CN115286262A - Preparation method and preparation device of reinforced electronic microcrystalline glass - Google Patents
Preparation method and preparation device of reinforced electronic microcrystalline glass Download PDFInfo
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- CN115286262A CN115286262A CN202211100280.4A CN202211100280A CN115286262A CN 115286262 A CN115286262 A CN 115286262A CN 202211100280 A CN202211100280 A CN 202211100280A CN 115286262 A CN115286262 A CN 115286262A
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- 239000011521 glass Substances 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005728 strengthening Methods 0.000 claims abstract description 134
- 150000003839 salts Chemical class 0.000 claims abstract description 80
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000243 solution Substances 0.000 claims abstract description 68
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 34
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 34
- 239000011259 mixed solution Substances 0.000 claims abstract description 28
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 27
- 238000000137 annealing Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 18
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 18
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 18
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 18
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 18
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 229910001923 silver oxide Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 description 13
- 238000002156 mixing Methods 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 7
- 238000002791 soaking Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 239000003788 bath preparation Substances 0.000 description 1
- 238000003426 chemical strengthening reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000006058 strengthened glass Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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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
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
- C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention provides a preparation method and a preparation device of reinforced electronic glass ceramics, wherein the method comprises the following steps: heating a mixed solution of sodium nitrate and potassium nitrate to a first strengthening temperature to obtain a first salt bath solution; heating the mixed solution of potassium nitrate and potassium sulfate to a second strengthening temperature to obtain a second salt bath solution; heating the glass to a first strengthening temperature; immersing the glass heated to the first strengthening temperature into a first salt bath solution to carry out first strengthening treatment on the glass; putting the glass subjected to the first strengthening treatment into the steam of a second salt bath solution for second strengthening treatment; the temperature of the glass on which the second strengthening treatment is completed is lowered to room temperature to perform annealing treatment. The method solves the problem that the strength and the depth of the pressure stress layer of the glass can not be met simultaneously, and improves the performance and the quality of products.
Description
Technical Field
The disclosure relates to the technical field of microcrystalline glass, in particular to a preparation method and a preparation device of reinforced electronic microcrystalline glass.
Background
With the development of modern science and technology, the updating speed of glass materials is accelerated, the requirement on light weight is high, and the application requirement is more rigorous. For example, electronic glass application has higher requirements on the aspects of hardness, impact strength, friction resistance, falling resistance and the like. In view of the current situation, the microcrystalline glass with the characteristics of high mechanical strength, wear resistance and the like is more widely applied. The microcrystal glass is also called glass ceramic, and is a composite material containing a crystal phase and a glass phase and prepared by nucleating and crystallizing glass. By means of the mechanical properties of the microcrystalline phase material, the average hardness, the breaking strength, the fracture toughness and other properties of the glass can be improved, so that the scratch resistance, the impact strength, the falling resistance and other properties of the glass are adjusted.
The microcrystalline glass can be strengthened by a chemical toughening method, namely an ion exchange strengthening method. After ion exchange, a compressive stress layer with certain depth and strength is generated on the surface of the microcrystalline glass, so that the mechanical property of the microcrystalline glass is obviously enhanced. At present, the stress layer strength is basically enhanced by adopting a method for improving the stress layer strength, but if the depth of the microcrack exceeds the depth of the surface stress layer, the microcrack expands to directly cross the overpressure stress layer. Therefore, not only the stress layer strength but also the depth of the stress layer must be considered in the chemical strengthening of the glass ceramics. The exchange time is properly prolonged and the exchange temperature is increased to obtain larger exchange layer depth, but the excessive exchange temperature and the excessive exchange time can cause stress relaxation and reduce the surface stress; in order to obtain high surface stress, the exchange temperature is lowered, which in turn results in an insufficient depth of the stress layer.
Based on this, there is still a need for improvement in the art.
Disclosure of Invention
One technical problem to be solved by the present disclosure is: the method for preparing the strengthened electronic glass ceramics solves the problem that the strength and the depth of a pressure stress layer can not be met simultaneously by performing two-stage strengthening treatment on the glass in the steam of the first salt bath solution and the second salt bath solution, and improves the performance and the quality of products.
In order to solve the above technical problem, an embodiment of the present disclosure provides a method for preparing a strengthened electronic glass-ceramic, including: heating a mixed solution of sodium nitrate and potassium nitrate to a first strengthening temperature to obtain a first salt bath solution; heating the mixed solution of potassium nitrate and potassium sulfate to a second strengthening temperature to obtain a second salt bath solution; heating the glass to a first strengthening temperature; immersing glass heated to a first strengthening temperature into a first salt bath to perform first strengthening treatment on the glass; and putting the glass subjected to the first strengthening treatment into the steam of the second salt bath solution to carry out second strengthening treatment. The temperature of the glass on which the second strengthening treatment is completed is lowered to room temperature to perform an annealing treatment.
In some embodiments, the first salt bath has 50 to 90wt% and 10 to 50wt% sodium nitrate and potassium nitrate, respectively, and the second salt bath has 90 to 99wt% and 1 to 10wt% potassium nitrate and potassium sulfate, respectively.
In some embodiments, the first strengthening temperature is 400-450 ℃ and the second strengthening temperature is 500-550 ℃.
In some embodiments, heating the mixed solution of sodium nitrate and potassium nitrate to the first strengthening temperature, resulting in the first salt bath comprises: heating the mixed solution of sodium nitrate and potassium nitrate to a first strengthening temperature, and then preserving heat for 3 hours to obtain a first salt bath solution;
heating the mixed solution of potassium nitrate and potassium sulfate to a second strengthening temperature to obtain a second salt bath solution, which comprises the following steps: and heating the mixed solution of potassium nitrate and potassium sulfate to a second strengthening temperature, and then preserving the heat for 3 hours to obtain a second salt bath solution.
In some embodiments, immersing the glass heated to the first strengthening temperature in the first salt bath, and subjecting the glass to a first strengthening treatment includes: heating the glass to a first strengthening temperature, and then carrying out first strengthening treatment after heat preservation for 1-4.
In some embodiments, the time of the first strengthening treatment is 24-48 h, and the time of the second strengthening treatment is 12-24 h.
In some embodiments, the annealing time is 4 to 24 hours.
In some embodiments, the potassium nitrate, sodium nitrate, and potassium sulfate each have less than 50ppm of iron oxide, copper oxide, silver oxide, and titanium oxide.
In addition, the embodiment of the disclosure also provides a preparation device adopting the preparation method of the strengthened electronic glass ceramics, which includes a first closed container, a second closed container and a basket tool, wherein the first closed container is communicated with the second closed container, the first salt bath solution is placed in the first closed container, the second salt bath solution is placed in the second closed container, the first closed container is provided with an eccentric opening, the basket tool is fixed with the glass to be strengthened, and the basket tool is placed in the first closed container through the eccentric opening.
In some embodiments, the device further comprises a vent pipe provided with a vent valve, one end of the vent pipe penetrates through the eccentric opening to be communicated with the first closed container, and the other end of the vent pipe is communicated with the second closed container
According to the technical scheme, the preparation method and the preparation device of the strengthened electronic glass ceramics provided by the disclosure solve the problem that the strength and the depth of a compressive stress layer cannot be simultaneously met by two-stage strengthening treatment in the steam of the first salt bath solution and the second salt bath solution; through the steam treatment of the second salt bath, the salt spray strengthening ions are smaller, the treatment temperature field is uniform, the stress layer of the product is deeper, and the stress distribution is more uniform.
Drawings
In order to more clearly illustrate the embodiments of the present disclosure or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present disclosure, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of a method of making disclosed in embodiments of the present disclosure;
FIG. 2 is a schematic view of a first containment vessel disclosed in an embodiment of the disclosure;
FIG. 3 is a schematic view of a combination of a first closed container and a second closed container disclosed in the embodiment of the disclosure.
Description of reference numerals:
1. a first salt bath; 2. a second salt bath solution; 3. a first closed container; 4. a second closed container; 5. a basket tool; 6. an eccentric opening; 7. a breather pipe; 8. a vent valve; 9. and (7) sealing the cover.
Detailed Description
Embodiments of the present disclosure are described in further detail below with reference to the drawings and examples. The following detailed description of the embodiments and the accompanying drawings are included to illustrate the principles of the disclosure, but are not intended to limit the scope of the disclosure, which may be embodied in many different forms and not limited to the specific embodiments disclosed herein, but include all technical solutions falling within the scope of the claims.
These embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. It should be noted that: the relative arrangement of the components and steps, the composition of materials, numerical expressions and numerical values set forth in these embodiments are to be construed as merely illustrative, and not restrictive, unless specifically stated otherwise.
It is noted that in the description of the present disclosure, unless otherwise indicated, "a plurality" means greater than or equal to two; the terms "upper," "lower," "left," "right," "inner," "outer," and the like, indicate an orientation or positional relationship merely to facilitate the description of the disclosure and to simplify the description, and do not indicate or imply that the referenced devices or elements must be in a particular orientation, constructed and operated in a particular orientation, and therefore should not be construed as limiting the disclosure. When the absolute position of the object being described changes, the relative positional relationship may also change accordingly.
Moreover, the use of "first," "second," and similar words throughout this disclosure is not intended to imply any order, quantity, or importance, but rather merely to distinguish one element from another. "vertical" is not strictly vertical, but is within the tolerance of the error. "parallel" is not strictly parallel but within the tolerance of the error. The word "comprising" or "comprises", and the like, means that the element preceding the word covers the element listed after the word, and does not exclude the possibility that other elements are also covered.
It should also be noted that, in the description of the present disclosure, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; may be directly connected or indirectly connected through an intermediate. The specific meaning of the above terms in the present disclosure can be understood as appropriate to one of ordinary skill in the art. When a particular device is described as being between a first device and a second device, intervening devices may or may not be present between the particular device and the first device or the second device.
All terms used in the present disclosure have the same meaning as understood by one of ordinary skill in the art to which the present disclosure belongs, unless otherwise specifically defined. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate.
The invention discloses a preparation method of reinforced electronic glass ceramics, which comprises the following specific steps as shown in figures 1 and 3: step one, salt bath preparation: preparing a first salt bath solution 1, namely heating a mixed solution of sodium nitrate and potassium nitrate to a first strengthening temperature to obtain a first salt bath solution 1; preparing a second salt bath solution 2, namely heating a mixed solution of potassium nitrate and potassium sulfate to a second strengthening temperature to obtain the second salt bath solution 2; step two, strengthening treatment: heating the glass to a first strengthening temperature; a first strengthening treatment of immersing the glass heated to the first strengthening temperature in the first salt bath 1 to perform the first strengthening treatment on the glass; and a second strengthening treatment, namely putting the glass subjected to the first strengthening treatment into the steam of the second salt bath solution 2 for second strengthening treatment. And thirdly, annealing treatment, namely reducing the temperature of the glass subjected to the second strengthening treatment to room temperature. The preparation method solves the problem that the strength and the depth of a pressure stress layer can not be simultaneously met by two-stage strengthening treatment in the steam of the first salt bath solution 1 and the second salt bath solution 2; through the steam treatment of the second salt bath liquid 2, the salt spray strengthening ions are smaller, the treatment temperature field is uniform, the stress layer of the product is deeper, and the stress distribution is more uniform. The reinforced electronic glass-ceramic prepared by the method has the advantages of high hardness, high strength, high toughness, excellent impact resistance, excellent chemical stability, high light transmittance and fine crystals; and the preparation process has simple operation process and low cost and is suitable for industrial production.
Example 1, mixing 90wt% of sodium nitrate and 10wt% of potassium nitrate, heating the mixed solution for two hours to a first strengthening temperature, wherein the first strengthening temperature is 440 ℃, and keeping the temperature for three hours to obtain a first salt bath solution 1; weighing 96wt% of potassium nitrate and 4wt% of potassium sulfate according to the mass percentage, mixing, heating the mixed solution to a second strengthening temperature within two hours, wherein the second strengthening temperature is 550 ℃, and preserving the heat for three hours to obtain a second salt bath solution 2; putting the glass into an annealing furnace, heating the glass to a first strengthening temperature of 440 ℃ within one hour, preserving the heat for three hours, and then soaking the glass into the prepared first salt bath solution 1 for first strengthening treatment, wherein the time of the first strengthening treatment is 24 hours; putting the glass subjected to the first strengthening treatment into the steam of the prepared second salt bath solution 2 for second strengthening treatment, wherein the time of the second strengthening treatment is 16h; and finally, placing the glass subjected to the secondary strengthening treatment into an annealing furnace for cooling, cooling the glass to room temperature after 8 hours in the annealing furnace, taking out the glass, and cleaning the glass to obtain the strengthened electronic glass-ceramic.
Embodiment 2, mixing 80wt% of sodium nitrate and 20wt% of potassium nitrate, heating the mixed solution to a first strengthening temperature for two hours, wherein the first strengthening temperature is 420 ℃, and keeping the temperature for three hours to obtain a first salt bath solution 1; weighing 98wt% of potassium nitrate and 2wt% of potassium sulfate according to the mass percentage, mixing, heating the mixed solution to a second strengthening temperature for two hours, keeping the second strengthening temperature at 530 ℃, and preserving the heat for three hours to obtain a second salt bath solution 2; putting the glass into an annealing furnace, heating the glass to a first strengthening temperature of 420 ℃ within one hour, preserving the heat for three hours, and then soaking the glass into the prepared first salt bath solution 1 for first strengthening treatment, wherein the time of the first strengthening treatment is 28 hours; putting the glass subjected to the first strengthening treatment into the steam of the prepared second salt bath solution 2 for second strengthening treatment, wherein the time of the second strengthening treatment is 18h; and finally, putting the glass subjected to the secondary strengthening treatment into an annealing furnace for cooling, cooling the glass to room temperature in the annealing furnace for 10 hours, taking out the glass, and cleaning the glass to obtain the strengthened electronic glass ceramics.
Example 3, mixing 70wt% of sodium nitrate and 30wt% of potassium nitrate, heating the mixed solution for two hours to a first strengthening temperature, wherein the first strengthening temperature is 400 ℃, and keeping the temperature for three hours to obtain a first salt bath solution 1; weighing 96wt% of potassium nitrate and 4wt% of potassium sulfate according to the mass percentage, mixing, heating the mixed solution to a second strengthening temperature within two hours, wherein the second strengthening temperature is 500 ℃, and preserving the heat for three hours to obtain a second salt bath solution 2; putting the glass into an annealing furnace, heating the glass to a first strengthening temperature of 400 ℃ within one hour, preserving the heat for four hours, and then soaking the glass into the prepared first salt bath solution 1 for first strengthening treatment, wherein the time of the first strengthening treatment is 46 hours; putting the glass subjected to the first strengthening treatment into the steam of the prepared second salt bath solution 2 for second strengthening treatment, wherein the time of the second strengthening treatment is 24 hours; and finally, putting the glass subjected to the secondary strengthening treatment into an annealing furnace for cooling, cooling the glass to room temperature in the annealing furnace for 20 hours, taking out the glass, and cleaning the glass to obtain the strengthened electronic glass ceramics.
Example 4, mixing 85wt% of sodium nitrate and 15wt% of potassium nitrate, heating the mixed solution for two hours to a first strengthening temperature, wherein the first strengthening temperature is 430 ℃, and keeping the temperature for three hours to obtain a first salt bath solution 1; weighing 95wt% of potassium nitrate and 5wt% of potassium sulfate according to the mass percentage, mixing, heating the mixed solution to a second strengthening temperature within two hours, keeping the temperature at 530 ℃ for three hours to obtain a second salt bath solution 2; putting the glass into an annealing furnace, heating the glass to a first strengthening temperature (430 ℃) within one hour, preserving the heat for three hours, and then soaking the glass into the prepared first salt bath solution 1 for first strengthening treatment, wherein the time of the first strengthening treatment is 36 hours; putting the glass subjected to the first strengthening treatment into the steam of the prepared second salt bath solution 2 for second strengthening treatment, wherein the time of the second strengthening treatment is 18h; and finally, placing the glass subjected to the secondary strengthening treatment into an annealing furnace for cooling, cooling the glass in the annealing furnace to room temperature after 20 hours, taking out the glass, and cleaning the glass to obtain the strengthened electronic glass ceramics.
Example 5, mixing 60wt% of sodium nitrate and 40wt% of potassium nitrate, heating the mixed solution for two hours to a first strengthening temperature, wherein the first strengthening temperature is 440 ℃, and keeping the temperature for three hours to obtain a first salt bath solution 1; weighing 94wt% of potassium nitrate and 6wt% of potassium sulfate according to the mass percentage, mixing, heating the mixed solution to a second strengthening temperature for two hours, keeping the second strengthening temperature at 530 ℃, and preserving the heat for three hours to obtain a second salt bath solution 2; putting glass into an annealing furnace, heating the glass to a first strengthening temperature (440 ℃) after one hour, preserving the heat for three hours, and then soaking the glass into the prepared first salt bath solution 1 for first strengthening treatment, wherein the time of the first strengthening treatment is 40 hours; putting the glass subjected to the first strengthening treatment into the steam of the prepared second salt bath solution 2 for second strengthening treatment, wherein the time of the second strengthening treatment is 20h; and finally, placing the glass subjected to the secondary strengthening treatment into an annealing furnace for cooling, cooling the glass in the annealing furnace to room temperature after 20 hours, taking out the glass, and cleaning the glass to obtain the strengthened electronic glass ceramics.
Example 6, mixing 50wt% of sodium nitrate and 50wt% of potassium nitrate, heating the mixed solution for two hours to a first strengthening temperature, wherein the first strengthening temperature is 400 ℃, and keeping the temperature for three hours to obtain a first salt bath solution 1; weighing 90wt% of potassium nitrate and 10wt% of potassium sulfate according to the mass percentage, mixing, heating the mixed solution to a second strengthening temperature within two hours, wherein the second strengthening temperature is 500 ℃, and preserving the heat for three hours to obtain a second salt bath solution 2; putting the glass into an annealing furnace, heating the glass to a first strengthening temperature of 400 ℃ within one hour, preserving the heat for three hours, and then soaking the glass into the prepared first salt bath solution 1 for first strengthening treatment, wherein the time of the first strengthening treatment is 46 hours; putting the glass subjected to the first strengthening treatment into the steam of the prepared second salt bath solution 2 for second strengthening treatment, wherein the time of the second strengthening treatment is 22h; and finally, putting the glass subjected to the secondary strengthening treatment into an annealing furnace for cooling, cooling the glass to room temperature in the annealing furnace for 20 hours, taking out the glass, and cleaning the glass to obtain the strengthened electronic glass ceramics.
Further, the performance of the strengthened glass is tested, and the test instrument, the test method and the test conditions are as follows: the thickness of the glass is 1mm, and the spectral transmittance of 550nm is measured by using a U-4000 spectrophotometer; the value of the surface compressive stress and the depth of the compressive stress layer are measured by a glass surface stress meter FSM-6000LE, and the refractive index of a sample is 1.536, and the optical elastic constant is 28.7[ (nm/cm)/MPa ]; microhardness and fracture toughness are calculated by dividing the load of a diamond quadrangular pyramid pressure head with an included angle of 136 degrees on a test surface when the diamond quadrangular pyramid pressure head is pressed into a pyramid-shaped recess on the test surface by the length of the recess by adopting equipment HXD-3000; the four-point bending strength is tested by adopting a microcomputer controlled electronic universal tester TY8000-5000N and taking ASTM C158-2002 as a standard.
The specific test results are as follows:
the invention also discloses a preparation device adopting the preparation method of the strengthened electronic glass ceramics, and as shown in fig. 2 and fig. 3, the preparation device comprises a first closed container 3, a second closed container 4 and a basket tool 5, wherein the first closed container 3 is communicated with the second closed container 4, a first salt bath solution 1 is placed in the first closed container 3, a second salt bath solution 2 is placed in the second closed container 4, the first closed container 3 is provided with an eccentric opening 6, the basket tool 5 is fixed with glass to be strengthened, and the basket tool 5 is placed in the first closed container 3 through the eccentric opening 6.
Specifically, the glass which is cut and edged is fixed on a basket tool 5, then the basket tool 5 is put into an annealing furnace, the temperature is raised to 400-450 ℃ by one hour, and the temperature is kept for 1-4 hours; then, as shown in fig. 2, placing a basket 5 into a first closed container 3 through an eccentric port 6, rapidly immersing the basket into a first salt bath solution 1, and placing the first closed container in the first salt bath solution 1 at 400-450 ℃ for 24-48 h for first strengthening treatment; as shown in fig. 3, after the first strengthening treatment is completed, the first closed container 1 is rotated by 90 degrees, one side of the eccentric port 6 is upward, the glass is exposed out of the first salt bath solution, then the steam of the second salt bath solution 2 in the second closed container 4 is input into the upper space of the first closed container 3, and the steam of the second salt bath solution 2 is used for carrying out second strengthening treatment on the glass for 12-24 hours; and after the second strengthening treatment is finished, taking the glass out of the first closed container 3, putting the glass into an annealing furnace, cooling the glass to room temperature for 4-24 hours, taking out the glass, and cleaning the glass to obtain the strengthened electronic glass-ceramic.
In some embodiments, as shown in fig. 3, the preparation device further comprises a vent pipe 7, the vent pipe 7 is provided with a vent valve 8, one end of the vent pipe 7 passes through the eccentric opening 6 to communicate with the first closed container 3, and the other end of the vent pipe 7 communicates with the second closed container 4. Specifically, a sealing cover 9 is arranged on the eccentric opening 6, and the vent pipe 7 passes through the sealing cover 9 on the eccentric opening 6 to be communicated with the first closed container 3.
Thus far, various embodiments of the present disclosure have been described in detail. Some details that are well known in the art have not been described in order to avoid obscuring the concepts of the present disclosure. It will be fully apparent to those skilled in the art from the foregoing description how to practice the presently disclosed embodiments.
Although some specific embodiments of the present disclosure have been described in detail by way of example, it should be understood by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the present disclosure. It will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope and spirit of the present disclosure. In particular, the technical features mentioned in the embodiments can be combined in any way as long as there is no structural conflict.
Claims (10)
1. The preparation method of the reinforced electronic glass ceramics is characterized by comprising the following steps:
heating a mixed solution of sodium nitrate and potassium nitrate to a first strengthening temperature to obtain a first salt bath solution (1);
heating the mixed solution of potassium nitrate and potassium sulfate to a second strengthening temperature to obtain a second salt bath solution (2);
heating the glass to the first strengthening temperature;
immersing the glass heated to the first strengthening temperature into the first salt bath (1) to perform first strengthening treatment on the glass;
putting the glass subjected to the first strengthening treatment into the steam of the second salt bath solution (2) to carry out second strengthening treatment;
and reducing the temperature of the glass subjected to the second strengthening treatment to room temperature to perform annealing treatment.
2. The method for preparing reinforced electronic glass-ceramic according to claim 1, wherein the mass percentages of the sodium nitrate and the potassium nitrate in the first salt bath solution (1) are 50-90 wt% and 10-50 wt%, respectively, and the mass percentages of the potassium nitrate and the potassium sulfate in the second salt bath solution (2) are 90-99 wt% and 1-10 wt%, respectively.
3. The method for preparing the strengthened electronic glass-ceramic according to claim 2, wherein the first strengthening temperature is 400-450 ℃ and the second strengthening temperature is 500-550 ℃.
4. The method for preparing the strengthened electronic glass-ceramic according to claim 3, wherein the step of heating the mixed solution of sodium nitrate and potassium nitrate to the first strengthening temperature to obtain the first salt bath solution (1) comprises: heating the mixed solution of the sodium nitrate and the potassium nitrate to the first strengthening temperature, and then preserving heat for 3 hours to obtain a first salt bath solution (1);
heating the mixed solution of potassium nitrate and potassium sulfate to a second strengthening temperature to obtain a second salt bath solution (2) comprising: and heating the mixed solution of potassium nitrate and potassium sulfate to the second strengthening temperature, and then preserving the heat for 3 hours to obtain the second salt bath solution (2).
5. The method for producing a strengthened electronic glass-ceramic according to claim 4, wherein the glass heated to the first strengthening temperature is immersed in the first salt bath (1), and the first strengthening treatment of the glass comprises: and heating the glass to the first strengthening temperature, preserving the heat for 1-4 h, and then carrying out the first strengthening treatment.
6. The method for preparing the strengthened electronic glass-ceramic according to claim 5, wherein the time of the first strengthening treatment is 24-48 h, and the time of the second strengthening treatment is 12-24 h.
7. The method for preparing the strengthened electronic glass-ceramic according to claim 6, wherein the annealing time is 4-24 h.
8. The method for preparing the reinforced electronic glass-ceramic according to claim 1, wherein the potassium nitrate, the sodium nitrate and the potassium sulfate contain less than 50ppm of iron oxide, copper oxide, silver oxide and titanium oxide.
9. A manufacturing apparatus using the method for manufacturing strengthened electronic glass-ceramics according to any one of claims 1-8, comprising a first closed container (3), a second closed container (4), and a basket (5), wherein the first closed container (3) and the second closed container (4) are communicated, the first salt bath solution (1) is placed in the first closed container (3), the second salt bath solution (2) is placed in the second closed container (4), an eccentric opening (6) is arranged on the first closed container (3), the glass to be strengthened is fixed on the basket (5), and the basket (5) is placed in the first closed container (3) through the eccentric opening (6).
10. The preparation device according to claim 9, further comprising a vent pipe (7), wherein a vent valve (8) is disposed on the vent pipe (7), and one end of the vent pipe (7) is communicated with the first closed container (3) through the eccentric opening (6) and the other end is communicated with the second closed container (4).
Priority Applications (1)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116002992A (en) * | 2022-12-29 | 2023-04-25 | 东莞市晶博光电股份有限公司 | Glass strengthening process capable of prolonging service life of furnace salt |
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- 2022-09-09 CN CN202211100280.4A patent/CN115286262A/en active Pending
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| 陈季丹等: "《燃烧理论与污染控制》", 30 September 2019, 机械工业出版社, pages: 142 - 77 * |
| 陈季丹等: "《电介质物理学》", 机械工业出版社, pages: 33 - 77 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116002992A (en) * | 2022-12-29 | 2023-04-25 | 东莞市晶博光电股份有限公司 | Glass strengthening process capable of prolonging service life of furnace salt |
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