CN115304279B - Spinel crystal phase and India Dan Jingxiang composite microcrystalline glass and preparation method thereof - Google Patents
Spinel crystal phase and India Dan Jingxiang composite microcrystalline glass and preparation method thereof Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 47
- 239000011521 glass Substances 0.000 title claims abstract description 44
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 25
- 239000011029 spinel Substances 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 9
- 229910018068 Li 2 O Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 37
- 229910052593 corundum Inorganic materials 0.000 claims description 13
- 239000010431 corundum Substances 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 239000005347 annealed glass Substances 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims description 2
- 238000003723 Smelting Methods 0.000 description 16
- -1 magnesium aluminum silicon Chemical compound 0.000 description 5
- 239000006060 molten glass Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229910020068 MgAl Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000008395 clarifying agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- 238000013461 design Methods 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
- 238000010309 melting process Methods 0.000 description 2
- 239000002667 nucleating agent Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process 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
- 238000010586 diagram 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
- 230000006698 induction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000013080 microcrystalline material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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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
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses spinel crystal phase and India Dan Jingxiang composite glass ceramics, which comprises the following raw materials in percentage by weight: siO (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%. The invention also provides a preparation method of the microcrystalline glass, and the spinel crystal phase with high hardness, high strength, high toughness and low dielectric strength and the India Dan Jingxiang composite microcrystalline glass 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 India Dan Jingxiang composite microcrystalline glass and a preparation method thereof.
Background
Glass ceramics (also known as glass ceramics) are inorganic nonmetallic materials that contain a regular ordered crystalline phase component and an amorphous glass phase component, and their unique microstructural properties provide them with the common advantageous features of both glass and ceramics. By utilizing the characteristic that the microcrystalline glass itself contains ordered crystal phase components, the main crystal phase of the microcrystalline glass can be controllably adjusted by adopting various methods, and the microcrystalline glass product with the required performance target can be rapidly obtained. It is well known that the unique performance characteristics exhibited by different materials are often determined by their unique microstructure, crystalline phase type. Through proper design of basic glass components and proper heat treatment process, the main crystal phase of the sample characteristic is regulated and controlled, and the microcrystalline glass product with the target performance characteristic can be obtained rapidly. In the early stage, people mostly pay attention to visual performance characteristics such as corrosion resistance, stability and thermal expansibility, and the like, which are exhibited by the glass ceramics, and develop corresponding actual production and living products based on the characteristics, including glass ceramics electromagnetic oven panels, various architectural decorations, glass ceramics plates for industrial protection, and the like which are commonly used at present. With the continuous and intensive research, it is found that, under the same conditions, a microcrystalline glass product with specific crystalline phase composition and certain special optical, electrical, magnetic and thermal functions can be obtained by adjusting and controlling the basic glass component design and the subsequent heat treatment process parameters.
Glass ceramic panels having specific crystalline phase characteristics have excellent performance advantages over conventional glass panels in terms of electronic device panels. Due to the performance characteristics corresponding to the specific crystalline phase composition, the microcrystalline glass panel not only can meet various application requirements of the electronic device panel to the greatest extent, but also can help the electronic device get rid of an external unnecessary coat protection device, so that the durability of the device is enhanced, the use cost of a user is reduced, and the experience is enhanced.
At present, glass ceramics (or glass ceramics) panels in electronic devices are mainly magnesium aluminum silicon system glass ceramics with cordierite as a main crystal phase. Several related patents have reported on magnesia-alumina-silica-based glass ceramics. Patent CN110357435A reports a composition containing MgO and Al 2 O 3 、SiO 2 、ZrO 2 、B 2 O 3 The high-strength high-modulus magnesium aluminum silicon glass ceramics taking CaO and MnO as components realizes the improvement of the mechanical strength and Young modulus of the magnesium aluminum silicon glass ceramics and the reduction of dielectric loss, but has a plurality of and miscellaneous crystalline phase components, and the related content of the regulation and control of a main crystalline phase is seen. Patent CN111320391A prepared with MgO and Al 2 O 3 、SiO 2 、B 2 O 3 Is composed ofThe magnesium aluminum silicon series microcrystalline glass prepared by the method is colorless and transparent, has high surface hardness, low expansion coefficient and high bending strength, is suitable for display panels, but the preparation process needs to carry out split-phase heat treatment and crystallization heat treatment for multiple times, has complex operation and huge energy consumption, and is accompanied with other impurity phases along with the main crystal of the cordierite. Patent CN109265011a describes a magnesium aluminum silicon system glass and a high crystallinity transparent glass ceramic and a method for preparing the same. The method adopts a melting process of 'temperature perturbation induction high-temperature convection stirring', however, the method has too severe requirements on instruments, and especially is difficult to realize accurate temperature regulation and control at the high temperature exceeding 1600 ℃, and research reports related to the regulation and control of a main crystal phase are not related.
Disclosure of Invention
The invention aims to solve the technical problem of providing spinel crystal phase and India Dan Jingxiang composite glass ceramics with high hardness, high strength, high toughness and low dielectric and a preparation method thereof.
In order to solve the technical problems, the invention provides spinel crystal phase and India Dan Jingxiang composite glass ceramics, which comprises the following raw materials 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 the India Dan Jingxiang composite glass ceramics, the composite glass ceramics comprises the following raw materials in percentage by weight: siO (SiO) 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 spinel crystal phase and India Dan Jingxiang composite glass ceramics, which comprises the following steps:
(1) Ball milling the raw materials in a mechanical ball mill (24 h), and sieving with a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible, and 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 the powder raw materials at a high temperature for 10+/-0.5 h;
(3) Pouring the glass liquid obtained by high-temperature melting into a preheated graphite mould preheated to 550+/-50 ℃ in advance for casting forming, putting the cast glass into an annealing furnace along with the graphite mould, annealing for 8-10 h at 500-600 ℃, and then cooling to room temperature along with the furnace;
(4) And (3) placing the annealed glass into a mould, heating to 950-980 ℃ at a heating rate of 3 ℃/min, and performing heat treatment for 2+/-0.2 h to obtain the spinel crystal phase and India Dan Jingxiang composite glass ceramics.
In the present invention: the appropriate silicon content provides the glass primary skeleton structure; the addition of MgO participates in forming a framework on one hand, and on the other hand, the surface hardness of the glass matrix can be improved; suitable Al 2 O 3 The content is participated in serving as a glass skeleton, and can prevent impurity phase precipitation to ensure the formation of a main crystal phase; suitable Li 2 The O content as a fluxing agent can help the glass to melt, while the excess Li 2 The content of O can promote the precipitation of impurity phases; proper ZnO can help the melting effect to be better in the glass melting process. ZrO (ZrO) 2 The components are used as nucleating agents, so that the temperature required by pre-nucleating and nucleating of a glass sample can be effectively reduced, and the precipitation of a main crystal phase can be ensured by proper content. P (P) 2 O 5 The component is used as a nucleating agent, is beneficial to nucleation of glass ceramics and reduces the temperature required by nucleation. Na (Na) 2 O, which is a flux in the bulk system, is used to reduce the viscosity of the glass. While excessive Na2O reduces the thermal stability, chemical stability and mechanical strength of the glass. Said 2wt% Sb 2 O 3 As a clarifying agent in the system, the clarifying agent absorbs oxygen at low temperature and releases oxygen at high temperature, thereby helping the glass liquid to discharge dissolved oxygen and small bubbles quickly and realizing clarification and homogenization of the glass liquid.
The invention is thatProvides a spinel crystal phase and Indian Dan Jingxiang composite microcrystalline glass material, which is characterized by that its main crystal phase is adjustable, the spinelle crystal phase and spinelle crystal phase are inlaid, and the combination of the spinelle crystal phase and spinelle crystal phase can raise the mechanical property and dielectric property of microcrystalline glass, its Vickers hardness is about 690-716 Hv, bending strength is about 138-145 MPa and fracture toughness is about 2.0 MPa-m l/2 About, the elastic modulus is larger than 100GPa, the dielectric constant (1 MHz) is about 6.4-6.6, the dielectric loss (1 MHz) is about 0.006, and the related performance requirements of the field of electronic devices are met.
In conclusion, the spinel crystal phase and India Dan Jingxiang composite glass ceramic 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 the embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 is an SEM image of glass ceramics.
FIG. 2 is XRD patterns of examples No.1 to 4;
in the figure, examples 4, 3, 2 and 1 are shown in this order from top to bottom.
Detailed Description
The invention will be further described with reference to the following specific examples, but the scope of the invention is not limited thereto:
the present invention provides 4 examples, numbered No.1-4, wherein the specific component contents and performance parameters of each example microcrystalline material are shown in table 1 below.
TABLE 1
Each performance test was performed on the above examples, the vickers hardness was tested according to GB/T37900-2019, the flexural strength was tested according to GB/T35160.3-2017, the visible light transmittance was tested according to GB/T2410-2008, and the results were as described in the above table.
Specific examples thereof are as follows:
example 1
(1) Accurately weighing the raw materials according to the formula of the table 1, mixing and stirring, mechanically ball-milling for 24 hours, and sieving with a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible for smelting, placing the corundum crucible into a smelting furnace, heating the smelting furnace to 1620 ℃ according to a heating rate of 6 ℃/min, and smelting at a high temperature for 10 hours;
(3) Pouring the molten glass obtained by high-temperature melting into a graphite mold preheated to 550 ℃, putting the molten glass together with the graphite mold into an annealing furnace, annealing for 10 hours at 550 ℃, and then cooling to room temperature along with the furnace;
(4) And 3) placing the glass obtained in the step 3) into a mould, heating to 980 ℃ at a heating rate of 3 ℃/min, and performing heat treatment for 2 hours to obtain the spinel crystal phase and the Indian Dan Jingxiang composite glass ceramic.
Example 2
(1) Accurately weighing the raw materials according to the formula of the table 1, mixing and stirring, mechanically ball-milling for 24 hours, and sieving with a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible for smelting, placing the corundum crucible into a smelting furnace, heating the smelting furnace to 1620 ℃ according to a heating rate of 6 ℃/min, and smelting for 10 hours;
(3) Pouring the molten glass obtained by high-temperature melting into a graphite mold preheated to 550 ℃, putting the glass together with the graphite mold into an annealing furnace, annealing for 10 hours at 550 ℃, and then cooling to room temperature along with the furnace;
(4) And 3) placing the glass obtained in the step 3) into a mould, heating to 980 ℃ at a heating rate of 3 ℃/min, and performing heat treatment for 2 hours to obtain the microcrystalline glass with indian 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 of the table 1, mixing and stirring, mechanically ball-milling for 24 hours, and sieving with a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible for smelting, placing the corundum crucible into a smelting furnace, and heating the smelting furnace to 1650 ℃ according to a heating rate of 6 ℃/min, and smelting the corundum crucible for 10 hours at a high temperature;
(3) Pouring the molten glass obtained by high-temperature melting into a graphite mold preheated to 600 ℃ in advance, putting the glass together with the graphite mold into an annealing furnace, annealing for 8 hours at 600 ℃, and then cooling to room temperature along with the furnace;
(4) And 3) placing the glass obtained in the step 3) into a mould, heating to 950 ℃ at a heating rate of 3 ℃/min, and performing heat treatment for 2 hours 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 of the table 1, mixing and stirring, mechanically ball-milling for 24 hours, and sieving with a 300-mesh sieve to obtain uniformly dispersed powder raw materials;
(2) Adding the uniformly dispersed powder raw materials into a corundum crucible for smelting, placing the corundum crucible into a smelting furnace, heating the smelting furnace to 1600 ℃ according to a heating rate of 6 ℃/min, and smelting at a high temperature for 10 hours;
(3) Pouring the molten glass obtained by high-temperature melting into a graphite mold preheated to 500 ℃, putting the 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) And 3) placing 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 2 hours to obtain the spinel crystal phase and India Dan Jingxiang composite glass ceramics.
The SEM diagram of spinel crystal phase and Indian Dan Jingxiang composite glass ceramics obtained in example 1 is shown in FIG. 1, and the crystal phase size is between 30 and 70 nm; the XRD patterns of the spinel crystal phases and the Indian Dan Jingxiang composite glass ceramics obtained in examples 1 to 4 are shown in FIG. 2, and the main crystal phase is an Indian stone crystal phase, a spinel crystal phase or both of the spinel crystal phases coexist, so that the crystal phase can be adjusted.
Comparative example 1, the glass ceramics comprises the following components in percentage by weight: siO (SiO) 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 700Hv, bending strength 139MPa, fracture toughness 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 and formulation of glass ceramics are the same as example 1.
Example 1, step 4) was changed to: the heat treatment was carried out by heating to 780℃at a heating rate of 6℃per minute for 1 hour, and the rest was the same as in example 1.
The main crystal phase of the obtained product is MgAl 2 Si 4 O 12 Vickers hardness 600Hv, bending strength 120MPa, fracture toughness 1.67 MPa.m l/2 The elastic modulus was 90GPa, the dielectric constant (1 MHz) was 9.2, and the dielectric loss (1 MHz) was about 0.012.
Finally, it should also be noted that the above list is merely a few specific embodiments of the present invention. Obviously, the invention is not limited to the above embodiments, but many variations are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (2)
1. The preparation method of the spinel crystal phase and India Dan Jingxiang composite glass ceramics is characterized by comprising the following steps of:
the spinel crystal phase and the India Dan Jingxiang composite glass ceramic raw materials comprise the following components in percentage by weight: siO (SiO) 2 35~40 wt%、MgO 15~17 wt%、Al 2 O 3 34~37 wt%、Li 2 O 0~0.5 wt%、ZnO 0~0.5 wt%、ZrO 2 3~4 wt%、P 2 O 5 3~4 wt%、Na 2 O 2 wt%、Sb 2 O 3 2 wt%；
The method comprises the following steps:
(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, and 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 a high temperature of 10+/-0.5 h;
(3) Pouring the glass liquid obtained by high-temperature melting into a preheated graphite mould preheated to 550+/-50 ℃ in advance for casting forming, putting the cast glass and the graphite mould into an annealing furnace together, annealing for 8-10 hours at the temperature of 500-600 ℃, and then cooling to room temperature along with the furnace;
(4) And (3) placing the annealed glass into a die, heating to 950-980 ℃ at a heating rate of 3 ℃/min, and performing heat treatment for 2+/-0.2 h to obtain the spinel crystal phase and India Dan Jingxiang composite glass ceramics.
2. The method for preparing the glass-ceramic compounded by the spinel crystal phase and the India Dan Jingxiang according to claim 1, wherein the raw materials of the glass-ceramic compounded by the spinel crystal phase and the India Dan Jingxiang comprise the following components in percentage by weight: siO (SiO) 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%。
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| CN1241547A (en) * | 1998-07-10 | 2000-01-19 | 赵凤宇 | Preparation of devitrified glass pipe |
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| US8664130B2 (en) * | 2012-04-13 | 2014-03-04 | Corning Incorporated | White, opaque β-spodumene/rutile glass-ceramic articles and methods for making the same |
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