CN113816611A - Microcrystalline glass for 5G intelligent communication equipment backboard and preparation method thereof - Google Patents
Microcrystalline glass for 5G intelligent communication equipment backboard and preparation method thereof Download PDFInfo
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- CN113816611A CN113816611A CN202111275257.4A CN202111275257A CN113816611A CN 113816611 A CN113816611 A CN 113816611A CN 202111275257 A CN202111275257 A CN 202111275257A CN 113816611 A CN113816611 A CN 113816611A
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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
- 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
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- 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
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- 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
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Abstract
The invention relates to microcrystalline glass for a 5G intelligent communication equipment backboard and a preparation method thereof. The microcrystalline glass comprises the following raw materials in percentage by weight: SiO 22 35‑40％；ZnO 20‑25％；Al2O3 15‑20％；MgO 5‑10％；CaO 5‑10％；SrO 0.5‑3％；BaO 0.5‑3％；B2O3 0.5‑3％；ZrO2 0‑5％；TiO2 5‑10％；Sb2O30 to 1 percent. The microcrystalline glass has high hardness (Vickers hardness is more than 8GPa), high strength (bending strength is more than 300MPa), good heat dissipation performance (thermal conductivity is more than 3W/(m.K)), andthe dielectric property is excellent (the dielectric constant is less than 8, 3GHz) and the like, the preparation method is suitable for being applied to the 5G intelligent communication equipment backboard, and meanwhile, the preparation method is low in preparation cost, simple in process and suitable for actual mass production.
Description
Technical Field
The invention relates to microcrystalline glass for a 5G intelligent communication equipment back plate and a preparation method thereof, belonging to the technical field of glass ceramics.
Background
At present, the communication equipment back plate (such as a mobile phone back plate) made of inorganic nonmetal materials on the market mainly comprises high alumina glass and zirconia ceramics.
High alumina glass is excellent in mechanical strength, electrical insulation and chemical stability, but has problems in that the surface hardness is low (mohs hardness of 6), and the surface is easily scratched; secondly, the heat dissipation performance is poor (the heat conductivity coefficient is about 1W/(m.K)), which is not beneficial to the heat dissipation of the communication equipment; in addition, the SiO in the high-alumina glass component2And Al2O3The content is high, the glass melting temperature is high, bubbles and stripes in the glass are not easy to remove, and the preparation difficulty is high.
The zirconia ceramic has high surface hardness, bending strength and fracture toughness, can meet the mechanical property requirement of a communication equipment rear cover, but has a plurality of problems. For example, the dielectric constant of the material is high (about 30), which has a certain effect on electromagnetic wave signals; secondly, the zirconia ceramics have poor heat dissipation performance (the thermal conductivity is about 2W/(m.K)), which is not beneficial to the heat dissipation of communication equipment; besides, the zirconia ceramics need to be processed by nano-scale powder preparation, slurry preparation, granulation, molding, sintering, post-processing and other processes, the preparation process is complex, the yield of products is low (20% -30%), the price is high, and the popularization and the application are not facilitated.
CN104478219A discloses a nano spinel glass ceramics, which comprises the following components by weight percent: SiO 2256-62％；Al2O3 19-23％；MgO 2-6.5％；ZnO 6-15％，ZrO2 2-7％；TiO22 to 6 percent. The nano spinel microcrystalline glass has the bending strength of 110MPa, the Vickers hardness of 5GPa, the dielectric constant of 5 and the corresponding grain size of 30 nm.
CN108516688A discloses a spinel glass-ceramic prepared by using aluminum ash as main raw material. The microcrystalline glass has a main crystal phase of spinel and a secondary crystal phase of amphibole; the bending strength is 70-90 MPa, the compressive strength is 400-500 MPa, and the Mohs hardness is 7-8.
CN109809696A discloses a magnesium aluminate spinel microcrystalline glass, which comprises the following components in percentage by weight: SiO 2225-60％；Al2O3 20-45％；MgO 8-18％；ZrO2 0-5％；TiO2 3-10％；P2O5 0-3％；Li2O 0-2％；Na2O 0-2％；K2O 0-2％；Sb2O30.5 to 3 percent. The microcrystalline glass has a main crystal phase of magnesium aluminate spinel and a secondary crystal phase of zirconium titanate; the bending strength is 140-200 MPa, and the Vickers hardness is 910-1000 Hv.
CN111615500A discloses a high hardness and modulus transparent zinc spinel-spinel glass ceramic. The weight percentage composition of the material comprises: SiO 22 55.0-70.0％；Al2O315.0 to 20.0 percent; 0-10.0% of MgO; 0 to 12.5 percent of ZnO, the microcrystalline glass contains a plurality of alkali metal oxides, can perform ion exchange, and must contain one of MgO or ZnO. The microcrystalline glass contains spinel crystals, and the Mohs hardness of the spinel crystals is more than 7.
In summary, the spinel microcrystalline glass disclosed at present is mainly concerned with improving the mechanical properties, especially the hardness. However, when the material is applied to the 5G intelligent communication equipment backboard, the material needs to have excellent scratch resistance, and the bending strength, the heat dissipation performance, the dielectric performance and the like of the material need to be considered.
Disclosure of Invention
The invention provides microcrystalline glass for a 5G intelligent communication equipment backboard and a preparation method thereof, aiming at the problems of small hardness, low strength, poor heat dissipation, high dielectric constant and the like of the traditional glass backboard. The preparation method not only can obviously improve the problems, but also has low preparation cost and simple process and is suitable for actual mass production.
The invention adopts the following technical scheme for achieving the purpose:
the microcrystalline glass for the 5G intelligent communication equipment back plate comprises the following raw materials: the weight percentage composition is as follows: SiO 22 35-40％；ZnO 20-25％；Al2O3 15-20％；MgO 5-10％；CaO 5-10％；SrO 0.5-3％；BaO 0.5-3％；B2O3 0.5-3％；ZrO2 0-5％；TiO2 5-10％；Sb2O3 0-1％。
Further, the preparation method of the microcrystalline glass for the 5G intelligent communication equipment backboard comprises the following steps:
(a) ingredients
Weighing the raw materials according to the weight percentage, and uniformly mixing to obtain the batch.
(b) Melting
And heating the batch to 1500-.
(c) Shaping and annealing
And pouring the molten glass into a pre-preheated copper mold, forming, transferring to an annealing furnace, annealing at the temperature of 500-600 ℃ for 1-2 hours, and cooling to room temperature along with the furnace to obtain the base glass.
(d) Thermal treatment
And (2) putting the basic glass into a crystallization furnace for heat treatment, nucleating at the temperature of 700-750 ℃ for 1-2 hours, crystallizing at the temperature of 950-1000 ℃ for 1-2 hours, and annealing to obtain the glass ceramics, wherein the crystalline phase of the glass ceramics has a complex phase structure of gahnite, enstatite and diopside. Preferably, the nucleation temperature is 720 ℃, and the nucleation time is 2 hours; the crystallization temperature is 950-.
Furthermore, the optimal content of each glass component of the microcrystalline glass is as follows:
SiO2is a glass network former oxide. When SiO is present2When the content is too high, the melting temperature of the glass is too high, a quartz crystal phase is easy to separate out, and the mechanical property of the microcrystalline glass is poor; when SiO is present2When the content is too low, the glass forming ability is poor and crystallization is easy. SiO in the glass component2The optimum content is 35-40 wt%.
Al2O3Is a glass network intermediate oxide. When Al is present2O3The content is too high, and the number of columnar pyroxene crystals is smallThe length-diameter ratio is small, and the mechanical property of the microcrystalline glass is poor; when Al is present2O3The content is too low, the microcrystalline glass is not easy to be crystallized integrally, and the mechanical property and the heat-conducting property of the microcrystalline glass are influenced. Al in glass component2O3The optimal content is 15-20 wt%.
ZnO is an important constituent of the zinc spinel crystal phase in the glass-ceramic. The proper increase of the ZnO content is beneficial to the overall crystallization and the improvement of the heat conductivity coefficient of the microcrystalline glass; when the content of ZnO is too high, the crystallization tendency of the microcrystalline glass is increased, the crystallization is easily caused in the glass forming process, and the optimal content of ZnO in the glass component is 20-25 wt%.
MgO and CaO are important components of enstatite and diopside crystal phases in the glass ceramics. When the content of the pyroxene phase and the pyroxene phase is too low, the microcrystalline glass has low fracture toughness; on the contrary, when the content of the two is too high, the zinc spinel phase is not favorably separated out, and the heat conductivity coefficient of the microcrystalline glass is low. The optimal content of MgO and CaO in the glass component is 5-10 wt%.
BaO and SrO are exonic oxides. The proper amount of the glass ceramics can increase the density of the glass ceramics, improve the heat conductivity coefficient of the glass ceramics and accelerate the melting and the clarification of the glass. The optimum content of BaO and SrO in the glass component is 0.5-3 wt%.
B2O3The microcrystalline glass mainly has the functions of adjusting the expansion coefficient of a glass phase and preventing the microcrystalline glass from cracking due to the mismatch of the expansion coefficients of the crystal phase and the glass phase; meanwhile, the glass melting agent also plays a role in fluxing and accelerates the melting and the clarification of the glass. Notably, B is2O3The content should not be too high, otherwise the mechanical properties of the glass-ceramic will be affected. In the glass component B2O3The optimum content is 0.5-3 wt%.
TiO2And ZrO2Is a crystal nucleus agent. The crystallization performance of the microcrystalline glass can be obviously improved by properly increasing the content of the nucleating agent, and the microcrystalline glass has excellent mechanical property and heat-conducting property; when the content of the crystal nucleating agent is too high, other unnecessary crystal phases are easy to precipitate in the microcrystalline glass, and the mechanical property and the heat conducting property of the microcrystalline glass are influenced; in addition TiO2In excess ofHigh, the dielectric constant of the microcrystalline glass is large. TiO 22And ZrO2The optimum content of the crystal nucleus agent is 5-10 wt% and 0-5 wt%, respectively.
Sb2O3Is a clarifying agent, and the optimal content is 0-1 wt%.
Furthermore, in each glass component of the microcrystalline glass, SiO is controlled2/Al2O3The mass ratio of (1): 1.8-2.2.
Further, SiO control2(CaO + MgO) mass ratio of 1: 2.5-3.4.
Furthermore, the mass sum of ZnO and MgO is controlled to be 22-27 percent of the total mass of all the components of the glass.
More preferably, SiO is controlled in each glass component of the microcrystalline glass2/Al2O3The mass ratio of (1): 1.9-2.1; control of SiO2(CaO + MgO) mass ratio of 1: 2.5 to 3.2, and the mass sum of ZnO and MgO is controlled to be 23 to 27 percent of the total mass of all components of the glass.
More preferably, the microcrystalline glass for the 5G intelligent communication equipment backboard is prepared from the following raw materials in percentage by weight: SiO 22 37％；ZnO 17％；Al2O3 20％；MgO 6％；CaO 8％；SrO 1.2％；BaO 1％；B2O3 1％；ZrO20.8％；TiO2 7.5％；Sb2O3 0.5％。
Compared with the prior art, the invention has the following beneficial effects:
(1) the spinel microcrystalline glass disclosed at present mainly focuses on improving the hardness of the glass, and the spinel microcrystalline glass provided by the invention has the advantages of high hardness, high strength, high thermal conductivity, low dielectric constant and excellent comprehensive performance.
(2) The mechanical properties of the presently disclosed spinel glass-ceramics are provided primarily by the spinel crystal phase having a high modulus of elasticity. The microcrystalline glass provided by the invention not only contains a spinel crystal phase with high elastic modulus, but also forms an interlocking microstructure with columnar pyroxene crystals in staggered distribution, and the structure can effectively change the expansion path of the microcrack when the microcrack expands, thereby improving the mechanical strength of the microcrystalline glass.
(3) The gaps among the columnar pyroxene crystals of the microcrystalline glass are filled by spinel crystals with fine grain sizes, the crystals are densely stacked, and the density and the heat conductivity of the microcrystalline glass can be further improved.
(4) The spinel glass ceramics disclosed in the prior art usually incorporate alkali metal oxides to lower the melting temperature of the glass, and the glass ceramics of the present invention use mixed alkaline earth metal oxides instead of alkali metal oxides. The melting temperature of the glass can be reduced, and the reduction of the density of a glass network structure (reduction of mechanical properties) caused by the introduction of alkali metal ions and the influence of the precipitation of the alkali metal ions in the glass material on electronic equipment are avoided.
Through composition design and process optimization, controllable crystallization of various crystals is realized, and the microcrystalline glass is cut and polished to prepare high-hardness, high-strength, high-heat-conductivity and low-dielectric microcrystalline glass with the thickness of less than 0.7mm, can be applied to communication equipment backboards such as 5G smart phones and the like, and meets the performance requirements of wireless charging, chip heat dissipation, scratch resistance, drop resistance and the like.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
A preparation method of microcrystalline glass for a 5G intelligent communication equipment backboard,
the method comprises the following steps:
(a) ingredients
Weighing the following raw materials in percentage by weight: SiO 22 35-40％；ZnO 20-25％；Al2O3 15-20％；MgO 5-10％；CaO 5-10％；SrO 0.5-3％；BaO 0.5-3％；B2O3 0.5-3％；ZrO2 0-5％；TiO2 5-10％；Sb2O30 to 1 percent. The raw materials are uniformly mixed to be used as a batch.
(b) Melting
And heating the batch to 1500-.
(c) Shaping and annealing
And pouring the molten glass into a pre-preheated copper mold, forming, transferring to an annealing furnace, annealing at the temperature of 500-600 ℃ for 1-2 hours, and cooling to room temperature along with the furnace to obtain the base glass.
(d) Thermal treatment
And (2) putting the basic glass into a crystallization furnace for heat treatment, nucleating at the temperature of 700-750 ℃ for 1-2 hours, crystallizing at the temperature of 950-1000 ℃ for 1-2 hours, and annealing to obtain the glass ceramics, wherein the crystalline phase of the glass ceramics has a complex phase structure of gahnite, enstatite and diopside.
Examples 1 to 5
In each example, the raw materials were weighed according to the compositions corresponding to those in table 1 and mixed uniformly; heating to a melting system corresponding to the melting system in the table 2, and melting, clarifying and homogenizing to obtain molten glass; pouring the molten glass into a pre-preheated copper mold, transferring the molded glass to an annealing furnace, annealing at the temperature of 500 ℃ for 1-2 hours, and cooling to room temperature along with the furnace to obtain base glass; the obtained basic glass is put into a crystallization furnace for heat treatment according to the nucleation and crystallization system corresponding to the table 2, and the microcrystalline glass of the invention is obtained after annealing.
Comparative examples 1 to 2
Weighing the raw materials according to the corresponding compositions in the table 1 in each proportion, and uniformly mixing; heating to a melting system corresponding to the melting system in the table 2, and melting, clarifying and homogenizing to obtain molten glass; pouring the molten glass into a pre-preheated copper mold, transferring the molded glass to an annealing furnace, annealing at the temperature of 500 ℃ for 1-2 hours, and cooling to room temperature along with the furnace to obtain base glass; the obtained base glass is put into a crystallization furnace to be subjected to heat treatment according to the nucleation and crystallization system corresponding to the table 2, and the microcrystalline glass of the comparative example is obtained after annealing.
TABLE 1 compositions and control requirements (unit: wt%) of examples and comparative examples
TABLE 2 preparation Process and Performance parameters of the examples and comparative examples
TABLE 3 Properties of crystallized glasses obtained in examples and comparative examples
As is clear from the data of the examples in Table 2, the glass-ceramics of the present invention 1 to 5 are characterized by high hardness (Vickers hardness > 8GPa), high strength (bending strength > 300MPa), good heat dissipation properties (thermal conductivity > 3W/(m.K)), and excellent dielectric properties (dielectric constant < 8, 3 GHz).
Comparative example 1 SiO in comparison with example 22Addition of excess amounts, with simultaneous induction of "SiO2/Al2O3And SiO2The mass ratio of CaO + MgO exceeds the control range, so that the prepared microcrystalline glass has low bending strength and thermal conductivity and high dielectric constant.
Compared with example 2, the nucleation and crystallization temperatures of comparative example 2 are out of the control range, resulting in poor bending strength, low thermal conductivity and low vickers hardness of the obtained glass-ceramic.
The above specific examples of the crystallized glass of the present invention are given by way of illustration only for illustrating the performance of the crystallized glass of the present invention, and are not intended to limit the embodiments of the present invention. Variations or modifications in other variations will be apparent to persons skilled in the art based on the foregoing description. All embodiments are not necessarily or exclusively enumerated herein. And such obvious variations or modifications are intended to be included within the scope of the present invention as expressed in the following claims.
Claims (10)
1. The microcrystalline glass for the 5G intelligent communication equipment backboard is characterized by comprising the following raw materials in percentage by weight: SiO 22 35-40％；ZnO 17-22％；Al2O3 15-20％；MgO 5-10％；CaO 5-10％；SrO 0.5-3％；BaO 0.5-3％；B2O3 0.5-3％；ZrO2 0-5％；TiO2 5-10％；Sb2O3 0-1％。
2. The glass-ceramic according to claim 1, wherein SiO is contained in the raw material composition2And Al2O3The mass ratio of (1): 1.8-2.2; SiO in the raw material composition2The mass of the CaO-MgO is 2.5 to 3.2 times of the total mass of the CaO and the MgO.
3. The glass-ceramic according to claim 2, wherein the sum of the mass of ZnO and MgO in the raw material composition is 22 to 27% of the total mass of the glass-ceramic raw materials.
4. The glass-ceramic according to claim 3,
SiO in the raw material composition2And Al2O3The mass ratio of (1): 1.9-2.1;
SiO in the raw material composition2The mass of the CaO-MgO is 2.5 to 3.2 times of the total mass of the CaO and the MgO;
the sum of the mass of ZnO and MgO in the raw material composition is 23-27% of the total mass of the microcrystalline glass raw material.
5. The microcrystalline glass according to claim 4, wherein the microcrystalline glass consists of the following raw materials in percentage by weight: SiO 22 37％；ZnO 17％；Al2O3 20％；MgO 6％；CaO 8％；SrO 1.2％；BaO 1％；B2O3 1％；ZrO2 0.8％；TiO2 7.5％；Sb2O3 0.5％。
6. The glass-ceramic according to claim 1, wherein the crystalline phase of the glass-ceramic has a complex phase structure of gahnite, enstatite and diopside.
7. The preparation method of the microcrystalline glass for the 5G intelligent communication equipment backboard, which is disclosed by any one of claims 1 to 6, comprises the following steps: firstly, mixing and melting raw materials to prepare molten glass; preparing base glass from the molten glass; finally, putting the basic glass into a crystallization furnace for nucleation and crystallization system for heat treatment, wherein the nucleation temperature is 700-750 ℃, and the nucleation time is 1-2 hours; the crystallization temperature is 950 ℃ and 1000 ℃, and the crystallization time is 1-2 hours; and annealing to obtain the target glass ceramics.
8. The method of claim 7, wherein the nucleation temperature is 720 ℃ and the nucleation time is 2 hours; the crystallization temperature is 950-.
9. The method as claimed in claim 8, wherein the melting temperature is 1500-;
10. the method according to claim 9, wherein the molten glass is used for preparing the base glass by the following specific operation steps: and pouring the molten glass into a pre-preheated copper mold, forming, transferring to an annealing furnace, annealing at the temperature of 500-600 ℃ for 1-2 hours, and cooling to room temperature along with the furnace to obtain the base glass.
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| CN114149179A (en) * | 2021-12-28 | 2022-03-08 | 海南大学 | Diopside microcrystalline glass and preparation method thereof |
| WO2023122933A1 (en) * | 2021-12-28 | 2023-07-06 | 海南大学 | Diopside microcrystalline glass and preparation method therefor |
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| CN113816611B (en) | 2022-08-05 |
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