CN116514540A - Glass ceramic composite material, preparation method thereof and electronic equipment - Google Patents
Glass ceramic composite material, preparation method thereof and electronic equipment Download PDFInfo
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- CN116514540A CN116514540A CN202210081955.9A CN202210081955A CN116514540A CN 116514540 A CN116514540 A CN 116514540A CN 202210081955 A CN202210081955 A CN 202210081955A CN 116514540 A CN116514540 A CN 116514540A
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- 239000002131 composite material Substances 0.000 title claims abstract description 69
- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 105
- 239000000919 ceramic Substances 0.000 claims abstract description 91
- 239000011159 matrix material Substances 0.000 claims abstract description 68
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims abstract description 12
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 7
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 37
- 239000002994 raw material Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 11
- 238000002834 transmittance Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 9
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 9
- 229910052810 boron oxide Inorganic materials 0.000 claims description 7
- 238000005238 degreasing Methods 0.000 claims description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 7
- 238000011282 treatment Methods 0.000 claims description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 description 15
- 238000001746 injection moulding Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 238000003801 milling Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910011255 B2O3 Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/04—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with articles made from glass
- C04B37/042—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with articles made from glass in a direct manner
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B2235/3246—Stabilised zirconias, e.g. YSZ or cerium stabilised zirconia
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Composite Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The application provides a glass ceramic composite material, a preparation method thereof and electronic equipment, wherein the glass ceramic composite material comprises a ceramic matrix with a cavity and glass filled in the cavity, and the ceramic matrix and the glass are integrally formed; wherein the material of the ceramic matrix comprises yttrium stabilized zirconia. The glass ceramic composite material comprises glass and glass filled in the cavity, wherein the ceramic matrix and the glass are integrally formed and are in seamless combination, and the interface combination strength of the ceramic matrix and the glass is high, so that the glass ceramic composite material is good in structural stability and high in quality reliability.
Description
Technical Field
The application relates to the technical field of composite materials, in particular to a glass ceramic composite material, a preparation method thereof and electronic equipment.
Background
Currently, ceramic materials are often used to prepare the back cover of electronic devices such as smart watches, and in order to provide an optical signal collection window, a cavity is usually formed in the ceramic material and glass is filled therein. However, the adhesive is often used in the industry to bond the glass and the ceramic material, and the phenomenon of loosening between the glass and the ceramic material after long-term use can cause the air tightness of the materials to be reduced, and even the glass to fall off.
Disclosure of Invention
In view of the above, the application provides a glass ceramic composite material, a preparation method thereof and electronic equipment, wherein the glass ceramic composite material comprises glass filled in the cavity, the ceramic matrix and the glass are integrally formed and are in seamless combination, and the interface combination strength of the ceramic matrix and the glass is high, so that the glass ceramic composite material has good structural stability and high quality reliability.
In particular, a first aspect of the present application provides a glass-ceramic composite comprising a ceramic matrix having a cavity, and glass filled in the cavity, the ceramic matrix being integrally formed with the glass; wherein the material of the ceramic matrix comprises yttrium stabilized zirconia.
The ceramic matrix and the glass are integrally formed, and are in seamless combination without the help of an additional adhesive, so that the glass ceramic composite material cannot deform, crack, fall off of the glass from the cavity and the like after being used for a long time.
Alternatively, the glass has a coefficient of thermal expansion of 7X 10 -6 /℃-11×10 -6 /℃。
Optionally, the ceramic matrix has a melting point greater than the melting point of the glass.
Optionally, the glass comprises the following components in parts by weight: 0-10 parts of aluminum oxide, 55-70 parts of silicon oxide, 0-10 parts of magnesium oxide, 10-20 parts of boron oxide and 15-25 parts of sodium oxide. Preferably, the glass comprises the following components in parts by weight: 3-5 parts of aluminum oxide, 60-70 parts of silicon oxide, 1-5 parts of magnesium oxide, 10-15 parts of boron oxide and 15-21 parts of sodium oxide.
Alternatively, the bonding strength between the ceramic substrate and the glass is 10Kgf to 12Kgf.
Optionally, the visible light transmittance of the glass is not less than 85%. Preferably, the visible light transmittance of the glass is not less than 90%.
Optionally, no bubbles are visible to the naked eye within the glass.
In a second aspect, the present application provides a glass ceramic composite comprising the steps of:
(1) Forming a ceramic raw material into a ceramic matrix blank, and sequentially degreasing and sintering the ceramic matrix blank to prepare a ceramic matrix with a cavity structure; wherein the ceramic raw material comprises yttrium-stabilized zirconia;
(2) And filling glass raw materials into the cavity structure of the ceramic matrix, sintering in a sintering furnace, and cooling to room temperature to obtain the glass ceramic composite material provided by the first aspect of the application.
The preparation method is simple to operate, high in production efficiency and suitable for large-scale industrial production.
Optionally, in step (1), the sintering process is preceded by a pre-firing process of the ceramic matrix blank.
Optionally, in step (1), a ceramic raw material is molded into the ceramic matrix blank having the cavity structure, or holes are made in the ceramic matrix blank after the sintering treatment to obtain the ceramic matrix having the cavity structure.
Optionally, the glass raw material comprises glass gobs and/or glass frits.
Optionally, in the step (2), the sintering heat preservation temperature is 1000-1400 ℃, and the heat preservation time is 0.5-4h. Preferably, the sintering heat preservation temperature is 1000-1100 ℃, and the heat preservation time is 1-2 h.
Optionally, in the step (2), the temperature rising rate from the room temperature to the holding temperature is 1 ℃/min-3 ℃/min.
Optionally, after the step (2), the method further comprises milling and polishing the glass ceramic composite material sequentially.
A third aspect of the present application provides a glass-ceramic composite, the electronic device having the glass-ceramic composite provided in the first aspect of the present application. The electronic device comprises a terminal device, in particular a smart watch, a smart bracelet and other wearable electronic devices.
Drawings
FIG. 1 is a schematic structural view of a glass-ceramic composite material prepared in example 1 of the present application.
The reference numerals are explained as follows: 100-glass ceramic composite; 10-a ceramic matrix; 11-glass.
Detailed Description
The following describes the technical scheme of the application in detail with reference to the accompanying drawings.
Specifically, referring to fig. 1, an embodiment of the present application provides a glass ceramic composite 100, where the glass ceramic composite 100 includes a ceramic matrix 10 having a cavity, and a glass 11 filled in the cavity, and the ceramic matrix 10 is integrally formed with the glass 11; wherein the material of the ceramic matrix 10 comprises yttrium stabilized zirconia.
The ceramic matrix 10 and the glass 11 are integrally formed, and are in seamless combination, and the ceramic matrix 10 and the glass 11 are not required to be compounded by means of an additional adhesive, so that thermal stress caused by the adhesive in a composite material is avoided, the shear stress peak value between the ceramic matrix 10 and the glass 11 is reduced, and the structural stability of the glass ceramic composite material 100 is improved, so that the glass ceramic composite material cannot deform, crack, fall off from a cavity and the like after long-time use.
In this application, yttrium stabilized zirconia refers generally to yttrium stabilized tetragonal phase zirconia (Y-TZP), and specifically, the above Y-TZP includes, but is not limited to, 3.2Y-TZP, 3Y-TZP, 2.5Y-TZP, 2.1Y-TZP.
In the present embodiment, the thermal expansion coefficient (denoted as a) of the glass 11 is 7×10 -6 /℃-11×10 -6 and/C. At this time, the thermal expansion coefficient of the ceramic base 10 and the glass 11 is substantially oneTherefore, the glass ceramic composite material can be ensured to be formed smoothly, the mixture containing the glass ceramic composite material and the glass ceramic composite material can be prevented from layering and separating due to overlarge difference of thermal expansion coefficients in the cooling process after sintering, the glass ceramic composite material can not be obtained, and the glass ceramic composite material 100 is ensured to have lower thermal stress and higher thermal stability. In addition, the coefficient of thermal expansion (denoted b) of the ceramic matrix 10 is also 7×10 -6 /℃-11×10 -6 Within the range of/. Degree.C. The specific coefficient of thermal expansion values may be the same or different. In the case where the thermal expansion coefficient values are different, the degree of deviation should be 15% or less, wherein the degree of deviation is defined as |a-b|/b.
In the embodiment of the application, the glass 11 comprises the following components in parts by weight: 0-10 parts of aluminum oxide, 55-70 parts of silicon oxide, 0-10 parts of magnesium oxide, 10-20 parts of boron oxide and 15-25 parts of sodium oxide. In some embodiments of the present application, the glass comprises the following components in parts by weight: 3-5 parts of aluminum oxide, 60-70 parts of silicon oxide, 1-5 parts of magnesium oxide, 10-15 parts of boron oxide and 15-21 parts of sodium oxide. Illustratively, the parts by weight of alumina may be 3 parts, 4 parts, 5 parts, etc. Illustratively, the parts by weight of the silica may be 60 parts, 61 parts, 62 parts, 65 parts, 68 parts, 70 parts, etc. Illustratively, the parts by weight of magnesium oxide may be 1 part, 1.5 parts, 3 parts, 5 parts, etc. Illustratively, the parts by weight of boron oxide may be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, etc. Illustratively, the parts by weight of sodium oxide may be 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, etc. The presence of the components of the glass 11 in the appropriate proportions may ensure that the glass 11 has a certain glass phase to have the appropriate hardness and light transmittance, and that the coefficient of thermal expansion of the glass 11 is substantially the same as that of the ceramic matrix 10; and the glass liquid formed by melting the glass raw materials has proper viscosity, so that bubbles generated in the glass liquid can be smoothly discharged, thereby ensuring that bubbles are not generated in the glass 11 and at the interface of the ceramic matrix 10 and the glass 11 in the formed glass ceramic composite material 100, and ensuring the structural strength and stability of the glass ceramic composite material 100.
In the present embodiment, no bubbles are visible to the naked eye within the glass 11. When the size of bubbles in the glass is at the micrometer level or less (not more than 1 μm) and the number is small, it is considered that no bubbles can be observed by naked eyes, and when the glass 11 meets the above requirements, it is advantageous to ensure the strength of the glass 11, also advantageous to the application of the glass ceramic composite 100 in the field of electronic devices and the like, and in addition, it is also possible to improve the aesthetic degree of the glass ceramic composite 100.
In some embodiments of the present application, the visible light transmittance of the glass 11 is not less than 85%. In other embodiments, the visible light transmittance of the glass 11 is not less than 90%. The higher visible light transmittance is beneficial to the application of the glass ceramic composite material 100 in the fields of electronic equipment and the like. Illustratively, it facilitates optical signal transmission of a smart watch, smart bracelet, or other wearable device.
In the present embodiment, the bonding strength between the ceramic base 10 and the glass 11 is 10Kgf to 12Kgf. The two have higher bonding strength, so that the structural stability of the glass ceramic composite material 100 can be ensured, and the quality reliability of the glass ceramic composite material is ensured.
In the present embodiment, the melting point of the ceramic base 10 is greater than the melting point of the glass 11. The melting points of the ceramic matrix 10 and the glass 11 satisfy the above conditions, and the preparation of the glass-ceramic composite material 100 can be ensured.
In the present embodiment, the area of the cavity (i.e., the glass portion) may be determined according to actual production needs. The thickness of the glass 11 may also be determined according to actual production requirements, and may be, for example, 0.5mm, 1mm, 2mm, 5mm, 10mm, or the like.
Correspondingly, the embodiment of the application also provides a preparation method of the glass ceramic composite material, which is suitable for preparing the glass ceramic composite material 100.
Specifically, the preparation method of the glass ceramic composite material comprises the following steps:
(1) Preparing a ceramic raw material into a ceramic matrix blank, and sequentially degreasing and sintering to prepare a ceramic matrix with a cavity structure; wherein the ceramic raw material comprises yttrium-stabilized zirconia;
(2) And filling glass raw materials into the cavity structure of the ceramic matrix, sintering in a sintering furnace, preserving heat for a period of time, and cooling to room temperature to obtain the glass ceramic composite material provided by the embodiment of the application.
In the preparation process, the glass raw material is filled into the cavity structure of the sintered ceramic matrix, and then the ceramic matrix and the glass raw material are placed in a sintering furnace together for re-sintering treatment. Under the action of high temperature, the glass raw material is converted into glass liquid with certain viscosity, and the glass liquid and yttrium-stabilized zirconia undergo solid melting reaction or even chemical reaction. In the cooling process, the glass raw material and the ceramic matrix are naturally bonded together, so that seamless bonding between the glass raw material and the ceramic matrix is realized, and strong interfacial bonding force is realized between the yttrium-stabilized zirconia ceramic and the glass, thereby improving the structural stability and the quality reliability of the glass ceramic composite material.
In general, in the production of ceramics, an organic component such as a binder is introduced into a ceramic raw material to shape the ceramics. Degreasing is removing the binder from the ceramic matrix.
In some embodiments of the present application, the ceramic raw material may be directly molded into the ceramic matrix blank having the cavity structure. For example, dry pressing, injection molding, casting, gel casting, and the like may be used to prepare the ceramic matrix blank. In some embodiments, a ceramic feedstock (yttrium stabilized zirconia) injection molded feed may be fed into an injection molding machine, and a ceramic matrix blank with a cavity structure may be produced by injection molding. In other embodiments, in step (1), holes are made in the ceramic matrix blank after the sintering process to obtain the ceramic matrix having the cavity structure.
In some embodiments of the present application, in step (1), the degreasing treatment may be a gradient heating process commonly used by those skilled in the art, and specifically, the method may include the following steps: firstly, the temperature is raised to 150 ℃ from room temperature at a heating rate of 2 ℃/min, the temperature is kept at 150 ℃ for 1h, then the temperature is raised to 400 ℃ at a heating rate of 0.15 ℃/min, the temperature is kept for 2h, and then the temperature is raised to 450 ℃ at a heating rate of 0.8 ℃/min, and the temperature is kept for 2h.
In the embodiment of the present application, in the step (1), the sintering may be a process commonly used by those skilled in the art. Specifically, the method comprises the following steps: heating to 1300-1500 ℃ at a heating rate of 1.5 ℃/min, preserving heat for 2h, and naturally cooling to room temperature.
In an embodiment of the present application, in step (2), the glass raw material includes glass gobs and/or glass frits. In a specific embodiment, a backing plate is first added below (on the side away from the outer surface) the ceramic matrix cavity structure to form a space that can accommodate molten glass or glass frit. In some embodiments, a suitably sized glass block is placed over the cavity structure of the ceramic substrate and sintered together in a sintering furnace. In other implementations, a proper amount of glass powder is filled into the accommodating space formed by the cavity structures of the backing plate and the ceramic matrix, and the backing plate and the ceramic matrix are placed in a sintering furnace together for sintering. After sintering is completed, the backing plate can be directly removed or removed from the glass ceramic composite material by a milling process or the like.
In some embodiments of the present application, in step (2), the sintering temperature is 1000 ℃ to 1400 ℃, and the heating rate is 1 ℃/min to 3 ℃/min. In a preferred embodiment, the sintering is carried out at a soak temperature in the range of 1000 ℃ to 1100 ℃. In the preparation method, the glass raw material and the ceramic matrix which is sintered are sintered again, the sintering temperature depends on the properties of the glass raw material, and the control of the sintering temperature in the above range is beneficial to ensuring the high strength of the sintered glass.
In some embodiments of the present application, in step (2), the incubation time is 0.5 to 4 hours. In other embodiments, the incubation time is 1h to 2h. Proper heat preservation time can ensure that bubbles generated in the melting process of the glass raw materials are completely removed, and further ensure that the strength of the finally obtained glass is higher. In addition, the strength of the ceramic matrix can be ensured to be high.
In some embodiments of the present application, after step (2), the method further comprises milling and polishing the glass ceramic composite material sequentially. Milling and polishing treatments can improve the surface flatness and surface finish of the glass-ceramic composites described above.
Embodiments of the present application also provide an electronic device having the glass-ceramic composite 100 provided by embodiments of the present application. The electronic device comprises a terminal device, and particularly comprises a smart watch, a smart bracelet, other wearable electronic devices and the like.
The following describes the technical scheme of the present application in detail in a plurality of embodiments.
Example 1
(1) Shaping of the ceramic matrix blank: injecting yttrium-stabilized zirconia injection molding feed into an injection molding machine, and preparing a ceramic matrix blank with a cavity structure by an injection molding method, wherein the injection molding conditions are as follows: the injection molding temperature is 210 ℃, the injection molding pressure is 100MPa, and the holding pressure is 100MPa.
(2) Degreasing: degreasing conditions are as follows: the temperature is kept for 1h from room temperature to 150 ℃ at a heating rate of 2 ℃/min, the temperature is kept for 2h from 150 ℃ to 400 ℃ at a heating rate of 0.15 ℃/min, and the temperature is kept for 2h from 400 ℃ to 450 ℃ at a heating rate of 0.8 ℃/min.
(3) Sintering: the sintering conditions are as follows: heating to 1400 ℃ at a heating rate of 1.5 ℃/min, preserving heat for 2 hours, and naturally cooling to room temperature to obtain the ceramic matrix. Wherein the ceramic matrix has a thermal expansion coefficient of 8.9X10 -6 /℃。
(4) Preparation of glass ceramic composite material: and adding a backing plate below the cavity structure of the ceramic matrix, placing glass raw materials with proper sizes above the cavity structure of the ceramic matrix, and sintering in a sintering furnace. Wherein the glass raw material contains 4.9% alumina, 61.6% silica, 1.3% magnesia, 12.3% boric oxide and 19.9% sodium oxide, and the thermal expansion coefficient of the glass raw material is 9.1X10 -6 and/C. The sintering conditions are as follows: the heating rate of 2 ℃/min is increased from room temperature to 1200 ℃, the temperature is kept for 2 hours, then the glass ceramic composite material is cooled to room temperature, and then milling, grinding and polishing are sequentially carried out, so that the glass ceramic composite material with the thickness of 1mm is prepared.
Example 2
The differences from example 1 are: the glass raw material contains 4.9 percent of alumina,61.4% silica, 1.3% magnesia, 14.5% boric oxide and 17.9% sodium oxide. And the coefficient of thermal expansion of the glass raw material is 8.1X10 -6 /℃。
Example 3
The differences from example 1 are: the glass raw material contains 3.3% of alumina, 59.9% of silicon oxide, 1.3% of magnesium oxide, 14.6% of boron oxide and 20.9% of sodium oxide. And the coefficient of thermal expansion of the above glass raw material (i.e., the coefficient of thermal expansion of glass in the glass-ceramic composite material) is 9.2X10 -6 /℃。
Example 4
The difference from example 1 is that the sintering conditions in the above-mentioned (3) sintering treatment are: the heating rate of 2 ℃/min is increased from room temperature to 1000 ℃, the temperature is kept for 2 hours, and then the ceramic matrix is obtained after natural cooling to room temperature.
Example 5
The difference from example 1 is that the sintering conditions in the above-mentioned (3) sintering treatment are: the heating rate of 2 ℃/min is increased from room temperature to 1400 ℃, the temperature is kept for 2 hours, and then the ceramic matrix is obtained after natural cooling to room temperature.
To highlight the beneficial effects of the embodiments of the present application, the following comparative examples are set forth.
Comparative example 1
The differences from example 1 are: and bonding the glass block with proper size with the ceramic matrix with the cavity structure by using an adhesive to obtain the glass ceramic composite material with the thickness of 1 mm.
The following tests were performed on the glass ceramic composites prepared in the above examples and comparative examples:
(1) Appearance test: under the standard light source condition, quality staff detects the appearance of the glass part by naked eyes and observes whether bubbles exist at interfaces of glass, glass and ceramic matrix in the glass ceramic composite material. The test standard refers to a method for testing the transmittance of the light-transmitting fine ceramic of the JCT 2020-2010. The test results are summarized in table 1.
(2) And (3) binding force test: the glass ceramic composite material with the thickness of 1mm is fixed on a jig, and a downward acting force is applied to the glass part of the glass ceramic composite material by using a universal testing machine until the glass is broken or the glass falls off from the glass ceramic composite material. And recording the maximum force value applied by the universal testing machine in the process, wherein the maximum force value is the bonding strength between the ceramic matrix and the glass. The results are summarized in table 1.
Table 1 summary of test results for glass ceramic composites prepared in each of the examples and comparative examples
| Experiment number | Bond strength/kgf | Transmittance of glass portion | Bubble detection result |
| Example 1 | 11.5 | 91％ | No bubbles visible to naked eyes |
| Example 2 | 11.3 | 90％ | No bubbles visible to naked eyes |
| Example 3 | 10.2 | 90％ | No bubbles visible to naked eyes |
| Example 4 | 10.5 | 90％ | No bubbles visible to naked eyes |
| Example 5 | 11.6 | 85％ | No bubbles visible to naked eyes |
| Comparative example 1 | 6 | 90％ | No bubbles visible to naked eyes |
As can be seen from the data in table 1, the glass-ceramic composites provided in examples 1-5 of the present application have much greater bonding strength than comparative example 1, and the transmittance of the glass in the glass-ceramic composites provided in the present application is comparable to that of comparative example 1.
While the foregoing is directed to exemplary embodiments of the present application, it will be appreciated by those of ordinary skill in the art that numerous modifications and variations can be made thereto without departing from the principles of the present application, and such modifications and variations are to be regarded as being within the scope of the present application.
Claims (10)
1. A glass-ceramic composite comprising a ceramic matrix having a cavity, and glass filled in the cavity, the ceramic matrix being integrally formed with the glass; wherein the material of the ceramic matrix comprises yttrium stabilized zirconia.
2. The glass-ceramic composite of claim 1, wherein the glass has a coefficient of thermal expansion of 7 x 10 -6 /℃-11×10 -6 /℃。
3. The glass-ceramic composite according to any one of claims 1 to 2, wherein the glass comprises the following components in parts by weight: 0-10 parts of aluminum oxide, 55-70 parts of silicon oxide, 0-10 parts of magnesium oxide, 10-20 parts of boron oxide and 15-25 parts of sodium oxide.
4. The glass-ceramic composite of claim 1, wherein no bubbles are visible to the naked eye within the glass.
5. The glass-ceramic composite of claim 1, wherein the glass has a visible light transmittance of not less than 85%.
6. The glass-ceramic composite according to claim 1, wherein the bonding strength between the ceramic matrix and the glass is 10Kgf-12Kgf.
7. A method for preparing a glass ceramic composite material, comprising the steps of:
(1) Forming a ceramic raw material into a ceramic matrix blank, and sequentially degreasing and sintering the ceramic matrix blank to prepare a ceramic matrix with a cavity structure; wherein the ceramic raw material comprises yttrium-stabilized zirconia;
(2) Filling glass raw materials into the cavity structure of the ceramic matrix, sintering in a sintering furnace, and cooling to room temperature to obtain the glass ceramic composite material as claimed in any one of claims 1-6.
8. The method according to claim 7, wherein in the step (2), the sintering is performed at a temperature of 1000 ℃ to 1400 ℃ for a time of 0.5 to 4 hours.
9. The method according to claim 7, wherein in the step (1), a ceramic raw material is molded into the ceramic base blank having the cavity structure, or holes are made in the ceramic base blank after the sintering treatment to obtain the ceramic base having the cavity structure.
10. An electronic device having the glass-ceramic composite material according to any one of claims 1 to 6.
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