CN115304279A - Spinel crystal phase and indian stone crystal phase composite microcrystalline glass and preparation method thereof - Google Patents
Spinel crystal phase and indian stone crystal phase composite microcrystalline glass and preparation method thereof Download PDFInfo
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- CN115304279A CN115304279A CN202210887923.8A CN202210887923A CN115304279A CN 115304279 A CN115304279 A CN 115304279A CN 202210887923 A CN202210887923 A CN 202210887923A CN 115304279 A CN115304279 A CN 115304279A
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- 239000013078 crystal Substances 0.000 title claims abstract description 66
- 239000011521 glass Substances 0.000 title claims abstract description 65
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 25
- 239000011029 spinel Substances 0.000 title claims abstract description 25
- 239000004575 stone Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 8
- 229910018068 Li 2 O Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 38
- 238000002844 melting Methods 0.000 claims description 29
- 230000008018 melting Effects 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 239000010431 corundum Substances 0.000 claims description 12
- 239000002241 glass-ceramic Substances 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000006060 molten glass Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000005347 annealed glass Substances 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- -1 magnesium-aluminum-silicon Chemical compound 0.000 description 6
- 238000005452 bending Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000008395 clarifying agent Substances 0.000 description 3
- 239000000156 glass melt Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910020068 MgAl Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000002667 nucleating agent Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000013080 microcrystalline material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- 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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
Abstract
The invention discloses a spinel crystal phase and indian stone crystal phase composite microcrystalline glass, which is prepared from the following raw materials in percentage by weight: siO 2 2 35～40wt％、MgO 15～17wt％、Al 2 O 3 34～37wt％、Li 2 O 0～0.5wt％、ZnO 0～0.5wt％、ZrO 2 3～4wt％、P 2 O 5 3～4wt％、Na 2 O 2wt％、Sb 2 O 3 2wt%. The invention also provides a preparation method of the microcrystalline glass, and the spinel crystal phase and indian stone crystal phase composite microcrystalline glass with high hardness, high strength, high toughness and low dielectric constant can be obtained by adopting the method.
Description
Technical Field
The invention relates to the field of microcrystalline glass, in particular to spinel crystal phase and indian stone crystal phase composite microcrystalline glass and a preparation method thereof.
Background
The microcrystal glass (also called glass ceramic) is an inorganic non-metal material containing regular ordered crystal phase component and amorphous glass phase component, and its unique microstructure property can make it possess the common advantages of glass and ceramic at the same time. By utilizing the essential characteristic that the microcrystalline glass contains ordered crystalline phase components, the microcrystalline glass product with the required performance target can be quickly obtained by adopting various methods to controllably adjust the main crystalline phase of the microcrystalline glass. It is well known that the unique performance characteristics exhibited by different materials are often determined by their unique microstructure, crystalline phase type. By properly designing the basic glass components and selecting a proper heat treatment process to regulate and control the characteristic main crystal phase of the sample, the microcrystalline glass product with the target performance characteristics can be quickly obtained. In the early days, most people pay attention to the intuitive performance characteristics of the microcrystalline glass, such as corrosion resistance, stability, thermal expansibility and the like, and develop corresponding products in practical production and living by relying on the characteristics, wherein the products comprise the microcrystalline glass electromagnetic oven panel which is generally applied at present, various microcrystalline glass plates for architectural decoration and industrial protection and the like. With the continuous and intensive research, the microcrystalline glass product with specific crystalline phase composition and certain special optical, electrical, magnetic and thermal functions can be obtained by designing the basic glass components and regulating and controlling the subsequent heat treatment process parameters under the same other conditions.
In the context of electronic device panels, glass-ceramic panels having specific crystalline phase characteristics have superior performance advantages over ordinary glass panels. Due to the performance characteristics corresponding to the specific crystalline phase composition, the microcrystalline glass panel can not only meet various application requirements of the electronic device panel to the greatest extent, but also additionally help the electronic equipment to get rid of an external unnecessary coat protection device, so that the durability of the equipment device is enhanced, the use cost of a user is reduced, and the experience is enhanced.
At present, a microcrystalline glass (or glass ceramic) panel in an electronic device is mainly a magnesium-aluminum-silicon system microcrystalline glass with cordierite as a main crystal phase. There have been many related patents on microcrystalline glass of magnesium, aluminum and silicon series. Patent CN110357435A reports that MgO and Al are used 2 O 3 、SiO 2 、ZrO 2 、B 2 O 3 The high-strength high-modulus magnesium-aluminum-silicon microcrystalline glass with CaO and MnO as components realizes the improvement of the mechanical strength and Young modulus and the reduction of the dielectric loss of the magnesium-aluminum-silicon microcrystalline glass, but the magnesium-aluminum-silicon microcrystalline glass has a plurality of and mixed crystal phase components and has related content of regulation and control of a main crystal phase. CN111320391A prepares a compound with MgO and Al 2 O 3 、SiO 2 、B 2 O 3 The magnesium-aluminum-silicon microcrystalline glass prepared by the method is colorless and transparent, has large surface hardness, low expansion coefficient and proper bending strength, is suitable for a display panel, but needs multiple phase separation heat treatment and crystallization heat treatment in the preparation process, has complex operation and large energy consumption, and the main crystal phase of the cordierite is accompanied with other impure phases. Patent CN109265011A describes a magnesium-aluminum-silicon system glass and a high-crystallinity transparent microcrystalline glass and a preparation method thereof. The method adopts a melting process of inducing high-temperature convection stirring by temperature perturbation, but the method has too strict requirements on instruments, is difficult to realize accurate temperature regulation and control particularly at high temperature of more than 1600 ℃, and does not relate to research reports related to the regulation and control of a main crystal phase.
Disclosure of Invention
The invention aims to provide spinel crystal phase and indian stone crystal phase composite glass ceramics with high hardness, high strength, high toughness and low dielectric constant and a preparation method thereof.
In order to solve the technical problems, the invention provides a microcrystalline glass compounded by a spinel crystal phase and an indian stone crystal phase, wherein the raw materials of the compound microcrystalline glass comprise the following components in percentage by weight:
SiO 2 35～40wt％、MgO 15～17wt％、Al 2 O 3 34～37wt％、Li 2 O 0～0.5wt％、ZnO 0～0.5wt％、ZrO 2 3～4wt％、P 2 O 5 3～4wt％、Na 2 O 2wt％、Sb 2 O 3 2wt％。
as an improvement of the spinel crystal phase and indian stone crystal phase composite glass ceramics, the composite glass ceramics comprises the following components by weight percent: siO 2 2 38％、MgO15％、Al 2 O 3 35％、Li 2 O0.5％、ZnO0.5％、ZrO 2 3.5％、P 2 O 5 3.5％、Na 2 O2％、Sb 2 O 3 2％。
The invention also provides a preparation method of the microcrystalline glass compounded by the spinel crystal phase and the indian stone crystal phase, which comprises the following steps:
(1) Ball-milling the raw materials in a mechanical ball mill for 24 hours, and sieving the raw materials by a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw material into a corundum crucible, placing the corundum crucible into a melting furnace, heating the melting furnace to 1600-1650 ℃ according to the heating rate of 6 ℃/min, and melting at high temperature for 10 +/-0.5 h;
(3) Pouring the molten glass obtained by high-temperature melting into a preheated graphite mold preheated to 550 +/-50 ℃ in advance for casting molding, putting the cast glass into an annealing furnace along with the graphite mold, annealing at the temperature of 500-600 ℃ for 8-10 h, and then cooling to room temperature along with the furnace;
(4) And (3) putting the annealed glass into a mold, heating to 950-980 ℃ at a heating rate of 3 ℃/min, and carrying out heat treatment for 2 +/-0.2 h to obtain the microcrystalline glass with the spinel crystal phase and the indian stone crystal phase.
In the present invention: the proper silicon content provides the main skeleton structure of the glass; the addition of MgO participates in the formation of a framework on one hand, and can improve the surface hardness of the glass matrix on the other hand; appropriate Al 2 O 3 The content is participated in serving as a glass framework on one hand, and can prevent impurity phases from being separated out to ensure the formation of a main crystal phase on the other hand; suitable Li 2 With an O content ofFluxing agent, capable of assisting glass melting, and excess Li 2 The content of O can promote the precipitation of an impurity phase; proper ZnO can help the melting effect to be better in the glass melting process. ZrO (ZrO) 2 The components as the nucleating agent can effectively reduce the temperature required by pre-nucleating and nucleating of the glass sample, and the proper content can ensure the precipitation of the main crystal phase. P is 2 O 5 The component is used as a nucleating agent, which is beneficial to nucleating the microcrystalline glass and reducing the temperature required by nucleating. Na (Na) 2 O, as a flux in the present system, is used to reduce the viscosity of the glass. While excessive Na2O reduces the thermal, chemical and mechanical strength of the glass. Said 2wt% of Sb 2 O 3 The glass melt clarifying agent is used as a clarifying agent in the system, and the clarifying agent absorbs oxygen at low temperature and releases oxygen at low temperature, so that the glass melt is helped to discharge dissolved oxygen and small bubbles quickly, and the clarification and homogenization of the glass melt are realized.
The invention provides a microcrystalline glass material compounded by spinel crystal phase and indian stone crystal phase, which obtains an adjustable main crystal phase by adjusting the raw material formula and optimizing the heat treatment process, combines the indian stone crystal phase and the spinel crystal phase by a characteristic crystal phase embedded with each other and the indian stone crystal phase and the spinel crystal phase, comprehensively improves the mechanical property and the dielectric property of the microcrystalline glass, and has the Vickers hardness ranging from 690 Hv to 716Hv, the bending strength ranging from 138 MPa to 145MPa and the fracture toughness ranging from 2.0 MPa.m l/2 The elastic modulus is larger than 100GPa, the dielectric constant (1 MHz) is in the range of 6.4-6.6, and the dielectric loss (1 MHz) is about 0.006, so that the related performance requirements in the field of electronic devices are met.
In conclusion, the spinel crystal phase and indian stone crystal phase composite microcrystalline glass has the characteristics of adjustable main crystal phase, high hardness, high strength, high toughness, excellent dielectric property and the like, and has potential application prospects in the field of electronic device panels.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 is a SEM image of microcrystalline glass.
FIG. 2 is XRD patterns of examples Nos. 1 to 4;
in the figure, example 4, example 3, example 2, and example 1 are shown in this order from top to bottom.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
the invention provides 4 examples, respectively numbered as Nos. 1-4, wherein the specific component contents and performance parameters of the microcrystalline material of each example are shown in Table 1 below.
TABLE 1
The above examples were tested for various properties, the Vickers hardness was measured according to GB/T37900-2019, the bending strength was measured according to GB/T35160.3-2017, the visible light transmittance was measured according to GB/T2410-2008, and the results are shown in the table above.
The specific embodiment is as follows:
example 1
(1) Accurately weighing the raw materials according to the formula in the table 1, mixing and stirring, then mechanically ball-milling for 24 hours, and sieving by a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw material into a corundum crucible for melting, placing the corundum crucible into a melting furnace, and heating the melting furnace to 1620 ℃ at the heating rate of 6 ℃/min to perform high-temperature melting for 10 hours;
(3) Pouring the molten glass obtained by high-temperature melting into a graphite mold preheated to 550 ℃ in advance, putting the molten glass into an annealing furnace along with the graphite mold, annealing for 10 hours at the temperature of 550 ℃, and then cooling to room temperature along with the furnace;
(4) Putting the glass obtained in the step 3) into a mould, and heating to 980 ℃ at a heating rate of 3 ℃/min for heat treatment for 2h to obtain the spinel crystal phase and indian stone crystal phase composite glass ceramics.
Example 2
(1) Accurately weighing the raw materials according to the formula in the table 1, mixing and stirring, then mechanically ball-milling for 24 hours, and sieving by a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible for melting, putting the corundum crucible into a melting furnace, and heating the melting furnace to 1620 ℃ at the heating rate of 6 ℃/min to melt for 10 hours;
(3) Pouring molten glass obtained by high-temperature melting into a graphite mold preheated to 550 ℃ in advance, putting the glass together with the graphite mold into an annealing furnace, annealing at 550 ℃ for 10 hours, and cooling to room temperature along with the furnace;
(4) Putting the glass obtained in the step 3) into a mould, heating to 980 ℃ at a heating rate of 3 ℃/min, and carrying out heat treatment for 2h to obtain the microcrystalline glass with india stone as a main crystal phase and a small amount of spinel crystal phase.
Example 3
(1) Accurately weighing the raw materials according to the formula in the table 1, mixing and stirring, then mechanically milling for 24 hours, and sieving by using a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible for melting, putting the corundum crucible into a melting furnace, heating the melting furnace to 1650 ℃ according to the heating rate of 6 ℃/min, and melting at high temperature for 10 hours;
(3) Pouring molten glass obtained by high-temperature melting into a graphite mold preheated to 600 ℃ in advance, putting the glass and the graphite mold into an annealing furnace, annealing at the temperature of 600 ℃ for 8 hours, and cooling to room temperature along with the furnace;
(4) Putting the glass obtained in the step 3) into a mould, heating to 950 ℃ at a heating rate of 3 ℃/min, and carrying out heat treatment for 2h to obtain the microcrystalline glass with spinel as a main crystal phase and a small amount of indian stone crystal phase.
Example 4
(1) Accurately weighing the raw materials according to the formula in the table 1, mixing and stirring, then mechanically milling for 24 hours, and sieving by using a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible for melting, putting the corundum crucible into a melting furnace, heating the melting furnace to 1600 ℃ according to the heating rate of 6 ℃/min, and melting for 10 hours at high temperature;
(3) Pouring molten glass obtained by high-temperature melting into a graphite mold preheated to 500 ℃ in advance, putting glass together with the graphite mold into an annealing furnace, annealing for 8 hours at the temperature of 500 ℃, and then cooling to room temperature along with the furnace;
(4) Putting the glass obtained in the step 3) into a mould, heating to 950 ℃ at a heating rate of 3 ℃/min, and carrying out heat treatment for 2h to obtain the microcrystalline glass with the spinel crystal phase and the indian stone crystal phase.
SEM images of the spinel crystal phase and the Indian stone crystal phase composite glass ceramics obtained in the example 1 are shown in figure 1, and the crystal phase size is between 30 and 70 nm; XRD patterns of spinel crystal phase and indian stone crystal phase composite microcrystalline glasses obtained in examples 1-4 are shown in figure 2, and the main crystal phase is indian stone crystal phase, spinel crystal phase or both crystal phases, so that the crystal phase can be adjusted.
Comparative example 1, the raw materials of the glass ceramics consist of the following components in percentage by weight: siO 2 2 58wt％、MgO 15wt％、Al 2 O 3 13wt％、Li 2 O 1wt％、ZnO 2wt％、ZrO 2 3.5wt％、P 2 O 5 3.5wt％、Na 2 O 2wt％、Sb 2 O 3 2wt%. The remaining steps are identical to example 1.
The main crystal phase of the obtained product is MgAl 2 Si 4 O 12 Vickers hardness of 700Hv, bending strength of 139MPa, fracture toughness of 1.88 MPa.m l/2 The elastic modulus was 100GPa, the dielectric constant (1 MHz) was 6.7, and the dielectric loss (1 MHz) was 0.007.
Comparative example 2, glass ceramics formulation is identical to example 1.
The step 4) of the embodiment 1 is changed into the following steps: heating to 780 ℃ at the heating rate of 6 ℃/min for heat treatment, wherein the treatment time is 1h, and the rest is equal to that of example 1.
The main crystal phase of the obtained product is MgAl 2 Si 4 O 12 Vickers hardness of 600Hv, bending strength of 120MPa, fracture toughness of 1.67 MPa.m l/2 The elastic modulus 90GPa, the dielectric constant (1 MHz) 9.2 and the dielectric loss (1 MHz) about 0.012.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (3)
1. The microcrystalline glass compounded by the spinel crystal phase and the indian stone crystal phase is characterized in that the raw materials of the compound microcrystalline glass consist of the following components in percentage by weight:
SiO 2 35～40wt％、MgO 15～17wt％、Al 2 O 3 34～37wt％、Li 2 O 0～0.5wt％、ZnO 0～0.5wt％、ZrO 2 3～4wt％、P 2 O 5 3～4wt％、Na 2 O 2wt％、Sb 2 O 3 2wt％。
2. the spinel and ayanite composite glass-ceramic according to claim 1, characterized in that the raw materials of the composite glass-ceramic consist of the following components in percentage by weight: siO 2 2 38％、MgO15％、Al 2 O 3 35％、Li 2 O0.5％、ZnO0.5％、ZrO 2 3.5％、P 2 O 5 3.5％、Na 2 O2％、Sb 2 O 3 2％。
3. A method for producing a crystallized glass in which a spinel crystal phase and an indialite crystal phase are combined according to claim 1 or 2, characterized by comprising the steps of:
(1) Ball-milling the raw materials in a mechanical ball mill, and sieving the raw materials with a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible, placing the corundum crucible into a melting furnace, heating the melting furnace to 1600-1650 ℃ according to the heating rate of 6 ℃/min, and melting at high temperature for 10 +/-0.5 h;
(3) Pouring the molten glass obtained by high-temperature melting into a preheated graphite mold preheated to 550 +/-50 ℃ in advance for casting and molding, putting the cast and molded glass into an annealing furnace along with the graphite mold, annealing for 8-10 h at the temperature of 500-600 ℃, and then cooling to room temperature along with the furnace;
(4) And (3) putting the annealed glass into a mold, heating to 950-980 ℃ at a heating rate of 3 ℃/min, and carrying out heat treatment for 2 +/-0.2 h to obtain the microcrystalline glass with the spinel crystal phase and the indian stone crystal phase compounded.
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