CN108751703B - Heat-resistant and radiation-resistant glass and preparation method thereof - Google Patents
Heat-resistant and radiation-resistant glass and preparation method thereof Download PDFInfo
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- CN108751703B CN108751703B CN201810831838.3A CN201810831838A CN108751703B CN 108751703 B CN108751703 B CN 108751703B CN 201810831838 A CN201810831838 A CN 201810831838A CN 108751703 B CN108751703 B CN 108751703B
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- 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
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- 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
- C03B5/18—Stirring devices; Homogenisation
- C03B5/187—Stirring devices; Homogenisation with moving elements
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Abstract
The invention relates to heat-resistant and radiation-resistant glass and a preparation method thereof, wherein the preparation method comprises the following steps: mixing quartz sand, boric acid, alkali salt and CeO2And Sb2O3Mixing and pretreating to obtain a pretreated material; melting the pretreated material at high temperature, electromagnetically stirring and stirring, forming leaked material, and annealing to obtain heat-resistant and anti-radiation glass; the heat-resistant and radiation-resistant glass comprises the following components in percentage by weight: SiO 22：75‑85％；B2O3：11‑20％；R2O: 1-5% of R2O is Na2O and/or K2O；CeO2：2‑5％；Sb2O3: 0.2 to 0.6 percent. The heat-resistant and radiation-resistant glass has low expansion coefficient and better thermal shock resistance, and is suitable for outer space tungsten group packaging windows.
Description
Technical Field
The invention relates to the technical field of special glass preparation, in particular to heat-resistant and radiation-resistant glass and a preparation method thereof.
Background
The glass can generate color centers under the radiation of high-energy rays, and the transmittance of the glass is reduced. In order to improve the radiation resistance of the glass, it is usual to incorporate a small amount of a valence-altering oxide, such as CeO, into the base glass2、TiO2、Fe2O3And Mn2O3And the valence state change of the valence-variable ions is utilized to absorb high-energy rays, so that the glass body is inhibited from generating no color center, and the radiation-resistant stability of the glass is improved.
At present, there are two main types of radiation-resistant glasses reported: one is the anti-radiation quartz glass and the other is,the quartz glass is doped with trace (less than or equal to 1 wt.%) of high-purity CeO by a special process2Expansion coefficient of not more than 5.8 x 10-7The product has good thermal shock resistance, can be used for observation windows, sight glasses, display panels and the like of spacecrafts, but is limited to complex preparation process and CeO2The doping amount is low, and the radiation resistance of the glass needs to be improved; the second is radiation-resistant borosilicate glass which is prepared by doping a small amount of CeO into a borosilicate glass matrix2、TiO2And Fe2O3Etc., the coefficient of expansion is (60-90). times.10-7The temperature per DEG C is mainly used for a cover plate of the space solar cell to prevent the radiation damage of the space high-energy rays to the solar cell. The thermal shock resistance of the radiation resistant glass is determined by the expansion coefficient of the base glass, which can be adjusted according to the composition change of the base glass.
In the optimization of the glass composition, it is also necessary to consider the incorporation of CeO2The influence on the coloring of the matrix glass, if the coloring of the glass is too heavy, the transmittance is low, and the application value of the glass is lost. Glass coloring is mainly composed of a matrix and CeO2Content, melting atmosphere, etc. Wherein the matrix composition has a more complex effect on the glass coloration, in general, B2O3The higher the content, the more severe the glass is colored; CeO (CeO)2The higher the content, the greater the radiation resistance of the glass, but the more severe the coloration of the glass. Therefore, on the premise of ensuring the radiation resistance, the expansion coefficient of the glass needs to be adjusted, and the thermal shock resistance is optimized, so as to expand the application field of the radiation-resistant glass.
Disclosure of Invention
The invention mainly aims to provide novel heat-resistant and radiation-resistant glass and a preparation method thereof, and aims to solve the technical problem that the heat-resistant and radiation-resistant glass has the characteristics of low expansion coefficient, good radiation resistance, thermal shock resistance and the like, and can be used for outer space tungsten group packaging windows, so that the glass is more practical.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The invention provides a preparation method of heat-resistant and radiation-resistant glass, which comprises the following steps:
mixing quartz sand, boric acid, alkali salt and CeO2And Sb2O3Mixing and pretreating to obtain a pretreated material;
melting the pretreated material at high temperature, electromagnetically stirring and stirring, forming leaked material, and annealing to obtain heat-resistant and anti-radiation glass;
the heat-resistant and radiation-resistant glass comprises the following components in percentage by weight:
SiO2：75-85％；
B2O3：11-20％；
R2o: 1-5% of R2O is Na2O and/or K2O；
CeO2：2-5％；
Sb2O3：0.2-0.6％。
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the method for manufacturing heat-resistant and radiation-resistant glass, the alkali salt is at least one of sodium carbonate, sodium nitrate, potassium carbonate and potassium nitrate.
Preferably, in the preparation method of the heat-resistant and radiation-resistant glass, the pretreatment temperature is 750-.
Preferably, in the preparation method of the heat-resistant and radiation-resistant glass, the high-temperature melting temperature is 1620-.
Preferably, in the preparation method of the heat-resistant and radiation-resistant glass, the high-temperature melting and the electromagnetic flipping are generated by medium-frequency induction, and the frequency of the medium-frequency induction is 900-1200 Hz.
Preferably, in the method for preparing the heat-resistant and radiation-resistant glass, the stirring speed is 20-60rpm, and the stirring time is 3-5 h.
Preferably, in the method for preparing the heat-resistant and radiation-resistant glass, the high-temperature melting is protected by an atmosphere; the atmosphere is mixed gas of nitrogen and air, wherein the volume ratio of the nitrogen to the air is 0.2-0.6.
Preferably, in the method for preparing the heat-resistant and radiation-resistant glass, the temperature for forming the leaking material is 1420-1480 ℃.
Preferably, the preparation method of the heat-resistant and radiation-resistant glass comprises the following steps of:
SiO2：78-82％；
B2O3：15-18％；
R2o: 2-4% of which R2O is Na2O and/or K2O；
CeO2：3-4％；
Sb2O3：0.3-0.5％。
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The heat-resistant and radiation-resistant glass provided by the invention is prepared by the method; the thermal-resistant radiation-resistant glass has an expansion coefficient of less than or equal to 33 multiplied by 10-7/℃。
By the technical scheme, the heat-resistant and radiation-resistant glass and the preparation method thereof at least have the following advantages:
1) the heat-resistant and radiation-resistant glass has low expansion coefficient (less than or equal to 33 multiplied by 10)-7/° c), has better thermal shock resistance, and is suitable for the outer space tungsten group packaging window.
2) According to the preparation method of the heat-resistant and radiation-resistant glass, the electromagnetic stirring effect generated by the medium-frequency induction heating system is utilized, so that the problem of homogenization of high-viscosity glass melt is effectively solved; adjusting Ce in glass by controlling melting atmosphere3+/Ce4+The glass has both radiation resistance and transmittance.
3) The preparation method of the heat-resistant and radiation-resistant glass has the advantages of short flow, simple operation and easy replacement of glass varieties.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to the embodiments, structures, features and effects of the heat-resistant and radiation-resistant glass and the preparation method thereof according to the present invention in combination with the preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
One embodiment of the present invention provides a method for preparing heat-resistant and radiation-resistant glass, which comprises:
mixing quartz sand, boric acid, alkali salt and CeO2And Sb2O3Mixing and pretreating to obtain a pretreated material;
melting the pretreated material at high temperature, electromagnetically stirring and stirring, forming leaked material, and annealing to obtain heat-resistant and anti-radiation glass;
the heat-resistant and radiation-resistant glass comprises the following components in percentage by weight:
SiO2：75-85％；
B2O3：11-20％；
R2o: 1-5% of R2O is Na2O and/or K2O；
CeO2：2-5％；
Sb2O3：0.2-0.6％。
Preferably, the alkali salt is at least one of sodium carbonate, sodium nitrate, potassium carbonate and potassium nitrate.
Preferably, the temperature of the pretreatment is 750-. Pretreating H in the glass raw material2O、CO2The gas is discharged, which is helpful for controlling the melting atmosphere.
Preferably, the high-temperature melting is carried out in a zirconium dispersion Pt crucible, and medium-frequency induction heating is adopted, wherein the melting temperature is 1620-. In the melting process, the glass liquid is homogenized up and down due to the electromagnetic turning generated by medium-frequency induction; meanwhile, a zirconium dispersion Pt stirrer is used for forcibly stirring the pretreated material, so that bubbles and stripes are eliminated, and glass homogenization is realized. The medium frequency induction frequency is 900-1200Hz, the stirring speed is 20-60rpm, and the stirring time is 3-5 h.
Preferably, in order to ensure that the glass has good radiation resistance, atmosphere protection is adopted for high-temperature melting; the atmosphere is mixed gas of nitrogen and air, wherein the volume ratio of the nitrogen to the air is 0.2-0.6. According to the content of CeO in the glass component2The content is different, and the mixed protective gas with different ratios is selected.
Preferably, the material leakage pipe is heated by a Pt electrode, and the temperature for forming the material leakage is 1420-1480 ℃.
Preferably, the heat-resistant and radiation-resistant glass comprises the following components in percentage by weight:
SiO2：78-82％；
B2O3：15-18％；
R2o: 2-4% of which R2O is Na2O and/or K2O；
CeO2：3-4％；
Sb2O3：0.3-0.5％。
Another embodiment of the present invention provides a heat-resistant and radiation-resistant glass, which is prepared by the above method; the thermal-resistant radiation-resistant glass has an expansion coefficient of less than or equal to 33 multiplied by 10-7/℃。
Example 1
One embodiment of the present invention provides a method for preparing heat-resistant and radiation-resistant glass, which comprises:
mixing high-purity quartz sand, boric acid, sodium carbonate and CeO according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 3h at 750 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, performing high-temperature melting at 1620 ℃ by adopting medium-frequency induction heating, electromagnetically stirring, and introducing N2Atmosphere preservation with 0.3/air ratio of mixed gasProtecting; mechanically stirring the molten glass by adopting a double-blade stirrer, wherein the rotating speed of blades is 40rpm, and the time is 3 hours; and cooling to 1420 ℃, performing leaking molding, and annealing to obtain the heat-resistant and radiation-resistant glass.
Another embodiment of the present invention provides a heat and radiation resistant glass prepared by the method of embodiment 1; the composition of the heat and radiation resistant glass of example 1 is shown in table 1.
Example 2
One embodiment of the present invention provides a method for preparing heat-resistant and radiation-resistant glass, which comprises:
high-purity quartz sand, boric acid, sodium carbonate, potassium nitrate and CeO are mixed according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 2h at 800 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, performing high-temperature melting at 1620 ℃ by adopting medium-frequency induction heating, electromagnetically stirring, and introducing N2Atmosphere protection is carried out on the mixed gas with the air ratio of 0.2; mechanically stirring the molten glass by adopting a double-blade stirrer, wherein the rotating speed of blades is 60rpm, and the time is 5 hours; and cooling to 1420 ℃, performing leaking molding, and annealing to obtain the heat-resistant and radiation-resistant glass.
Another embodiment of the present invention provides a heat and radiation resistant glass prepared by the method of embodiment 2; the composition of the heat and radiation resistant glass of example 2 is shown in table 1.
Example 3
One embodiment of the present invention provides a method for preparing heat-resistant and radiation-resistant glass, which comprises:
high-purity quartz sand, boric acid, sodium nitrate, potassium nitrate and CeO are mixed according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 2h at 850 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, performing high-temperature melting at 1630 ℃ by adopting medium-frequency induction heating, electromagnetically stirring, and introducing N2Atmosphere protection is carried out on the mixed gas with the air ratio of 0.4; mechanical stirring of glass liquid by double-blade stirrerStirring at a paddle rotation speed of 20rpm for 5 h; and cooling to 1450 ℃, performing material leakage forming, and annealing to obtain the heat-resistant and radiation-resistant glass.
Another embodiment of the present invention provides a heat and radiation resistant glass prepared by the method of embodiment 3; the composition of the heat and radiation resistant glass of example 3 is shown in table 1.
Example 4
One embodiment of the present invention provides a method for preparing heat-resistant and radiation-resistant glass, which comprises:
mixing high-purity quartz sand, boric acid, sodium nitrate and CeO according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 2h at 900 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, adopting medium-frequency induction heating to carry out high-temperature melting at 1650 ℃, electromagnetically turning, and introducing N2Atmosphere protection is carried out on the mixed gas with the air ratio of 0.4; mechanically stirring the molten glass by adopting a double-blade stirrer, wherein the rotating speed of blades is 50rpm, and the time is 4 hours; and cooling to 1460 ℃ for material leakage forming, and annealing to obtain the heat-resistant and radiation-resistant glass.
Another embodiment of the present invention provides a heat and radiation resistant glass prepared by the method of embodiment 4; the composition of the heat and radiation resistant glass of example 4 is shown in table 1.
Example 5
One embodiment of the present invention provides a method for preparing heat-resistant and radiation-resistant glass, which comprises:
mixing high-purity quartz sand, boric acid, sodium nitrate, potassium carbonate and CeO according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 1h at 900 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, adopting medium-frequency induction heating to carry out high-temperature melting at 1660 ℃, electromagnetically turning, and introducing N2Atmosphere protection is carried out on the mixed gas with the air ratio of 0.6; mechanically stirring the molten glass by adopting a double-blade stirrer, wherein the rotating speed of blades is 40rpm, and the time is 3 hours; cooling to 1460 deg.C for leakingAnd forming and annealing to obtain the heat-resistant and radiation-resistant glass.
Another embodiment of the present invention provides a heat and radiation resistant glass prepared by the method of embodiment 5; the composition of the heat and radiation resistant glass of example 5 is shown in table 1.
Example 6
One embodiment of the present invention provides a method for preparing heat-resistant and radiation-resistant glass, which comprises:
mixing high-purity quartz sand, boric acid, sodium carbonate, potassium carbonate and CeO according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 3h at 900 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, adopting medium-frequency induction heating to carry out high-temperature melting at 1680 ℃, electromagnetically turning, and introducing N2Atmosphere protection is carried out on the mixed gas with the air ratio of 0.2; mechanically stirring the molten glass by adopting a double-blade stirrer, wherein the rotating speed of blades is 50rpm, and the time is 3 hours; and cooling to 1480 ℃ for material leakage molding, and annealing to obtain the heat-resistant and anti-radiation glass.
Another embodiment of the present invention provides a heat and radiation resistant glass prepared by the method of embodiment 6; the composition of the heat and radiation resistant glass of example 6 is shown in table 1.
Comparative example 1
A comparative example of the present invention proposes a method for preparing a heat-resistant and radiation-resistant glass, which comprises:
mixing high-purity quartz sand, boric acid, sodium carbonate, potassium carbonate and CeO according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 3h at 900 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, heating to 1680 ℃ for high-temperature melting, and introducing N2Atmosphere protection is carried out on the mixed gas with the air ratio of 0.2; mechanically stirring the molten glass by adopting a double-blade stirrer, wherein the rotating speed of blades is 50rpm, and the time is 3 hours; and cooling to 1480 ℃ for material leakage molding, and annealing to obtain the heat-resistant and anti-radiation glass.
Another comparative example of the present invention proposes a heat-resistant and radiation-resistant glass prepared by the method of comparative example 1; the composition of the heat and radiation resistant glass of comparative example 1 is shown in table 1.
Comparative example 2
A comparative example of the present invention proposes a method for preparing a heat-resistant and radiation-resistant glass, which comprises:
mixing high-purity quartz sand, boric acid, sodium nitrate and CeO according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 3h at 900 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, heating to 1680 ℃ for high-temperature melting, and introducing N2Atmosphere protection is carried out on the mixed gas with the air ratio of 0.2; mechanically stirring the molten glass by adopting a double-blade stirrer, wherein the rotating speed of blades is 50rpm, and the time is 3 hours; cooling to 1480 ℃ for material leakage molding, and annealing to obtain the final product.
Comparative example 3
A comparative example of the present invention proposes a method for preparing a heat-resistant and radiation-resistant glass, which comprises:
mixing high-purity quartz sand, boric acid, sodium nitrate, potassium carbonate and CeO according to the proportion required in Table 12And Sb2O3Weighing and mixing, pretreating for 3h at 900 ℃, and cooling to obtain a pretreatment material;
putting the pretreated material into a zirconium dispersion Pt crucible, heating to 1680 ℃ for high-temperature melting, and introducing N2Atmosphere protection is carried out on the mixed gas with the air ratio of 0.2; mechanically stirring the molten glass by adopting a double-blade stirrer, wherein the rotating speed of blades is 50rpm, and the time is 3 hours; and cooling to 1480 ℃ for material leakage molding, and annealing to obtain the heat-resistant and anti-radiation glass.
Another comparative example of the present invention proposes a heat-resistant and radiation-resistant glass prepared by the method of comparative example 3; the composition of the heat and radiation resistant glass of comparative example 3 is shown in table 1.
The heat and radiation resistant glasses of examples 1 to 6 and comparative examples 1 and 3 were processed to 20X 1mm, and after polishing, the transmittance at 500 and 800nm was measured using a spectrophotometer and the average value was determined.
By using60Co (gamma ray) irradiation source the 20X 1mm glass sheets of examples 1 to 6 and comparative examples 1 and 3 were subjected to high energy irradiation with a total dose of 20krad, and then the transmittance T at 780nm of the glass sheets before and after the irradiation was measuredFront sideAnd TRear endThe irradiation attenuation rate s of the glass is calculated by the following formula:
s＝(Tfront side-TRear end)×100％/TFront side
According to GB/T7962.16-2010 colorless optical glass test method part 16: linear expansion coefficient, transition temperature and sag temperature of the test glass; the thermal shock resistance temperature difference of the glass is tested according to SJ/T11037-96 electronic glass thermal stability test method. The heat and radiation resistant glass properties of examples 1 to 6 and comparative examples 1 and 3 are shown in Table 1.
Table 1 composition (wt.%) and main properties of the glasses of the examples
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (8)
1. A preparation method of heat-resistant and radiation-resistant glass is characterized by comprising the following steps:
mixing quartz sand, boric acid, alkali salt and CeO2And Sb2O3Mixing and pretreating to obtain a pretreated material;
melting the pretreated material at high temperature, electromagnetically stirring and stirring, forming leaked material, and annealing to obtain heat-resistant and anti-radiation glass; the high-temperature melting and the electromagnetic turning are generated through medium-frequency induction; the high-temperature melting adopts atmosphere protection; the atmosphere is mixed gas of nitrogen and air, wherein the volume ratio of the nitrogen to the air is 0.2-0.6;
the heat-resistant and radiation-resistant glass comprises the following components in percentage by weight:
SiO2：80-85％；
B2O3：11-12.6％；
R2o: 1.5-2%, wherein R2O is Na2O and/or K2O；
CeO2：2-5％；
Sb2O3：0.4-0.6％。
2. The method of claim 1, wherein the alkali salt is at least one of sodium carbonate, sodium nitrate, potassium carbonate, and potassium nitrate.
3. The method for preparing heat-resistant and radiation-resistant glass according to claim 1, wherein the temperature of the pretreatment is 750-900 ℃ and the pretreatment time is 1-3 h.
4. The method as claimed in claim 1, wherein the melting temperature is 1620 ℃ and 1680 ℃ and the melting time is 5-8 h.
5. The method as claimed in claim 1, wherein the frequency of the MF induction is 900-1200 Hz.
6. The method for preparing heat and radiation resistant glass according to claim 1, wherein the stirring speed is 20-60rpm and the stirring time is 3-5 h.
7. The method as claimed in claim 1, wherein the temperature of the frit molding is 1420-1480 ℃.
8. A heat-resistant and radiation-resistant glass prepared by the method according to any one of claims 1 to 7;the thermal-resistant radiation-resistant glass has an expansion coefficient less than or equal to 29 multiplied by 10-7/℃。
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