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CN109650720B - Mobile terminal glass back cover substrate and production method thereof - Google Patents

Mobile terminal glass back cover substrate and production method thereof Download PDF

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Publication number
CN109650720B
CN109650720B CN201910029634.2A CN201910029634A CN109650720B CN 109650720 B CN109650720 B CN 109650720B CN 201910029634 A CN201910029634 A CN 201910029634A CN 109650720 B CN109650720 B CN 109650720B
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glass
temperature
raw materials
mold
batch
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CN109650720A (en
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胡勇波
肖调坤
郑卓群
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Ningbo Meishan Free Trade Port Litai Enterprise Management Partnership LP
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Ningbo Xingshu New Energy Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/076Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/095Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/06Other 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
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • C03B25/02Annealing glass products in a discontinuous way
    • C03B25/025Glass sheets
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B33/00Severing cooled glass
    • C03B33/02Cutting or splitting sheet glass or ribbons; Apparatus or machines therefor
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/04Opacifiers, e.g. fluorides or phosphates; Pigments
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/076Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a mobile terminal glass back cover substrate and a production method thereof. The invention has simple production process, convenient operation, high dimensional precision, high production efficiency, high qualification rate, stable quality and low cost, can be used for large-scale industrial production, and is particularly suitable for producing the 5G mobile terminal glass back cover substrate with high strength, high toughness and lighter weight.

Description

Mobile terminal glass back cover substrate and production method thereof
Technical Field
The invention relates to the field of mobile terminal parts, in particular to a mobile terminal glass back cover substrate and a production method thereof.
Background
Glass belongs to the material applied to the back cover of the mobile phone earlier, but because the traditional glass material has lower strength, the glass is very easy to cause breakage, cracks or scratches in daily use processes of falling, collision, scraping and the like, and is quickly replaced by metal. Through development for many years, the performance of the glass is greatly improved, the problems of fragility, scratching and the like are basically solved, and the advantages of the glass compared with a metal material begin to appear. Because of the characteristic that glass is softened by heating, the glass can be easily processed into a curved surface shape by heating, and the cost is greatly reduced compared with that of a metal material. With the coming of 5G communication and the gradual popularization of wireless charging, the signal shielding defect of the metal back cover is obvious, and the demetalization of the mobile phone back cover is a great trend. The glass scheme has high maturity and lower cost, and is expected to become a mainstream scheme of medium and high-end models. The double vitrification of the cover plate (the panel and the back plate) of the mobile phone can drive the rapid explosion of the industry scale.
Currently, the mainstream production process of the glass back cover substrate of the mobile terminal adopts an overflow down-draw process: when the molten glass liquid fills the whole tank body, the excessive glass liquid overflows from the edge of the tank and is collected at the bottom of the tank to form a plane and flows downwards to form an uninterrupted thin sheet. In this process, engineers use advanced processes and highly automated equipment to shape the glass in air and then stretch it into a thin, flat piece of glass. However, it is difficult to produce thin glass sheet products with high yield and flatness using the fusion overflow downdraw process. Many experts have overcome many technical and process problems that may affect process stability during the formation of thin glass sheets over the years, but only two or three companies have been able to industrialize the "overflow downdraw" process worldwide to date.
The other mainstream process is to prepare the thin glass plate by using a float process, and has obvious advantages, such as easy scientific management, realization of full-line mechanization and automation and high labor productivity; the continuous operation period can be as long as several years, which is beneficial to stable production, but the investment of disposable equipment is large, the cost of the kiln is high, and the strength and the toughness of the produced glass are poor.
No matter the 'overflow down-draw' process or the 'float process', the method has strict requirements on the components of the glass raw materials so as to ensure that the molten glass has good material property, namely the fluidity of the molten glass, but the glass with good material property has poor strength; in order to improve the glass strength and meet the requirements of the glass back cover of the mobile terminal, the content of aluminum in the glass raw material (i.e., "high-alumina glass") is generally increased. However, high-alumina glass has high strength, but has poor material properties, and the high aluminum content is not favorable for homogenization and clarification of glass melt and for realization of overflow down-draw or float process, and the 'fragile' back cover of the mobile terminal glass is caused by the fact that the aluminum content in the raw materials cannot be too high.
Along with the improvement of aesthetic appearance and performance requirements of people on intelligent terminal products, back covers of mobile terminals such as mobile phones gradually transition from a plane to a 2.5D curved surface and a 3D curved surface. The 3D curved surface back cover requires the glass substrate to be light and thin, scratch-resistant, fall-resistant and capableThe plasticity is strong, so higher requirements are put forward on the formula regulation and processing technology of the glass raw materials. Conventional glass production processes are only suitable for making glass substrates of relatively fixed chemical composition, for example, glass produced by the float process, which has a composition of high calcium, medium magnesium, low aluminum, and micro-iron. The glass back cover of the mobile terminal is generally made of high-alumina glass, the mechanical strength of the glass can be improved by introducing aluminum, and the Al2O3Is around 13% and even higher, it is clear that the float process is not the best option. The introduction of other components affects the material property (or viscosity) and surface tension of the molten glass, and thus affects the shrinkage, thickness and uniformity during molding. Thus, the "overflow downdraw" process and the "float" process are not necessarily suitable for making functional glasses containing certain special components, such as ceramic toughened glass.
Disclosure of Invention
The invention provides a glass back cover substrate of a mobile terminal and a production method thereof to solve the technical problems.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
according to a first aspect of the embodiments of the present invention, there is provided a glass back cover substrate for a mobile terminal, comprising the following raw materials by weight: SiO 22 40-60%、Na2O 0-5%、CaO 0-10%、Al2O315-35% of MgO, 0-10% of MgO; and 5-45% of additive.
Preferably, the additive comprises TiO2、ZrO2、K2O、B2O3、BaO、ZnO、Y2O3、Ce2O3And Li2O, wherein the components account for the following weight percentage: b is2O3 0-15%、BaO 0-5%、ZnO 0-10%、Y2O3 0-5%、Ce2O3 0-5%、Li2O 0-5%、TiO2 0-5%、ZrO2 0-5%、K2O 0-5%。
Preferably, the dye further comprises an ionic colorant, and the ionic colorant comprises Mn2O3、CoO、Co3O4、Cr2O3One or more ionic coloring agents, wherein the ionic coloring agent accounts for 2 to 8 percent of the total weight.
According to a second aspect of the embodiments of the present invention, there is provided a method for producing a glass back cover substrate of a mobile terminal, comprising the steps of:
(1) preparing raw materials: weighing the following raw materials in percentage by weight, SiO2 40-60%、Na2O 0-5%、CaO 0-10%、Al2O315-35% of MgO, 0-10% of MgO; and 5-45% of additive;
(2) processing raw materials: purifying, crushing and screening the obtained raw materials to obtain raw material particles with the particle size of 0.10 micrometer to 0.80 millimeter;
(3) preparing a batch: grinding and mixing the obtained raw material particles into a mixed material of uniformly mixed powder by a ball mill, wherein the particle size of the mixed material after ball milling and screening is between 0.2 micron and 0.1 millimeter;
(4) preparing a glass ingot: preparing the batch into a microcrystalline glass ingot by a crucible breaking method, a model casting method or a secondary forming and sintering method;
(5) multi-wire cutting of diamond wires: the glass ingot is cut into a glass substrate with the thickness of 0.08-2.0 mm by a cutting machine, the cutting linear speed during cutting is 600-3000 m/min, and the cutting processing time is 10-900 min.
Preferably, the additive in step (1) comprises TiO2、ZrO2、K2O、B2O3、BaO、ZnO、Y2O3、Ce2O3And Li2O, wherein the components account for the following weight percentage: b is2O3 0-15%、BaO 0-5%、ZnO 0-10%、Y2O3 0-5%、Ce2O3 0-5%、Li2O 0-5%、TiO2 0-5%、ZrO2 0-5%、K2O 0-5%。
Preferably, the raw material in the step (1) further comprises an ionic colorant, and the ionic colorant accounts for 2 to 8 percent of the total weight.
Preferably, the crucible breaking method in the step (4) comprises the following specific steps: putting the batch mixture into a high-temperature-resistant mold, leveling and compacting, putting the batch mixture and the mold into a high-temperature furnace, heating to 800-900 ℃ at a heating rate of 7-15 ℃/min, preserving heat for 0.5-1.5 hours, continuously heating to 1450-1600 ℃ at a heating rate of 2-7 ℃/min, and preserving heat for 2-3 hours; generating molten glass under the action of high temperature, and removing the molten glass from the high-temperature furnace along with the mold after full melting, defoaming and clarification; and putting the cooled mold melted with the molten glass into an annealing furnace with the temperature raised to 400-700 ℃, annealing and preserving heat for 2-3 hours, then naturally cooling, and disassembling the mold to obtain a glass ingot.
Preferably, the annealed mold is transferred to a crystallization furnace with the crystallization temperature of 700-1000 ℃ to complete crystallization, and after the temperature is slowly reduced to the room temperature, the mold is disassembled to take out the glass ingot.
As another preferable mode, the specific steps of the mold casting method in the step (4) are as follows: putting the batch into a glass furnace, heating to 1000 ℃ at the heating rate of 7-15 ℃/min, preserving heat for 1.5 hours, then continuously heating to 1480 ℃ at the heating rate of 2-7 ℃/min, preserving heat for 3 hours, and generating uniform and viscous glass liquid under the action of high temperature; then pouring the molten glass into a mold preheated to 500-550 ℃, and cooling; and putting the cooled mold injected with the molten glass into an annealing furnace with the temperature raised to 400-700 ℃, annealing and preserving the heat for 30-300 minutes, then naturally cooling, and disassembling the mold to obtain the glass ingot.
Preferably, the annealed die is placed in a crystallization furnace preheated to the crystallization temperature of 700-900 ℃ for crystallization for 60-600 minutes; and finally, slowly cooling to room temperature according to a certain temperature system, removing the mold and taking out the microcrystalline glass ingot.
As still another preferable mode, the specific steps of the secondary forming and sintering method in the step (4) are as follows: (A) water quenching, crushing and ball milling: putting the batch mixture into a glass melting furnace, electrifying, heating to 1000 ℃ at the heating rate of 7-15 ℃/min, preserving heat for 1.5 hours, then continuously heating to 1550 ℃ at the heating rate of 2-7 ℃/min, preserving heat for 2.5 hours, and forming high-temperature molten glass under the action of high temperature; pouring the glass liquid into a container filled with clear water to form water-quenched glass particles, draining, drying, crushing, and ball-milling until the average particle size is less than 0.20 mm to prepare glass fine powder;
(B) pressing a glass ingot blank under high pressure: placing the glass fine powder into a mold, pressing by a 70MPa oil press, maintaining the pressure for 15 minutes, and demolding to obtain a glass ingot blank;
(C) and (3) firing a glass ingot: placing the glass ingot blank in a high-temperature furnace, continuously heating to 600 ℃ at the heating speed of 7-15 ℃/min, and preserving heat for 0.5-1 hour; then, continuously heating to 1010-1400 ℃ at the heating rate of 2-7 ℃/min, preserving heat for 2.5 hours, and sintering to form porcelain; then cooling to the crystallization temperature of 500-1000 ℃ at the cooling rate of 2-7 ℃/min for thorough crystallization, and preserving the heat for 3 hours; and naturally cooling to room temperature to obtain the glass ingot.
Preferably, in the step (B), a toughening material is added to the fine glass powder, the mixture is fully and uniformly mixed, and then the mixture is placed in a mold for pressing, wherein the weight percentage of the toughening material is 5-25%.
Preferably, the toughening material comprises one or more of zirconia powder, zirconia fiber or whisker and silicon carbide fiber or whisker.
Preferably, the length of an inner cavity of the used mold is 10-2000 mm, the width of the section of the inner cavity is 10-300 mm, and the height of the section of the inner cavity is 50-500 mm.
Preferably, the material of the mold is alumina, graphite, silicon carbide, or heat-resistant alloy steel.
Compared with the prior art, the mobile terminal glass back cover with high strength, high toughness, high scratch resistance and thinness is realized by designing the high-strength glass formula, and the problem that the mass production cannot be realized by adopting the traditional process for the high-strength glass formula is solved.
Drawings
Fig. 1 is a schematic flow chart of a method for producing a glass back cover substrate for a mobile terminal according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments shown in the drawings. These embodiments are not intended to limit the present invention, and structural, methodological, or functional changes made by those skilled in the art according to these embodiments are included in the scope of the present invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.
In a first aspect of the embodiments of the present invention, a glass back cover substrate for a mobile terminal is provided, which comprises the following raw materials by weight: SiO 22 40-60%、Na2O 0-5%、CaO 0-10%、Al2O315-35% of MgO, 0-10% of MgO; and 5-45% of additive.
The components are analyzed, synthesized and designed according to the performance requirements of lightness, thinness, scratch resistance, falling resistance, strong plasticity and the like by utilizing the existing materials, scientific knowledge and practical experience. SiO 22、Na2O、CaO、Al2O3MgO as a basic component, and introducing certain special raw materials for obtaining the necessary strength, toughness and scratch resistance of the glass.
Wherein the additive may comprise TiO2、ZrO2、K2O、B2O3、BaO、ZnO、Y2O3、Ce2O3And Li2O, wherein the components account for the following weight percentage: b is2O3 0-15%、BaO 0-5%、ZnO 0-10%、Y2O30-5%、Ce2O3 0-5%、Li2O 0-5%、TiO2 0-5%、ZrO2 0-5%、K20 to 5 percent of O. In addition, Sb may be added2O5、P2O5SiC and CeO2And the like. By addingThe toughening agent can realize the high-toughness mobile terminal glass back cover.
In particular, ionic colorants comprising Mn may also be included2O3、CoO、Co3O4、Cr2O3One or more of them. Through adding the ion colouring material, richen cell-phone back of the body lid colour, satisfy different consumer groups' demand: mn may be added if purple color is required2O3CoO can be added when sky blue is needed, and Co can be added when grey is needed3O4Cr may be added if green color is required2O3And the like. The ionic colorant typically comprises 2 to 8 weight percent of the total weight.
In a second aspect of the embodiments of the present invention, a method for producing a glass back cover substrate of a mobile terminal is provided, as shown in fig. 1, including the following steps:
(1) preparing raw materials: weighing the following raw materials in percentage by weight, SiO2 40-60%、Na2O 0-5%、CaO 0-10%、Al2O315-35% of MgO, 0-10% of MgO; and 5-45% of additive. Wherein the additive may comprise TiO2、ZrO2、K2O、B2O3、BaO、ZnO、Y2O3、Ce2O3And Li2O, wherein the components account for the following weight percentage: b is2O3 0-15%、BaO 0-5%、ZnO 0-10%、Y2O3 0-5%、Ce2O3 0-5%、Li2O 0-5%、TiO2 0-5%、ZrO2 0-5%、K2O 0-5%。
The raw materials can also comprise an ion coloring agent so as to enrich the color of the back cover of the mobile terminal and meet the requirements of different consumer groups. For example, Mn is added for purple2O3CoO is added for sky blue, and Co is added for gray3O4Cr is added for green2O3And the like.
(2) Processing raw materials: purifying, crushing and screening the obtained raw materials to obtain raw material particles with the particle size of 0.10 micron-0.80 mm.
In order to facilitate material flow, uniformly mix and accelerate the melting speed of the raw materials, the raw materials are processed, including the working procedures of purification, crushing/ball milling, screening and the like; in general, glass production requires that the raw materials have a particle size of between 0.10 microns and 0.80 mm, preferably between 0.20 microns and 0.10 mm.
(3) Preparing a batch: and grinding and mixing the obtained raw material particles by a ball mill to obtain a batch of uniformly mixed powder, wherein the particle size of the batch after ball milling and screening is between 0.2 micrometer and 0.1 millimeter.
(4) Preparing a glass ingot: the glass ingot of the microcrystal is prepared from the batch by a crucible breaking method, a model casting method or a secondary forming and sintering method.
No matter the crucible breaking method, the model pouring method or the secondary forming and sintering method for preparing the glass ingot, the process system of controlling the particle size of materials, uniformly mixing materials and strictly controlling the temperature is required. Through crystallization treatment, the mobile terminal glass back cover with high strength, high toughness and high scratch resistance can be realized.
The first method is a crucible breaking method, and comprises the following specific steps:
putting the batch mixture into a high-temperature-resistant mold, leveling and compacting, putting the batch mixture and the mold into a high-temperature furnace, heating to 800-900 ℃ at a heating rate of 7-15 ℃/min, preserving heat for 0.5-1.5 hours, continuously heating to 1450-1600 ℃ at a heating rate of 2-7 ℃/min, and preserving heat for 2-3 hours; generating molten glass under the action of high temperature, and removing the molten glass from the high-temperature furnace along with the mold after full melting, defoaming and clarification; and putting the cooled mold melted with the molten glass into an annealing furnace with the temperature raised to 400-700 ℃, annealing and preserving heat for 2-3 hours, then naturally cooling, and disassembling the mold to obtain a glass ingot.
In order to obtain better strength and toughness performance, the annealed mold can be transferred to a crystallization furnace with the crystallization temperature of 700-1000 ℃ to complete crystallization, and after the temperature is slowly reduced to the room temperature, the mold is disassembled to take out the glass ingot.
In addition, the crucible breaking method can also adopt another mode:
putting the batch mixture into a high-temperature-resistant mold, leveling and compacting, putting the batch mixture and the mold into a high-temperature furnace, generating glass liquid under the action of high temperature, fully melting, defoaming and clarifying the glass liquid, cooling the glass liquid to a crystallization temperature in the high-temperature furnace according to a proper temperature, fully crystallizing the glass liquid, and then slowly cooling the glass liquid to room temperature according to a certain temperature system; and finally, crushing the die and taking out the microcrystalline glass ingot.
The second method is a model casting method, and comprises the following specific steps:
putting the batch into a glass furnace, heating to 1000 ℃ at the heating rate of 7-15 ℃/min, preserving heat for 1.5 hours, then continuously heating to 1480 ℃ at the heating rate of 2-7 ℃/min, preserving heat for 3 hours, and generating uniform and viscous glass liquid under the action of high temperature; then pouring the molten glass into a mold preheated to 500-550 ℃, and cooling; and putting the cooled mold injected with the molten glass into an annealing furnace with the temperature raised to 400-700 ℃, annealing and preserving the heat for 30-300 minutes, then naturally cooling, and disassembling the mold to obtain the glass ingot.
In order to obtain better strength and toughness performance, the annealed die can be placed in a crystallization furnace preheated to the crystallization temperature of 700-900 ℃ for crystallization treatment, and the crystallization time is 60-600 minutes; and finally, slowly cooling to room temperature according to a certain temperature system, removing the mold and taking out the microcrystalline glass ingot.
The third method is a secondary forming and sintering method, which comprises the following steps:
(A) water quenching, crushing and ball milling: putting the batch mixture into a glass melting furnace, electrifying, heating to 1000 ℃ at the heating rate of 7-15 ℃/min, preserving heat for 1.5 hours, then continuously heating to 1550 ℃ at the heating rate of 2-7 ℃/min, preserving heat for 2.5 hours, and forming high-temperature molten glass under the action of high temperature; pouring the glass liquid into a container filled with clear water to form water-quenched glass particles, draining, drying, crushing, and ball-milling until the average particle size is less than 0.20 mm to prepare glass fine powder;
(B) pressing a glass ingot blank under high pressure: placing the glass fine powder into a mold, pressing by a 70MPa oil press, maintaining the pressure for 15 minutes, and demolding to obtain a glass ingot blank;
(C) and (3) firing a glass ingot: placing the glass ingot blank in a high-temperature furnace, continuously heating to 600 ℃ at the heating speed of 7-15 ℃/min, and preserving heat for 0.5-1 hour; then, continuously heating to 1010-1400 ℃ at the heating rate of 2-7 ℃/min, preserving heat for 2.5 hours, and sintering to form porcelain; then cooling to the crystallization temperature of 500-1000 ℃ at the cooling rate of 2-7 ℃/min for thorough crystallization, and preserving the heat for 3 hours; and naturally cooling to room temperature to obtain the glass ingot.
Particularly, in the step (B), the toughening material is added into the fine glass powder, the mixture is fully and uniformly mixed, and then the mixture is placed into a die for pressing, wherein the weight percentage of the toughening material is 5-25%. Wherein, the toughening material comprises one or more of zirconia powder, zirconia fiber or whisker and silicon carbide fiber or whisker.
In the method for preparing the glass ingots, the used mould is designed into a certain shape and size according to actual requirements, and the surface of the inner cavity of the mould is sprayed with a high-temperature resistant release agent to prevent adhesion. The shape of the mould is a cuboid, the size of the section width and the height of the inner cavity of the mould is determined by the specification and the requirement of the back cover provided by a mobile equipment manufacturer, and a machining allowance is properly reserved; the length of the die is determined by the equipment used in the subsequent diamond wire multi-wire cutting process. According to the preferable technical scheme, the length of an inner cavity of the mold is 10-2000 mm, and preferably 100-1200 mm; the cross section width of the inner cavity of the mold is 10-300 mm, preferably 50-250 mm; the height of the section of the inner cavity of the mold is 50-500 mm, and preferably 100-300 mm. The material of the die is preferably a high-temperature resistant inorganic material such as alumina, graphite or silicon carbide, or a high-temperature resistant metal material such as heat-resistant alloy die steel. The length of the inner cavity is 10-2000 mm, the width of the section of the inner cavity is 10-300 mm, and the height of the section of the inner cavity is 50-500 mm. By changing the size of the glass ingot mold, the requirement that the glass back covers of mobile terminals with various specifications and sizes are thinner can be met.
(5) Multi-wire cutting of diamond wires: the glass ingot is cut into a glass substrate with the thickness of 0.08-2.0 mm by a cutting machine, the cutting linear speed during cutting is 600-3000 m/min, and the cutting processing time is 10-900 min.
The diamond wire cutting has the characteristics of high cutting speed, high cutting precision, low material loss and the like, the diamond wire multi-wire cutting technology is applied to the field of processing of the glass back cover of the mobile terminal, the requirements of the market on lower cost, higher size progress and higher production efficiency can be met, and the diamond wire cutting is particularly suitable for cutting toughened glass sheets with thinner and thinner thickness. Preferably, the thickness of the glass back cover substrate of the mobile terminal subjected to diamond wire multi-wire cutting is 0.08-2 mm, and preferably 0.30-1.00 mm; the slicing time is 10 to 900 minutes, preferably 30 to 600 minutes. The type of the diamond wire is not limited, the diamond wire can be a resin bonded diamond wire or an electroplated diamond wire, and the diameter of the diamond wire is 9-1000 micrometers, preferably 30-600 micrometers; generally, the cutting speed is 600 to 3000 m/min.
Subsequent work, including inspection and further processing: the inspection comprises the items of detecting point defects, linear defects, dirt, shrinkage rate and the like, and testing the hardness of the toughened glass; deep processing, namely processing the glass substrate into 2.5D and 3D glass back cover finished products, wherein the process is the same as the process for processing and treating the glass substrate by using common plate glass or float glass or overflow downdraw glass, and the process flow mainly comprises the following steps: engineering → open material and open hole → fine carving → grinding → cleaning → hot bending → polishing → detection → tempering → UV transfer → coating film (PVD) → printing (silk screen printing, spray coating, UV machine light curing) → laminating → pasting → packaging, etc.
The following describes a method for producing a glass back cover substrate for a mobile terminal with reference to specific embodiments.
Example 1.
(1) Preparing raw materials: comprises the following components in percentage by mass: SiO 22 50.0%、Na2O 5.0%、Al2O3 15.0%、MgO 5.0%、CaO 5.0%、B2O3 10.0%、BaO 2.0%、ZnO 5.0%、Y2O3 1.0%、Ce2O3 1.0%, Li2O 1.0%。
(2) Processing raw materials: purifying, crushing and screening the raw materials, wherein the particle size of each raw material is not more than 0.80 mm.
(3) Preparation of the batch: accurately weighing the raw materials according to the mass percentage in the component design, grinding the raw materials into finer powder by a ball mill, and mixing the raw materials to obtain uniform mixed powder; the particle size of the batch after ball milling and screening is less than 0.0635 mm.
(4) Preparing a glass ingot: a crucible breaking method.
The die cavity size was 530 mm 80 mm 180 mm.
Melting: filling the empty mold with the batch, leveling, compacting, placing the mold in an electric furnace, electrifying the electric furnace, heating to 900 ℃ at a heating rate of 8 ℃/min, keeping the temperature for 0.5 hour, continuing to heat to 1450 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2 hours; the mold was then removed from the furnace.
Annealing: and putting the cooled mold with the molten glass into an annealing furnace with the temperature raised to 500 ℃, closing the door of the annealing furnace, preserving the heat for 2 hours, and cutting off the power to naturally cool the mold to obtain the cuboid glass ingot.
(5) Multi-wire cutting of diamond wires: in the embodiment, the model of the cutting machine is QPJ1660B/C, the diameter of the diamond wire is 200 microns, the groove pitch of the diamond wire is adjusted to 0.70 mm according to the product specification and the processing requirement, the glass ingot is cut into the mobile terminal glass back cover substrate with the thickness of 0.50 mm, the cutting line speed is 1600 m/min, and the processing time is not more than 4 hours.
The average thickness of the finally obtained mobile terminal glass back cover substrate is 0.501 mm.
Example 2.
(1) Preparing raw materials: according to the mass percentage, comprises SiO2 53.0%、Al2O3 22.0%、MgO 5.0%、CaO 5.0%、B2O3 10.0%、BaO 2.0%、Li2O 1.0%、Mn2O3 2.0 percent. Wherein Mn is2O3Is an ionic colorant to make the back cover of the mobile terminal appear purple.
(2) Processing raw materials: purifying, crushing, ball milling, screening the raw materials, wherein the particle size of the screened raw materials is less than 0.085 mm.
(3) Preparation of the batch: accurately weighing the raw materials according to the mass percentage in the component design, and fully mixing the raw materials by a V-shaped mixer to obtain uniform batch.
(4) Preparing a glass ingot: a crucible breaking method.
The die cavity size was 750 mm 80 mm 180 mm.
Melting: filling the empty mold with the batch, leveling, compacting, placing the mold in an electric furnace, electrifying the electric furnace, heating to 1000 ℃ at a heating rate of 8 ℃/min, keeping the temperature for 1.5 hours, then continuously heating to 1600 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 3 hours; the mold was then removed from the furnace.
Annealing: and putting the cooled mold with the molten glass into an annealing furnace with the temperature raised to 550 ℃, closing the door of the annealing furnace, preserving the heat for 2 hours, and cutting off the power to naturally cool the mold to obtain the cuboid glass ingot.
(5) Multi-wire cutting of diamond wires: in this embodiment, the model of the cutting machine is QPJ1660B/C (great company city), the diameter of the diamond wire is 200 micrometers, the groove pitch of the diamond wire is adjusted to 0.95 mm according to the product specification and the processing requirement, the glass ingot is cut into a mobile terminal glass back cover substrate with the thickness of 0.70 mm, the cutting line speed is 1600 m/min, and the processing time is not more than 4 hours.
The average thickness of the finally obtained mobile terminal glass back cover substrate is 0.698 mm.
Example 3.
(1) Preparing raw materials: comprises the following components in percentage by mass: SiO 22 60.0%、Al2O3 15.0%、MgO 5.0%、CaO 5.0%、ZnO5.0%、Y2O3 5.0%、Li2O 5.0%。
(2) Processing raw materials: purifying, crushing and screening the raw materials, wherein the particle size of each raw material is not more than 0.80 mm.
(3) Preparation of the batch: accurately weighing the raw materials according to the mass percentage in the component design, grinding the raw materials into finer powder by a ball mill, and mixing the raw materials to obtain uniform mixed powder; the particle size of the batch after ball milling and screening is less than 0.0635 mm.
(4) Preparing a glass ingot: a crucible breaking method.
The die cavity size was 680 mm 80 mm 180 mm.
Melting: filling the empty mold with the batch, leveling, compacting, placing the mold in an electric furnace, electrifying the electric furnace, heating to 800 ℃ at a heating rate of 8 ℃/min, keeping the temperature for 1.5 hours, continuing to heat to 1500 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 2 hours; the mold was then removed from the furnace.
Annealing: and putting the cooled mold with the molten glass into an annealing furnace with the temperature raised to 500 ℃, closing the door of the annealing furnace, preserving the heat for 2 hours, and cutting off the power to naturally cool the mold to obtain the cuboid glass ingot.
(5) Multi-wire cutting of diamond wires: in the embodiment, the model of the cutting machine is QPJ1660B/C (Dalianliancheng), the diameter of the diamond wire is 250 micrometers, the groove pitch of the diamond wire is adjusted to 1.25 millimeters according to the product specification and the processing requirement, the glass ingot is cut into mobile phone glass sheets with the thickness of 0.90 millimeters, the cutting speed is 2000 meters/minute, and the processing time is not more than 3.5 hours.
The average thickness of the finally obtained mobile terminal glass back cover substrate is 0.901 mm.
Example 4.
(1) Preparing raw materials: comprises the following components in percentage by mass: SiO 22 45.0%、Al2O3 25.0%、Na2O 5.0%、MgO 2.0%、B2O3 15.0%、ZrO21.5%、ZnO 5%、Li2O1.5%, etc.
(2) Processing raw materials: purifying, crushing, ball milling and screening the raw materials to ensure that the particle size of each raw material is not more than 0.127 mm.
(3) Preparation of the batch: accurately weighing the raw materials according to the mass percentage in the component design, and fully mixing the raw materials by a V-shaped mixer to obtain uniform batch.
(4) Preparing a glass ingot: and (3) a mold casting method.
The die cavity size was 330 mm 75 mm 150 mm.
Melting: the molding process of a 'model pouring method' is adopted, the batch is put into a glass melting furnace and the melting furnace is electrified, the temperature is raised to 1000 ℃ at the temperature raising speed of 8 ℃/min, the temperature is kept for 1.5 hours, the temperature is raised to 1480 ℃ at the temperature raising speed of 5 ℃/min, and the temperature is kept for 3 hours; the high temperature molten glass is then poured into a mold preheated to 500 ℃.
Annealing: and putting the cooled mold filled with the glass liquid into an annealing furnace with the temperature raised to 550 ℃, closing the door of the annealing furnace, preserving the heat for 3 hours, cutting off the power, naturally cooling the mold, and disassembling the mold to obtain the cuboid glass ingot.
(5) Multi-wire cutting of diamond wires: in the embodiment, the model of the cutting machine is QPJ1660B/C (Dalian Liancheng city), the diameter of the diamond wire is 200 microns, the groove pitch of the diamond wire is adjusted to 0.85 mm according to the product specification and the processing requirement, the glass ingot is cut into mobile phone glass sheets with the thickness of 0.60 mm, the cutting line speed is 1600 m/min, and the processing time is not more than 4 hours.
The final obtained glass back cover substrate of the mobile terminal has an average thickness of 0.602 mm.
Example 5.
(1) Preparing raw materials: comprises the following components in percentage by mass: SiO 22 55.4%、Na2O 5.0%、Al2O3 22.0%、MgO 3.0%、B2O3 10.6%、Ce2O3 1.5%、Li2O 2.5%。
(2) Processing raw materials: purifying, crushing, ball milling and screening the raw materials to ensure that the particle size of each raw material is not more than 0.127 mm.
(3) Preparation of the batch: accurately weighing the raw materials according to the mass percentage in the component design, and fully mixing the raw materials by a V-shaped mixer to obtain uniform batch.
(4) Preparing a glass ingot: and (3) a mold casting method.
The die cavity size was 330 mm 75 mm 150 mm.
Water quenching, crushing and ball milling: putting the batch into a glass furnace, electrifying the furnace, heating to 1000 ℃ at the heating rate of 8 ℃/min, preserving heat for 1.5 hours, then continuously heating to 1550 ℃ at the heating rate of 5 ℃/min, preserving heat for 2.5 hours, and forming high-temperature glass liquid; pouring the high-temperature glass liquid into a container filled with clean water to form water-quenched glass particles, draining, drying, crushing, and ball-milling until the average particle size is less than 0.072 mm to prepare glass fine powder.
Pressing a glass ingot blank under high pressure: and (3) placing the glass fine powder into high-strength alloy die steel, pressing by using a 70MPa oil press, maintaining the pressure for 15 minutes, and removing the die to obtain a glass ingot blank.
And (3) firing a glass ingot: placing the glass ingot blank in a high-temperature furnace, continuously heating to 600 ℃ at the heating rate of 8 ℃/min, and keeping the temperature for 0.5 h; then continuously heating to 1010 ℃ at the heating rate of 5 ℃/min, and preserving heat for 2.5 hours; then the temperature is reduced to 780 ℃ at the cooling speed of 5 ℃/min, and the temperature is preserved for 3 hours; and turning off the power supply, and naturally cooling to room temperature in the furnace to obtain the microcrystalline ceramic glass ingot.
(5) Multi-wire cutting of diamond wires: in this embodiment, the model of the cutting machine is QPJ1660B/C (great company city), the diameter of the diamond wire is 200 micrometers, the groove pitch of the diamond wire is adjusted to 0.85 mm according to the product specification and the processing requirement, the glass ingot is cut into a mobile terminal glass back cover substrate with the thickness of 0.60 mm, the cutting line speed is 1600 m/min, and the processing time is not more than 4 hours.
The final mobile terminal glass back cover substrate obtained has an average thickness of 0.601 mm.
Example 6.
(1) Preparing raw materials: comprises the following components in percentage by mass: SiO 22 60.0%、Na2O 5.0%、Al2O3 21.0%、CaO 3.1%、MgO 4.2%、TiO2 0.8%、K2O 2.5%、ZrO2 3.0%、Ce2O30.4%, etc.
(2) Processing raw materials: purifying, crushing, ball milling and screening the raw materials to ensure that the particle size of each raw material is not more than 0.127 mm.
(3) Preparation of the batch: accurately weighing the raw materials according to the mass percentage in the component design, and fully mixing the raw materials by a V-shaped mixer to obtain uniform batch.
(4) Preparing a glass ingot: secondary forming and sintering.
The die cavity size was 330 mm 75 mm 150 mm.
Water quenching, crushing and ball milling: putting the batch into a glass furnace, electrifying the furnace, heating to 1000 ℃ at the heating rate of 8 ℃/min, preserving heat for 1.5 hours, then continuously heating to 1550 ℃ at the heating rate of 5 ℃/min, preserving heat for 2.5 hours, and forming high-temperature glass liquid; pouring the high-temperature glass liquid into a container filled with clean water to form water-quenched glass particles, draining, drying, crushing, and ball-milling until the average particle size is less than 0.072 mm to prepare glass fine powder.
Pressing a glass ingot blank under high pressure: weighing nano ZrO2 fiber according to the mass percent of 8.5%, adopting a V-shaped mixer to fully and uniformly mix the glass fine powder and the ZrO2 fiber, then placing the mixture into a high-strength alloy die, pressing the mixture by a 70MPa oil press, maintaining the pressure for 15 minutes, and removing the die to obtain a glass ingot blank.
And (3) firing a glass ingot: placing the glass ingot blank in a high-temperature furnace, continuously heating to 600 ℃ at the heating rate of 8 ℃/min, and preserving heat for 1 hour; then continuously heating to 1075 ℃ at the heating rate of 5 ℃/min, and preserving heat for 3 h; then the temperature is reduced to 780 ℃ at the cooling speed of 5 ℃/min, and the temperature is preserved for 3 hours; and turning off the power supply, and naturally cooling to room temperature in the furnace to obtain the ZrO2 fiber toughened microcrystalline ceramic glass ingot.
(5) Multi-wire cutting of diamond wires: in this embodiment, the model of the cutting machine is QPJ1660B/C (great company city), the diameter of the diamond wire is 250 micrometers, the groove pitch of the diamond wire is adjusted to 0.65 mm according to the product specification and the processing requirement, the glass ingot is cut into a mobile terminal glass back cover substrate with the thickness of 0.40 mm, the cutting speed is 2000 m/min, and the processing time is not more than 5 hours.
The final mobile terminal glass back cover substrate obtained has an average thickness of 0.399 mm.
In the above embodiments, the proportioning data and the process parameters are obtained by production tests. The embodiments can show that the invention has simple production process, convenient operation, high dimensional precision, high production efficiency, high qualification rate, stable quality and low cost, can be used for large-scale industrial production, and is particularly suitable for producing the 5G mobile terminal glass back cover substrate with high strength, high toughness and lighter weight.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It will be understood that the invention is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.

Claims (2)

1. A production method of a mobile terminal glass back cover substrate is characterized by comprising the following steps:
(1) preparing raw materials: weighing the following raw materials in percentage by weight, SiO2 45-60%、Na2O 0-5%、CaO 3.1-5%、Al2O315-25% of MgO, 2-5% of MgO; and 5-45% of additive;
the additive comprises TiO2、ZrO2、K2O、B2O3、BaO、ZnO、Y2O3、Ce2O3And Li2O, wherein the components account for the following weight percentage: b is2O3 0-15%、BaO 0-2%、ZnO 0-10%、Y2O3 0-5%、Ce2O3 0-5%、Li2O 0-5%、TiO2 0-0.8%、ZrO2 0-3%、K2O0-2.5%, and ionic coloring agent including Mn2O3、CoO、Co3O4、Cr2O3One or more of the ionic coloring agent, wherein the ionic coloring agent accounts for 2 percent of the total weight; the raw materials are heavyThe sum of the quantity percentages is 100 percent;
(2) processing raw materials: purifying, crushing and screening the obtained raw materials to obtain raw material particles with the particle size of 0.10 micrometer to 0.80 millimeter;
(3) preparing a batch: ball-milling the obtained raw material particles by a ball mill and mixing into a batch of uniformly mixed powder, wherein the particle size of the batch after ball-milling and screening is between 0.2 micron and 0.1 millimeter;
(4) preparing a glass ingot: preparing the batch into a microcrystalline glass ingot by a secondary forming and sintering method; the secondary forming and sintering method comprises the following specific steps: water quenching, crushing and ball milling: putting the batch into a glass melting furnace, electrifying, heating to 400-1200 ℃ at a heating rate of 7-15 ℃/min, preserving heat for 1.5 hours, then continuously heating to 1000-2000 ℃ at a heating rate of 2-7 ℃/min, preserving heat for 2.5 hours, and forming high-temperature glass liquid under the action of high temperature; pouring the glass liquid into a container filled with clear water to form water-quenched glass particles, draining, drying, crushing, and ball-milling until the average particle size is less than 0.20 mm to prepare glass fine powder; pressing a glass ingot blank under high pressure: placing the glass fine powder into a mold, adding a toughening material into the glass fine powder, fully and uniformly mixing, then placing into the mold for pressing, wherein the weight percentage of the toughening material is 5-25%, the toughening material comprises one or more of zirconia powder, zirconia fiber or whisker and silicon carbide fiber or whisker, pressing by a 70MPa oil press, maintaining the pressure for 15 minutes, and removing the mold to obtain a glass ingot blank; and (3) firing a glass ingot: placing the glass ingot blank into a high-temperature furnace, continuously heating to 600-1200 ℃ at the heating rate of 7-15 ℃/min, and preserving heat for 0.5-1 hour; then, continuously heating to 1000-1400 ℃ at the heating rate of 2-7 ℃/min, preserving heat for 2.5 hours, and sintering to form porcelain; then cooling to the crystallization temperature of 500-1000 ℃ at the cooling rate of 2-7 ℃/min for thorough crystallization, and preserving the heat for 3 hours; naturally cooling to room temperature to obtain a glass ingot;
(5) multi-wire cutting of diamond wires: the glass ingot is cut into a glass substrate with the thickness of 0.08-2.0 mm by a cutting machine, the cutting linear speed during cutting is 600-3000 m/min, and the cutting processing time is 10-900 min.
2. The method for producing a glass back cover substrate of a mobile terminal according to claim 1, wherein the length of the inner cavity of the mold is 10-2000 mm, the width of the cross section of the inner cavity is 10-300 mm, and the height of the cross section of the inner cavity is 50-500 mm; the material of the mould is alumina, graphite, silicon carbide or heat-resisting alloy steel.
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