CN113121111A - Heat-insulating energy-saving glass and preparation method thereof - Google Patents
Heat-insulating energy-saving glass and preparation method thereof Download PDFInfo
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- CN113121111A CN113121111A CN202110289254.XA CN202110289254A CN113121111A CN 113121111 A CN113121111 A CN 113121111A CN 202110289254 A CN202110289254 A CN 202110289254A CN 113121111 A CN113121111 A CN 113121111A
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- 239000011521 glass Substances 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title abstract description 6
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000137 annealing Methods 0.000 claims abstract description 25
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 12
- 238000010791 quenching Methods 0.000 claims abstract description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims abstract description 11
- 150000008041 alkali metal carbonates Chemical class 0.000 claims abstract description 11
- 229910001508 alkali metal halide Inorganic materials 0.000 claims abstract description 11
- 150000008045 alkali metal halides Chemical class 0.000 claims abstract description 11
- 229910052796 boron Inorganic materials 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004327 boric acid Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 229910021538 borax Inorganic materials 0.000 claims abstract description 3
- 239000008395 clarifying agent Substances 0.000 claims abstract description 3
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 24
- 239000006060 molten glass Substances 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 13
- 230000000171 quenching effect Effects 0.000 claims description 9
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims description 5
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 229910052701 rubidium Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 241000143437 Aciculosporium take Species 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 5
- 238000002834 transmittance Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 7
- 239000010408 film Substances 0.000 description 5
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000004134 energy conservation Methods 0.000 description 4
- -1 indium and antimony Chemical class 0.000 description 4
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 229910000906 Bronze Inorganic materials 0.000 description 3
- 239000010974 bronze Substances 0.000 description 3
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000156 glass melt Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000005340 laminated glass Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
Abstract
本发明公开了一种隔热节能玻璃及其制备方法，以钨酸、硼源材料、二氧化硅、任意两种或以上的不同碱金属卤化物或碱金属碳酸盐共掺的材料、作为澄清剂的三氧化二锑为原料，所述硼源材料为硼酸或硼砂；在真空升降炉中用还原性气氛、惰性气氛或空气气氛的炉内进行熔制，根据组分的不同选择合适温度熔制一定时间后取出，将玻璃液淬冷成型，然后玻璃片放入石墨坩埚中在退火炉中退火，退火后即可得到隔热节能玻璃。本发明提供的隔热节能玻璃其具有良好的近红外和紫外屏蔽性能，可以降低建筑或车辆内部温度，减少能耗，并且因为功能单元包覆在玻璃中因此具有更长的使用寿命和更好的化学稳定性。
The invention discloses a heat-insulating and energy-saving glass and a preparation method thereof. Tungstic acid, boron source material, silicon dioxide, any two or more different alkali metal halides or alkali metal carbonates are co-doped as a material. The antimony trioxide of the clarifying agent is used as the raw material, and the boron source material is boric acid or borax; it is melted in a vacuum lifting furnace with a reducing atmosphere, an inert atmosphere or an air atmosphere, and the appropriate temperature is selected according to the different components. After melting for a certain period of time, take it out, quench the glass liquid to form, and then put the glass sheet into a graphite crucible for annealing in an annealing furnace. After annealing, heat-insulating energy-saving glass can be obtained. The heat-insulating and energy-saving glass provided by the present invention has good near-infrared and ultraviolet shielding properties, can reduce the internal temperature of buildings or vehicles, reduce energy consumption, and has longer service life and better performance because the functional units are wrapped in the glass. chemical stability.
Description
Technical Field
The invention relates to heat-insulating energy-saving glass and a preparation method thereof, wherein the heat-insulating energy-saving glass has good near-infrared shielding performance and is mainly applied to the field of building or automobile energy conservation.
Background
The continuous increase of population and the rapid development of society lead to the continuous increase of energy consumption and the deterioration of natural environment. In the past decades, energy conservation and environmental protection have received extensive attention, and sustainable development and energy conservation and environmental protection have also become the subjects of the current times. Intense solar radiation in the summer season can cause the temperature inside a building or vehicle to rise beyond human tolerance, and air conditioning is a common option used by people to regulate the temperature inside a building or vehicle. However, the large use of the air conditioner necessarily increases the amount of energy consumption. In recent years, energy consumption applied to buildings accounts for 30-40% of the total energy consumption of the world, and building energy consumption also accounts for a larger proportion of the total energy consumption, and is expected to reach 30% in 2020. Therefore, reducing the building energy consumption plays an important role in energy conservation and emission reduction plans.
The wavelength range of visible light is about 380-780 nm, the solar spectrum mainly comprises 300-2500 nm, and the energy is mainly concentrated in the wavelength range; light in the wavelength range of 780-2500 nm is called near-infrared light, the wavelength energy of the part of the light accounts for about 50% of the total energy of the solar spectrum, the part of the light does not help to human visual imaging, if a material can shield the near-infrared light in an environment requiring a lower temperature, has high visible light transmittance and can shield part of harmful ultraviolet rays, the material can play a role in reducing energy consumption of buildings and vehicles, and a more comfortable environment is provided.
The main structure of the window is inorganic glass, such as soda-lime-silica glass, and the single-layer glass has higher heat conductivity coefficient (1 W.m)-1·K-1) Therefore, heat conduction and exchange are very easyIs easy. The traditional heat insulation glass comprises Low-E glass, ITO or ATO glass, hollow glass, vacuum glass, film-coated glass and the like, and in recent years, electrochromic intelligent windows, aerogels, photovoltaic glass, liquid crystal glass and the like are formed. However, these materials have more or less limiting factors, such as ITO or ATO uses two expensive rare metals, i.e. indium and antimony, the silver layer of Low-E glass needs to be sealed, and after water vapor, sulfide and oxide are corroded, the heat insulation performance is gradually lost, and the appearance becomes dark, discolored and gradually appears a lot of mildew. The electrochromic performance of the electrochromic intelligent window is optimized to a certain extent, but the cycle performance of the electrochromic film is still the development bottleneck of the electrochromic intelligent window, and the problem is not solved so far. While these insulating glasses suffer from high cost, they have limited their commercial use to some extent.
Tungsten oxide is an important transition metal oxide, has abundant reserves, various crystal structures and various chemical components, and has excellent chemical stability. Nanostructured tungsten bronze (M)xWO3M ═ Li, Na, K, Cs, and the like) material can selectively shield ultraviolet and near-infrared light while maintaining high visible light transparency, and has better near-infrared shielding ability than conventional materials. The tungsten oxide energy-saving window is widely researched in recent years, and a thin film structure is prepared by methods such as a sol-gel method, a sputtering method, a solid-phase reaction method and the like, and is combined on a glass substrate to form sandwich laminated glass; or forming tungsten bronze coating or film on the surface of the window glass to achieve the infrared shielding effect. However, there are also limiting factors in the commercial application of energy saving windows of nano tungsten bronze structures: the structure of the coating or the film is not stable enough and is directly exposed in the natural environment, so that the chemical stability of the material is tested, and the service life is limited; the sandwich layer electrochromic intelligent window is high in cost, limited in cycle service life, easy to degrade after being used for a long time in near infrared shielding capacity, and unstable in optical performance in damp-heat and alkaline environments.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects in the prior art, and provides heat-insulating energy-saving glass and a preparation method thereof, and provides low-cost heat-insulating energy-saving glass prepared by a traditional fusion annealing method.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
the heat-insulating energy-saving glass is prepared from tungstic acid, a boron source material, silicon dioxide, any two or more different alkali metal halides or alkali metal carbonates codoped material and antimony trioxide as a clarifying agent, wherein the boron source material is boric acid or borax, and the different alkali metal halides or alkali metal carbonates codoped material is MX and M2CO3The co-doped material is characterized in that M is at least one of Li, Na, K, Rb and Cs, and X is at least one of F, Cl, Br and I;
melting in a furnace with reducing atmosphere, inert atmosphere or air atmosphere in a vacuum lifting furnace, selecting proper temperature according to different components, melting for a certain time, taking out, quenching and forming glass liquid, then putting glass sheets into a graphite crucible, annealing in an annealing furnace, and annealing to obtain the heat-insulating energy-saving glass. The heat-insulating energy-saving glass with high visible wavelength transmittance and good shielding effect in the near-infrared band can be obtained after annealing, and has better stability compared with coated glass.
Preferably, the heat-insulating energy-saving glass comprises the following raw material components in percentage by mass: 0-20% of tungstic acid, 40-50% of boron source material, 10-20% of any two or more different alkali metal halides or alkali metal carbonates codoped, 20-30% of silicon dioxide and 0.4-2.0% of antimony trioxide.
Preferably, the raw materials are mixed and then melted in a reducing or inert atmosphere by changing any one parameter or any combination parameter of parameters of melting temperature, time and alkali metal doping ratio, and the heat-insulating energy-saving glass is obtained according to application requirements. According to the invention, the heat-insulating energy-saving glass with high visible wavelength transmittance and good shielding effect in the near infrared band is obtained according to application requirements.
Preferably, the content of tungstic acid in the raw material is not more than 20% and not 0 in percentage by weight.
Preferably, the glass melting atmosphere is conducted under an air atmosphere.
Preferably, the alkali metal salt employed in any two or more of the different alkali metal halide or alkali metal carbonate co-doped materials is introduced in a plurality of co-doped modes.
The invention relates to a preparation method of heat-insulating energy-saving glass, which comprises the following steps:
a. taking powder raw materials of each component according to a formula, and then fully mixing to obtain an initial mixture;
b. placing the mixture obtained in the step a into a corundum crucible, and placing the corundum crucible into an atmosphere furnace;
c. after the step b is finished, heating the mixture from room temperature to 1100-1600 ℃ at a heating rate of 5-10 ℃/min under the conditions of reducing atmosphere, inert atmosphere or air atmosphere and program temperature control, and preserving heat for 1-3 h to melt the batch materials to form molten glass;
d. cooling the molten glass prepared in the step c to 1000-1200 ℃, and pouring the molten glass into a graphite crucible to quench and form the molten glass;
e. and d, after the quenching step in the step d is finished, putting the quenched solid glass into an annealing furnace at the temperature of 400-550 ℃ for annealing for at least 6 hours, and annealing to obtain a heat-insulating energy-saving glass product. The ultraviolet-visible/near infrared spectrophotometer is used for testing the shielding performance of the heat-insulating energy-saving glass product prepared by the invention on different wave band light waves, and the heat-insulating energy-saving glass with high visible wavelength transmittance and good shielding effect on near infrared wave bands can be obtained after annealing.
Preferably, in the step a, the raw materials comprise the following components in percentage by mass: 0-20% of tungstic acid, 40-50% of boron source material, 10-20% of any two or more different alkali metal halides or alkali metal carbonates codoped, 20-30% of silicon dioxide and 0.4-2.0% of antimony trioxide.
Preferably, in the step a, the raw materials comprise the following components in percentage by mass: 14.95-15.47% of tungstic acid, 47.15-49.20% of boron source material, 12.31-15.31% of any two or more different alkali metal halides or alkali metal carbonates codoped, 20.64-21.37% of silicon dioxide and 1.60-1.61% of antimony trioxide.
Preferably, in the step c, after the step b is completed, the glass melt is formed by heating the batch material from room temperature to 1400-1600 ℃ at a heating rate of 5-10 ℃/min for 2-3 h under the conditions of reducing atmosphere, inert atmosphere or air atmosphere and program temperature control, so that the glass melt is formed.
Preferably, in the step d, the molten glass prepared in the step c is cooled to 1000-1100 ℃, and the molten glass is poured into a graphite crucible to be quenched and formed.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the method has the advantages that the cost of all raw materials is low, the mass production is easy, and the cost is greatly reduced compared with ITO glass, film-pasted glass, electrochromic intelligent windows and the like;
2. the traditional glass melting annealing process is adopted, the process is simple, the material with the infrared shielding performance can be directly added into the glass substrate to form a stable structure, and the stability is stronger than that of the film-coated glass exposed in the environment, so that the service life is longer;
3. the method of the invention selects tungstic acid as glass raw material, and tungsten bronze is generated by the reaction of tungstic acid and alkali metal salt, which can fully exert the near infrared shielding effect. Meanwhile, the adjustment or addition of the glass components has a large adjustment space, and various performances of the glass still have a large rising space through adjustment of various components, optimization of system processes such as temperature atmosphere and the like;
4. the glass has the simple structure of common glass and good processing and hardening performances, can obtain glass with different shapes according to requirements, and has wide application range of energy-saving glass.
Drawings
FIG. 1 is a graph showing the effect of the transmission spectrum performance of the energy-saving glass according to embodiments 1 to 6 of the present invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
example 1
In this embodiment, a method for preparing energy-saving glass includes the following steps:
a. taking the following powder components according to the formula by weight percent: tungstic acid (H)2WO4) 15.30%, boric acid (H)3BO3) 48.63%, silicon dioxide (SiO)2)21.12 percent, 9.13 percent of sodium fluoride (NaF), 4.21 percent of potassium fluoride (KF), and antimony trioxide (Sb)2O3) 1.61%, and then fully mixing for 20-60 min to obtain a mixture;
b. b, placing the mixture obtained in the step a into a corundum crucible, and placing the corundum crucible into an air atmosphere furnace;
c. after the step b is finished, heating the mixture from room temperature to 1400 ℃ at the heating rate of 10 ℃/min by using a silicon-molybdenum rod heating device under the control of a program, and keeping the temperature of the mixture for 2 hours to ensure that the batch forms molten glass in a proper environment, and clarifying and homogenizing the molten glass;
d. c, homogenizing the temperature of the sample in the step c, cooling to 1100 ℃, pouring the molten glass into a graphite crucible, and quenching and forming the molten glass;
e. and d, after the process in the step d is finished, putting the quenched sample into an annealing furnace at 500 ℃ for annealing, and obtaining the heat-insulating energy-saving glass after annealing.
The shielding performance of the heat-insulating energy-saving glass product prepared in the embodiment on different wave bands is tested by an ultraviolet-visible/near-infrared spectrophotometer, and the shielding performance is shown in table 1.
Example 2
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a method for preparing energy-saving glass includes the following steps:
a. taking the following powder components according to the formula by weight percent: tungstic acid (H)2WO4) 15.12% of boric acid (H)3BO3) 48.06%, silicon dioxide (SiO)2)20.87 percent, 6.01 percent of sodium fluoride (NaF), 8.32 percent of potassium fluoride (KF) and antimony trioxide (Sb)2O3)1.60 percent, and then fully mixing for 20-60 min to obtain a mixture;
b. the step is the same as the first embodiment;
c. the step is the same as the first embodiment;
d. c, homogenizing the temperature of the sample in the step c, cooling to 1100 ℃, pouring the molten glass into a graphite crucible, and quenching and forming the molten glass;
e. the procedure is the same as in the first embodiment.
The shielding performance of the heat-insulating energy-saving glass product prepared in the embodiment on different wave bands is tested by an ultraviolet-visible/near-infrared spectrophotometer, and the shielding performance is shown in table 1.
Example 3
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, a method for preparing energy-saving glass includes the following steps:
a. taking the following powder components according to the formula by weight percent: tungstic acid (H)2WO4) 15.12% of boric acid (H)3BO3) 48.06%, silicon dioxide (SiO)2)20.87 percent, 1.86 percent of lithium fluoride (LiF), 12.48 percent of potassium fluoride (KF) and antimony trioxide (Sb)2O3)1.60 percent, and then fully mixing for 20-60 min to obtain a mixture;
b. the step is the same as the first embodiment;
c. the step is the same as the first embodiment;
d. c, homogenizing the temperature of the sample in the step c, cooling to 1050 ℃, pouring the molten glass into a graphite crucible, and quenching and forming the molten glass;
e. the procedure is the same as in the first embodiment.
The shielding performance of the heat-insulating energy-saving glass product prepared in the embodiment on different wave bands is tested by an ultraviolet-visible/near-infrared spectrophotometer, and the shielding performance is shown in table 1.
Example 4
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, a method for preparing energy-saving glass includes the following steps:
a. taking the following powder components according to the formula by weight percent: tungstic acid (H)2WO4) 14.95% of boric acid (H)3BO3) 47.15%, silicon dioxide (SiO)2)20.64 percent of sodium fluoride (NaF), 2.97 percent of potassium fluoride (KF), 12.34 percent of antimony trioxide (Sb)2O3)1.60 percent, and then fully mixing for 20-60 min to obtain a mixture;
b. the step is the same as the first embodiment;
c. the step is the same as the first embodiment;
d. c, homogenizing the temperature of the sample in the step c, cooling to 1000 ℃, and pouring the molten glass into a graphite crucible to quench and form the molten glass;
e. the procedure is the same as in the first embodiment.
The shielding performance of the heat-insulating energy-saving glass product prepared in the embodiment on different wave bands is tested by an ultraviolet-visible/near-infrared spectrophotometer, and the shielding performance is shown in table 1.
Example 5
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, a method for preparing energy-saving glass includes the following steps:
a. taking the components according to the formula, and recording the components in percentage by weight: tungstic acid (H)2WO4) 15.47%, boric acid (H)3BO3) 49.20%, silicon dioxide (SiO)2) 21.37%, sodium fluoride (NaF) 10.31%, lithium fluoride (LiF) 2.00%, antimony trioxide (Sb)2O3) 1.60%, pulverizing to 200-400 meshThen fully mixing for 20-60 min to obtain a mixture;
b. the step is the same as the first embodiment;
c. the step is the same as the first embodiment;
d. the step is the same as the first embodiment;
e. the step is the same as the first embodiment;
the shielding performance of the heat-insulating energy-saving glass product prepared in the embodiment on different wave bands is tested by an ultraviolet-visible/near-infrared spectrophotometer, and the shielding performance is shown in table 1.
Experimental test analysis:
the visible and near infrared transmittance of the heat-insulating energy-saving glass of the embodiment is measured.
1. Test samples: the energy-saving glass prepared in the embodiment 1-6.
2. The test method comprises the following steps: the transmittance was measured using an ultraviolet-visible/near-infrared spectrophotometer manufactured by HITACHI corporation, japan.
3. The test results are shown in Table 1.
TABLE 1 comparison table of shielding performance of heat-insulating energy-saving glass products to different wave bands
| Group of | Visible light transmittance-550 nm (%) | Near Infrared light transmittance-1500 nm (%) |
| Example 1 | 81.8 | 69.6 |
| Example 2 | 81.0 | 68.9 |
| Example 3 | 80.4 | 62.9 |
| Example 4 | 80.4 | 57.3 |
| Example 5 | 63.4 | 7.0 |
| Example 6 | 73.4 | 27.5 |
As can be seen from the test results in Table 1, the scheme for preparing the heat-insulating energy-saving glass by co-doping the alkali metal salt is feasible. As can be seen from comparison of examples 1 to 4, the transmittance at 550nm of visible light is gradually reduced with the temperature reduction, the transmittance at 550nm of visible light is 50.4 to 81.8%, and the shielding effect on near infrared light is also gradually enhanced, the performance is most excellent when NaF and LiF are co-doped, the transmittance at 1500nm is only 7%, and the near infrared transmittance at 550nm is 57.3 to 69.6%. The blue wave cut-off of the energy-saving glass produced by the process is about 380nm basically, referring to fig. 1, the number of the spectral line corresponds to the serial number of the embodiment, the ultraviolet rays are effectively cut off while the near infrared light is shielded, and the harm to human bodies is reduced.
Example 6
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this embodiment, a method for preparing energy-saving glass includes the following steps:
a. taking the following powder components according to the formula by weight percent: tungstic acid (H)2WO4) 15.30%, boric acid (H)3BO3) 48.63%, silicon dioxide (SiO)2)21.12 percent, 9.13 percent of sodium fluoride (NaF), 4.21 percent of potassium fluoride (KF), and antimony trioxide (Sb)2O3) 1.61%, and then fully mixing for 20-60 min to obtain a mixture;
b. b, placing the mixture obtained in the step a into a corundum crucible, and placing the corundum crucible into a reducing or inert atmosphere furnace;
c. after the step b is finished, under the control of a program, heating the mixture from room temperature to 1600 ℃ by using a silicon-molybdenum rod heating device at the heating rate of 10 ℃/min to keep the temperature of the mixture for 3 hours, so that the batch forms molten glass in a proper environment, and the mixture is clarified and homogenized;
d. c, homogenizing the temperature of the sample in the step c, cooling to 1200 ℃, pouring the molten glass into a graphite crucible, and quenching and forming the molten glass;
e. and d, after the process in the step d is finished, putting the quenched sample into an annealing furnace at 400 ℃ for annealing, and obtaining the heat-insulating energy-saving glass after annealing.
In summary, the heat-insulating energy-saving glass of the above embodiment has good near infrared and ultraviolet shielding performance, can reduce the temperature inside a building or a vehicle, reduces energy consumption, and has longer service life and better chemical stability because the functional units are coated in the glass.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.
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