention, the material of described forming mould, can adopt metal or non-metallic material to be processed into, but, because ordinary metallic material at high temperature is easy to generate oxidation, non-metallic material such as carborundum plate, though boron plates etc. can be high temperature resistant, but easily broken when load-bearing, through screening, adopt the processing and manufacturing of 25Cr20Ni stainless material.
The present invention, when preventing that devitrified glass is higher than the above temperature of softening temperature and die surface be pasted together, before moulding, coating is evenly coated on the die-face, make the sealing coat that one deck 0.01mm-0.03mm is arranged between metal die and the devitrified glass.Described coating can be selected magnesium oxide, magnetic soil, talcum powder for use, is preferably magnesium oxide, converts water 8-12 doubly by magnesia powder, constitutes after 120 mesh sieves.With magnesium oxide as coating, neither can with mould generation chemical reaction, the corrosion material, can not paste together again, be easy to dispose, equally too devitrified glass with mould, after the moulding cooling, the coating that product external surfaces is adhered to can be disposed once brushing gently with hand brush.
Description of drawings:
Fig. 1 is a simple glass curved synoptic diagram;
Fig. 2 is devitrified glass curved (during the pressurization patrix) synoptic diagram;
Fig. 3 presses synoptic diagram for devitrified glass is roasting;
Fig. 4 presses synoptic diagram for the notch board devitrified glass is roasting;
Fig. 5-Fig. 6 is a notch board devitrified glass structural representation, and wherein Fig. 5 is a front view, and Fig. 6 is a sectional view;
Fig. 7 is the roasting molded temperature-time curve synoptic diagram of black glass ceramic;
Fig. 8 is the roasting molded temperature-time curve synoptic diagram of white micro-crystals glass, and wherein curve A is applicable to the white micro-crystals glass that does not add before the transparent grog, and curve B is applicable to the white micro-crystals glass that has added behind the transparent grog.
Among the figure, 10, counterdie 20, pressurization patrix 21, upper molded plate 22, go up mold pressing core 30, devitrified glass.
Embodiment:
Embodiment 1, black glass ceramic forming method.
With reference to Fig. 3, the heating unit of moulding process adopts electric furnace, mould adopts 25Cr20Ni stainless steel forming mould, forming mould is made of counterdie 10 and pressurization patrix 20, at first, on the working face of counterdie 10 and pressurization patrix 20, to coat, the oven dry back forms the sealing coat of one deck 0.01mm-0.03mm on the working face of mould, coating is converted water by magnesia powder and is made pulpous state for 10 times, after 120 mesh sieves, constitute after removing coarse particles and impurity, get φ 410mm, thick is the black crystallite sheet glass 30 by rolling process production of 5mm, individual layer places on the counterdie 10, and the weight of pressurization patrix 20 is got 15.5kg, the patrix 20 that pressurizes place fire door be preheated to 〉=400 ℃; Then the counterdie 10 that black crystallite sheet glass is housed is chosen in the electric furnace, preheating 1-5 minute, temperature is reached about 600 ℃, the patrix 20 that will pressurize is again chosen the top that stove into is built in crystallite sheet glass 30, fire door is closed, heat up by temperature time curve shown in Figure 7, constant temperature and cooling, promptly start at, be warming up to 840 ± 3 ℃, constant temperature 5 minutes with 480 ℃ speed per hour from being preheated to 600 ℃, be warming up to 960 ± 3 ℃ with 480 ℃ speed per hour again, constant temperature stops heating after 10 minutes, open fire door, naturally cools to below 800 ℃, outside the taking-up stove, allow it naturally cool to room temperature.Obtain the black glass ceramic of spherical cambered surface, obtain the black brilliant pot of large size of φ 407mm * h85mm after deburring, high-power matrix electromagnetic stove can be used for forming a complete production network.
Embodiment 2, white micro-crystals glass forming method.
With reference to Fig. 3, heating unit, forming mould and coating and the method for coating are identical with embodiment 1, white micro-crystals glass is got φ 320mm, thick is the white micro-crystals sheet glass 30 by rolling process production of 5mm, individual layer places on the counterdie 10, the weight of pressurization patrix 20 is got 11.5kg, the patrix 20 that pressurizes place fire door be preheated to 〉=400 ℃; Then the counterdie 10 that white micro-crystals sheet glass is housed is chosen in the electric furnace, preheating reaches about 600 ℃ temperature, the patrix 20 that will pressurize is again chosen the top that stove into is built in crystallite sheet glass 30, fire door is closed, heat up by temperature time curve shown in Figure 8, constant temperature and cooling, promptly start at from being preheated to 600 ℃, be warming up to 1050 ± 3 ℃ with 480 ℃ speed per hour and (be adapted to add the white micro-crystals glass after the transparent grog, shown in the curve B) or 1080 ± 3 ℃ (be adapted to not add the white micro-crystals glass before the transparent grog, shown in the curve A), constant temperature 30 minutes, stop heating then, open fire door, naturally cool to below 800 ℃, outside the taking-up stove, allow it naturally cool to room temperature.Obtain the white micro-crystals glass of spherical cambered surface, obtain the white brilliant pot of medium size of φ 317mm * h61mm after deburring, high-power matrix electromagnetic stove can be used for forming a complete production network.
The forming method of embodiment 3, white micro-crystals glass notch board
With reference to Fig. 4-Fig. 6, size 272 * 272 * 5mm of notch plate, central recessed sphere circular diameter is 112mm, depth of recess is 8.5mm, it is a grinding and polishing process after the first moulding of employing, the corner angle that just can present the central sphere circle of notch plate through flour milling are clearly demarcated, if can't embody by curved technology merely, so its last finished product is to carry out in two steps of branch.
1, curved.Specified dimension white micro-crystals glass is placed on the mold center position, the material of mould is identical with embodiment 1, coating is also identical, forming mould is made of counterdie 10, upper molded plate 21 and last mold pressing core 22, the method of putting of white micro-crystals glass 30 and mould as shown in Figure 4, place electric furnace to be heated to 1080 ± 3 ℃ then, insulation 20min postcooling takes out and gets final product.
2, grinding and polishing.Notch plate can only be calculated work in-process after the curved moulding, connect down also and must process through grinding and polishing, could embody the clearly demarcated of concave surface and plane corner angle, and grinding and polishing is processed as prior art, and description is omitted, the intaglio plate after grinding and polishing processing such as Fig. 5-and shown in Figure 6.
Claims (3)
1. lithium-aluminium-silicon system low-expansion glass-ceramics forming method, its technology comprises:
A, on the working face of forming mould, coat, dry for standby, forming mould comprise counterdie and the pressurization patrix;
B, will cut into piece, be positioned in the counterdie by the crystallite sheet glass that rolling process is produced;
C, the pressurization patrix place fire door be preheated to 〉=400 ℃;
D, then the counterdie that the dull and stereotyped broken glass of crystallite is housed is chosen in the electric furnace preheating;
E, the patrix that will pressurize are chosen the top that stove into is built in crystallite sheet glass;
F, fire door is closed, press temperature time curve intensification, constant temperature and cooling, make that devitrified glass is softening, after the crystallization forming, open when fire door is cooled to the following temperature of softening temperature and come out of the stove, mold temperature time curve during the preparation black glass ceramic is: start at from being preheated to 600 ℃, be warming up to 840 ± 3 ℃ with 480 ℃ speed per hour, constant temperature 5 minutes, be warming up to 960 ± 3 ℃ with 480 ℃ speed per hour again, constant temperature stops heating after 10 minutes, open fire door, naturally cools to below 800 ℃, outside the taking-up stove, allow it naturally cool to room temperature; Mold temperature time curve during preparation white micro-crystals glass is: start at from being preheated to 600 ℃, be warming up to 1050 ± 3 ℃ or 1080 ± 3 ℃ with 480 ℃ speed per hour, constant temperature 30 minutes, stop heating then, open fire door, naturally cool to below 800 ℃, take out outside the stove, allow it naturally cool to room temperature.
2. devitrified glass forming method according to claim 1 is characterized in that: described forming mould is processed into by the 25Cr20Ni stainless material.
3. devitrified glass forming method according to claim 1 is characterized in that: described coating is converted water 8-12 times pulp by magnesia powder, constitutes after 120 mesh sieves.
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CN101462820B true CN101462820B (en) | 2011-02-02 |
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CN103232152A (en) * | 2013-04-27 | 2013-08-07 | 四川一名微晶科技股份有限公司 | Production process of microcrystalline glass curved plate |
CN106166792A (en) | 2015-10-16 | 2016-11-30 | 圣戈本陶瓷及塑料股份有限公司 | There is crystalline ceramics and its manufacture method of complex geometric shapes |
CN105345938B (en) * | 2015-11-25 | 2018-03-27 | 哈尔滨奥瑞德光电技术有限公司 | A kind of mechanical hot bending sapphire forming method |
CN105776826A (en) * | 2016-03-14 | 2016-07-20 | 褚宗文 | Manufacturing process of glass melting |
CN111348834B (en) * | 2020-03-16 | 2022-06-07 | 科立视材料科技有限公司 | 3D glass ceramic and preparation method thereof |
CN114455811A (en) * | 2022-03-17 | 2022-05-10 | 南通向阳光学元件有限公司 | High-dispersion blue-green polycrystalline optical glass mould pressing production device |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0423698A1 (en) * | 1989-10-17 | 1991-04-24 | Asahi Glass Company Ltd. | Bend-shaping press mold, method of bend-shaping a glass plate and apparatus for bend-shaping a glass plate |
CN1157271A (en) * | 1996-12-23 | 1997-08-20 | 唐山市燕山产业有限公司 | Process for producing nucleated glass special-shaped decorative plates by using sintering method and special-purpose mould thereof |
CN1157268A (en) * | 1996-10-20 | 1997-08-20 | 湖州玻璃厂二分厂 | Nucleated glass special-shaped product shaping method and mould |
CN1566003A (en) * | 2003-07-09 | 2005-01-19 | 山东天虹弧板有限公司 | Manufacturing method for microcrystalline glass-ceramic composite curved plate |
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2009
- 2009-01-08 CN CN200910036518XA patent/CN101462820B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0423698A1 (en) * | 1989-10-17 | 1991-04-24 | Asahi Glass Company Ltd. | Bend-shaping press mold, method of bend-shaping a glass plate and apparatus for bend-shaping a glass plate |
CN1157268A (en) * | 1996-10-20 | 1997-08-20 | 湖州玻璃厂二分厂 | Nucleated glass special-shaped product shaping method and mould |
CN1157271A (en) * | 1996-12-23 | 1997-08-20 | 唐山市燕山产业有限公司 | Process for producing nucleated glass special-shaped decorative plates by using sintering method and special-purpose mould thereof |
CN1566003A (en) * | 2003-07-09 | 2005-01-19 | 山东天虹弧板有限公司 | Manufacturing method for microcrystalline glass-ceramic composite curved plate |
Non-Patent Citations (1)
Title |
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JP特开平6-211532A 1994.08.02 |
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