CN108821598A - Devitrified glass and preparation method thereof - Google Patents
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Abstract
The present invention provides a kind of with higher hardness and amber devitrified glass resistant to high temperature.Devitrified glass, weight percent composition contain：SiO250-70%；Al2O310.0-25%；TiO23-10%；CuO 0.2-0.7%；MgO 0-22%；ZnO 0-20%；And at least containing one of component in MgO and ZnO.Devitrified glass Mohs' hardness of the invention is 7.5-8H, can apply in ornament materials and ornament, overcome the scuffing problem of common amber glass.Devitrified glass of the invention does not soften at a high temperature of 1150 DEG C, high temperature resistant, can carry out further processing under the high temperature conditions.Devitrified glass of the invention has high mechanical strength, hardness, thermal stability, and chemical stability, wearability and electrical insulation capability are good, can be used for the high-grade fitting-out work such as ornament materials, building inside and outside wall, ground and corridor column.
Description
The application is for application No. is 201510875782.8, and the applying date is on December 3rd, 2015, entitled " crystallite
The divisional application of the application for a patent for invention of glass and preparation method thereof ".
Technical field
The present invention relates to a kind of devitrified glass and preparation method thereof, more particularly, to a kind of amber devitrified glass and its
Preparation method.
Technical background
Devitrified glass has the advantages that glass, ceramics and lithotome, and has excellent thermodynamic property, chemical stabilization
The features such as property is good, intensity is high, wearability is high, lustrous surface is uniformly sparkling and crystal-clear, easy to clean, these characteristics determine that devitrified glass exists
Material Field occupies an important position, and can be used in the high-grade fitting-out work such as building inside and outside wall, ground and corridor column.
Traditional amber glass is coloured by addition selenium and cadmium in glass, since cadmium is toxic, is not suitable for
In existing environment, common amber glass Mohs' hardness is in 5H, and the cutter Mohs' hardness used usually is in 5.5-6H, sand
In gravel or dust contain silica Mohs' hardness 7H, these can existing amber ambetti surface cause scratch or
Abrasion, influences its decorative effect and service life, and common amber glass non-refractory, soft in 700-800 DEG C of beginning
Change, cannot use at high temperature.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to have higher hardness and amber crystallite resistant to high temperature
Glass.
The present invention also provides a kind of preparation method of above-mentioned devitrified glass.
The technical solution adopted for solving the technical problem of the present invention is：Devitrified glass, weight percent composition contain：
SiO250-70%；Al2O310.0-25%；TiO23-10%；CuO 0.2-0.7%；MgO 0-22%；ZnO 0-20%；
And at least containing one of component in MgO and ZnO.
Further, also contain：ZrO20-6%；P2O50-1.5%；Sb2O30-1.5%；Na2O 0-2%；K2O 0-
2%；Y2O30-2%；La2O30-1%.
Further, Na2O and K2The total content of O is below 2% and/or TiO2、ZrO2And P2O5Total content be not less than
7%.
Further, the total content of ZnO and MgO is 5-22% and/or TiO25-8% and/or CuO 0.4-0.6% and/
Or SiO2、Al2O3Total content be 70-80%.
Further, the total content of ZnO and MgO is 8-15%.
Further, the devitrified glass is amber devitrified glass, and the Mohs' hardness of the devitrified glass is 7.5-
8H。
The preparation method of devitrified glass, this approach includes the following steps：
(a) ingredient
The weight that raw material is weighed according to weight ratio, is poured into mixing machine, is used as presoma glass raw material after mixing；
(b) melting
Above-mentioned presoma glass raw material is put into smelting furnace, is melted and is clarified at high temperature, by presoma glass
Dissolution of raw material is high temp glass stoste, while removing bubble and foreign matter in high temp glass stoste；
(c) it forms and anneals
The high temp glass stoste melted is formed under certain tapping temperature, then carries out black annealing；
(d) it is heat-treated
Glass after above-mentioned black annealing is put into high temperature furnace and is heat-treated, can be given birth in glass after heat treatment
At the crystallite of spinel crystal, devitrified glass is obtained.
Further, step (a) raw material, wherein MgO, Na2O、K2O is in the form of carbonate, nitrate or sulfate
It introduces, other components introduce in the form of the oxide.
Further, step (b) is described is molten into：Temperature is at 1550-1600 DEG C, and the time is in 4-10h；The clarification is：
Temperature is at 1600-1650 DEG C, and the time is in 4-10h.
Further, step (c) tapping temperature is 1500-1600 DEG C；It is described to be shaped to：By cold in mold heat
But it forms, or is formed by float glass process, die mould method.
Further, the mold heat is：Guarantee mold temperature at 100-450 DEG C in forming process；It is described to be cooled to：
After high-temperature glass liquid is poured into mold heat, cooling is blowed to mold heat.
Further, heat treatment described in step (d) includes that nucleus is precipitated and crystallite two stages of growth；The nucleus analysis
Stage required temperature is 750-900 DEG C out, duration 1-4h；The crystallite growth stage required temperature is 800-1000
DEG C, duration 0.5-4h.
The beneficial effects of the invention are as follows：The present invention is used and is heat-treated to presoma glass, the crystallization from glass matrix
Crystallite method is precipitated, prepares amber devitrified glass, preparation process of the invention is simple, and it is at low cost, it is suitble to large-scale
Production.The amber devitrified glass Mohs' hardness that the present invention prepares is 7.5-8H, can effectively be applied in ornament materials
In ornament, the scuffing problem of common amber glass is overcome, service life is extended.The amber that the present invention prepares
The devitrified glass of color has high softening temperature, does not soften, high temperature resistant at a high temperature of 1150 DEG C, can carry out in high temperature item
Further processing under part.The amber devitrified glass that the present invention prepares has high mechanical strength, hardness, thermostabilization
Property, chemical stability, wearability and electrical insulation capability are good, can be used for the top grades such as ornament materials, building inside and outside wall, ground and corridor column
Fitting-out work.
Specific embodiment
The present invention is with ZnO (MgO)-Al2O3-SiO2-TiO2- CuO is system, prepares presoma glass by melting process
Glass, presoma glass is annealed and is heat-treated, and prepares amber devitrified glass.Be described below its weight percent content and
It is acted on.
SiO2、Al2O3, perhaps ZnO is to constitute the main component of devitrified glass of the present invention according to MgO (or ZnO)-to MgO
Al2O3-SiO2Phasor, the present invention in, SiO2Content be 50-70%；Al2O3Content be 10-25%；The content of MgO is 0-
The content of 22%, ZnO are 0-20%, in the present invention, at least containing one of component in MgO and ZnO, and further,
MgO and ZnO total content is 5-22%, preferably 8-15%.After the content of MgO and ZnO exceeds above range, in glass can
There are other crystal, requirement of the invention is not achieved.SiO2And Al2O3Total content be 70-80%.Work as SiO2And Al2O3It is total
When content is less than 70%, the hardness of glass is not reached requirement, and works as SiO2And Al2O3Total content when being more than 80%, melting is difficult.
The content range of the above component can form magnesium aluminate spinel or/and gahnite crystallite in glass, to improve glass
The hardness of glass.
TiO2There are two effects in the present invention：1) due to TiO2It can be carried out coloring in glass system, no other
In the case of toner, the presentation of presoma glass is light yellow, and content cannot be very few, very few not have color developing effect；It 2) is crystallite of the present invention
The main nucleating agent of glass.TiO2Content be 3-10%, preferably 5-8%.If content is too low, glass nucleation quantity is low,
Influence glass crystallization；If content has been more than 10%, nucleating agent is excessive, forms and is easy hair-cream, can not form glass.
The main function of CuO is colorant, in the case where no other colorants, when the content of CuO is 0.2-0.7%
When, presoma glass is blue.When the content of CuO is lower than 0.2%, glass blue is shallow, effect of arriving；And when its content is high
When 0.7%, glass blue is too deep, and in the present invention, the content of CuO is 0.2-0.7%, preferably 0.4-0.6%.
The TiO of the above content is added simultaneously under glass system of the invention2And CuO, it is presented after the molding of presoma glass
Yellow green after heat treatment, in glass has small crystal, this crystal has scattering process in visible light, with presoma yellow green
Glass is mixed, and amber devitrified glass is formd.
ZrO2And P2O5It for the nucleating agent of crystal in glass, generally will use a variety of nucleating agents, nucleus number can be promoted in this way
Amount is more, and crystalline size is small and uniform after crystallization.ZrO2Fusion temperature is high, and content is usually no more than 6%；P2O5Content can excessively go out
Existing split-phase, is usually no more than 1.5%.
Preferably, nucleating agent TiO of the invention2、ZrO2And P2O5Total content be not less than 7%.
Sb2O3For clarifying agent, content is no more than 1.5%, and content does not have clarification excessively.
Na2O and K2O is cosolvent, reduction glass melting temperature and clarifying temp, but Na2O、K2The content of O all cannot
More than 2%, the hardness decline of glass excessively will lead to.Preferably, cosolvent Na of the invention2O and K2The total content of O 2% with
Under.
Y2O3And La2O3It is additional additive, under the premise of not reducing glass hard (HRC65Yi Shang), can slightly reduces the fusing of glass
Temperature, but cannot be too many, Y2O3Content no more than 2%, La2O3Content no more than 1%.
Amber devitrified glass of the invention, mainly using spinelle as principal crystalline phase, and containing a small amount of quartz solid solution,
The crystal such as cordierite and sapphirine.
Preparation method of the invention includes the following steps：
(a) ingredient
Content is formed according to the weight of presoma glass, wherein MgO, Na2O、K2O is drawn with carbonate, nitrate or sulfate
Enter, other components introduce in the form of an oxide.According to weight ratio, the weight of raw material is weighed, is poured into mixing machine, is uniformly mixed
It is used as presoma glass raw material afterwards；
(b) melting
Above-mentioned presoma glass raw material is put into smelting furnace, is melted and is clarified at high temperature, by presoma glass
Dissolution of raw material is high temp glass stoste, while removing bubble and foreign matter in high temp glass stoste；
(c) it forms and anneals
By the high temp glass stoste melted under certain tapping temperature, by lower molding cooling in mold heat, or pass through
Float glass process, the molding of die mould method, the glass of forming black annealing in Muffle furnace；
(d) it is heat-treated
The glass of above-mentioned black annealing is put into high temperature furnace Muffle furnace and is heat-treated, it can be in glass after heat treatment
The middle crystallite for generating spinel crystal, obtains high rigidity devitrified glass of the invention.
V-arrangement mixing machine can be used in mixing machine in above-mentioned steps (a).Being molten into above-mentioned steps (b)：Temperature exists
1550-1600 DEG C, the time is in 4-10h；Clarification is：Temperature is at 1600-1650 DEG C, and the time is in 4-10h；The smelting furnace is using electricity
Furnace or crucible furnace.Tapping temperature is 1500-1600 DEG C in above-mentioned steps (c)；Mold heat refers to：Guarantee mold in forming process
Temperature is at 100-450 DEG C；The cooling refers to：After high-temperature glass liquid is poured into mold heat, mold heat is blowed
It is cooling；Annealing temperature is to 700-800 DEG C；Heat treatment process in above-mentioned steps (d) includes that nucleus is precipitated and crystallite growth two
Stage, wherein temperature needed for nucleus precipitation phase is 750-900 DEG C, duration 1-4h；Needed for crystallite growth stage
Temperature is 800-1000 DEG C, duration 0.5-4h.
The present invention is heat-treated using presoma glass, and crystallite method is precipitated in crystallization from glass matrix, prepares amber
Amber color devitrified glass, Mohs' hardness are resistant to 1150 DEG C of high temperature in 7.5-8H.
Table 1-2 is the embodiment of the present invention 1-13, is carried out first, in accordance with weight content is formed in embodiment 1-13 in table 1-2
Weighing and burden can be carbonate, nitrate and oxide etc. in raw material, load weighted raw material be all then put into V-arrangement and is mixed
Conjunction machine is used as glass raw material after being thoroughly mixed.Then prepared glass raw material is put into electric furnace, at 1550-1600 DEG C
At a temperature of carry out fusing 4-10 hour, carried out at a temperature of 1600-1650 DEG C clarify 4-10 hours, the glass that then will have been melted
Liquid is come out of the stove at 1500-1600 DEG C, is molded, and mold temperature carries out strong wind cooling at 100-450 DEG C, molding, is made
Female glass in 700-800 DEG C of black annealing of Muffle furnace.
Female glass obtained is put into high temperature furnace and is heat-treated, the heat treatment process include nucleus be precipitated and crystallite at
Long two stages make the temperature in Muffle furnace be maintained at 750-900 DEG C wherein in nucleus precipitation phase, and continuing 1-4h makes glass
Middle generation polycrystalline core as far as possible, is then increased to 800-1000 DEG C or so for the temperature in Muffle furnace and enters crystallite growth stage
And continue 0.5~4h, amber devitrified glass of the invention is made.
Proportion composition, crystal phase type and the Mohs' hardness of devitrified glass are listed in table 1-2.
Table 1
Table 2
Claims (12)
1. devitrified glass, which is characterized in that its weight percent composition contains：SiO250-70%；Al2O310-25%；TiO2
3-10%；CuO 0.2-0.7%；MgO 0-22%；ZnO 0-20%；And at least containing one of group in MgO and ZnO
Point.
2. devitrified glass as described in claim 1, which is characterized in that also contain：ZrO20-6%；P2O50-1.5%；Sb2O3
0-1.5%；Na2O 0-2%；K2O 0-2%；Y2O30-2%；La2O30-1%.
3. devitrified glass as claimed in claim 2, which is characterized in that Na2O and K2The total content of O below 2% and/or
TiO2、ZrO2And P2O5Total content be not less than 7%.
4. devitrified glass as described in claim 1, which is characterized in that the total content of ZnO and MgO is 5-22% and/or TiO2
5-8% and/or CuO 0.4-0.6% and/or SiO2、Al2O3Total content be 70-80%.
5. devitrified glass as described in claim 1, which is characterized in that the total content of ZnO and MgO is 8-15%.
6. devitrified glass as described in claim 1, which is characterized in that the devitrified glass is amber devitrified glass, institute
The Mohs' hardness for stating devitrified glass is 7.5-8H.
7. the preparation method of devitrified glass, this approach includes the following steps：
(a) ingredient
The weight that raw material is weighed according to weight ratio, is poured into mixing machine, is used as presoma glass raw material after mixing；
(b) melting
Above-mentioned presoma glass raw material is put into smelting furnace, is melted and is clarified at high temperature, by presoma glass raw material
It is dissolved as high temp glass stoste, while removing bubble and foreign matter in high temp glass stoste；
(c) it forms and anneals
The high temp glass stoste melted is formed under certain tapping temperature, then carries out black annealing；
(d) it is heat-treated
Glass after above-mentioned black annealing is put into high temperature furnace and is heat-treated, point can be generated after heat treatment in glass
The crystallite of spar crystal, obtains devitrified glass.
8. the preparation method of devitrified glass as claimed in claim 7, which is characterized in that step (a) raw material, wherein MgO,
Na2O、K2O is introduced in the form of carbonate, nitrate or sulfate, and other components introduce in the form of the oxide.
9. the preparation method of devitrified glass as claimed in claim 7, which is characterized in that step (b) is described to be molten into：Temperature exists
1550-1600 DEG C, the time is in 4-10h；The clarification is：Temperature is at 1600-1650 DEG C, and the time is in 4-10h.
10. the preparation method of devitrified glass as claimed in claim 7, which is characterized in that step (c) tapping temperature is
1500-1600℃；It is described to be shaped to：It is formed by being cooled and shaped in mold heat, or by float glass process, die mould method.
11. the preparation method of devitrified glass as claimed in claim 10, which is characterized in that the mold heat is：It was forming
Guarantee mold temperature at 100-450 DEG C in journey；It is described to be cooled to：After high-temperature glass liquid is poured into mold heat, to mold heat
Cooling is blowed.
12. the preparation method of devitrified glass as claimed in claim 7, which is characterized in that heat treatment described in step (d) includes
Nucleus is precipitated and crystallite is grown up two stages；The nucleus precipitation phase required temperature is 750-900 DEG C, duration 1-
4h；The crystallite growth stage required temperature is 800-1000 DEG C, duration 0.5-4h.
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| CN105347685A (en) | 2016-02-24 |
| CN105347685B (en) | 2019-01-04 |
| CN108821598B (en) | 2021-09-28 |
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