WO2022228583A1 - Matériau vitrocéramique, procédé de préparation associé et application correspondante dans des dispositifs à semi-conducteurs - Google Patents

Matériau vitrocéramique, procédé de préparation associé et application correspondante dans des dispositifs à semi-conducteurs Download PDF

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WO2022228583A1
WO2022228583A1 PCT/CN2022/094351 CN2022094351W WO2022228583A1 WO 2022228583 A1 WO2022228583 A1 WO 2022228583A1 CN 2022094351 W CN2022094351 W CN 2022094351W WO 2022228583 A1 WO2022228583 A1 WO 2022228583A1
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glass
weight
ceramic material
ceramic
following components
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PCT/CN2022/094351
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Chinese (zh)
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赵天佑
赵国祥
刘浩然
赵成玉
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深圳晶酝科技有限公司
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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
    • C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • 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
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/004—Refining agents
    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04M—TELEPHONIC COMMUNICATION
    • H04M1/00—Substation equipment, e.g. for use by subscribers
    • H04M1/02—Constructional features of telephone sets
    • H04M1/0202—Portable telephone sets, e.g. cordless phones, mobile phones or bar type handsets

Definitions

  • the invention belongs to the technical field of semiconductor devices, and in particular relates to a glass-ceramic material, a preparation method thereof, and application in semiconductor devices.
  • 5G communication uses wireless spectrum above 3GHz, and the antenna structure will be more complex than 4G, and the existing antenna layout structure cannot meet the needs of 5G. Therefore, in the 5G era, smartphones will abandon the existing metal back cover for signal shielding, and ceramic back cover and glass back cover will become an alternative to 5G communication products.
  • the glass back cover made of glass-ceramic has excellent wear resistance and is easy to clean and toning, which has become a hot research topic at present.
  • glass-ceramics There are many types of glass-ceramics, and glass products with different uses can be produced by different component ratios and different processes. Most of the existing glass-ceramic products are single crystal phase, which are mainly used as architectural decorative materials, biological materials, craft products or small heating products, etc. At present, the production of high-hardness, high-strength and high-transparency glass-ceramic has not been found in the domestic market, and it is even more blank for semiconductor devices such as mobile phone panels and backplanes. Internationally, it is only produced by Corning Corporation of the United States, exclusively for Apple.
  • Patent CN110217985A discloses a kind of glass-ceramic, although it is a polycrystalline phase system, it has a lower expansion coefficient, higher hardness and strength, but its transparency still needs to be improved, and it has no impact performance and Mohs hardness. Transparency, impact performance and Mohs hardness are precisely the properties that are most concerned about in the preparation of mobile phone panels or back sheets.
  • the purpose of the present invention is to overcome the lack of high hardness, high strength and high transparency glass-ceramic in the prior art, and to provide a glass-ceramic material.
  • the glass-ceramic material provided by the present invention solves the performance defect of the single-crystal phase glass-ceramic by constructing a polycrystalline phase system, thereby ensuring the high hardness of the glass-ceramic and improving the performance of the glass-ceramic.
  • the transparency and impact strength of glass-ceramic is suitable for semiconductor devices, especially the use requirements of high-end mobile phone (including 5G) panels and backplane materials.
  • Another object of the present invention is to provide a method for preparing the above-mentioned glass-ceramic material.
  • Another object of the present invention is to provide the application of the above-mentioned glass-ceramic material in semiconductor devices.
  • a glass-ceramic material comprising base glass, nucleating agent, clarifying agent and additives, based on the total weight of the glass-ceramic material:
  • the base glass includes the following components by weight: Li 2 O 0.5-3.2%, Al 2 O 3 25.0-35.0%, SiO 2 45.0-60.0%, MgO 2.0-14.0%;
  • the crystal nucleating agent includes the following components by weight: SnO 2 0.1-1.0%, ZrO 2 1.0-5.0%;
  • the additive includes the following components by weight: La 2 O 3 0.1-1.0%, Y 2 O 3 0.1-1.0%.
  • the glass-ceramic material includes a glass matrix and a polycrystalline phase system dispersed in the glass matrix; the polycrystalline phase system is mainly composed of magnesia-aluminum spinel, supplemented by tetragonal zirconia, eucryptite and quartz solid solution; The weight fraction of spinel is not less than 15% to 20%; the total mass fraction of tetragonal zirconia, eucryptite and quartz solid solution is less than 3%.
  • the inventors of the present application have improved the formulation of glass-ceramic from the following aspects to improve transparency, impact resistance and Mohs hardness. specifically:
  • the glass-ceramic in patent CN110217985A is Li 2 O-Al 2 O 3 -SiO 2 series glass-ceramic, and its crystal phase is mainly spodumene, with part of eucryptite and quartz solid solution; and the glass-ceramic of the present application is constructed of A new crystal phase system is developed.
  • the glass-ceramic material of the present application is mainly composed of magnesia-aluminum spinel, supplemented by tetragonal zirconia, eucryptite and quartz solid solution (the weight fraction of magnesia-aluminum spinel is greater than The weight fraction of other crystalline phases is combined) to obtain a polycrystalline phase system, which is dispersed in the glass matrix, which can effectively improve the hardness, transparency and impact strength of glass-ceramics; at the same time, it increases its material properties and reduces the molding temperature, which is more suitable Various molding requirements for mobile phone covers.
  • the present application builds a specific polycrystalline phase system by optimizing the formulations of the base glass, crystal nucleating agent and additives, so as to improve the hardness, transparency and impact strength of the glass-ceramic, and at the same time improve the forming performance.
  • the glass-ceramic of the present application is mainly composed of magnesia-aluminum spinel, with tetragonal zirconia, eucryptite and The quartz solid solution is supplemented to obtain a polycrystalline phase system.
  • the weight ratio of ZrO 2 is adjusted in this application, and the use of ZrO 2 to toughen glass-ceramics is an important way to improve its toughness.
  • the toughening mechanism of ZrO 2 in glass-ceramics is mainly stress-induced phase transformation Toughening, crack partial toughening and micro-crack toughening.
  • the toughening effect is affected by the volume content of ZrO 2 in the glass-ceramic, the crystal form, crystal size and crystal morphology of ZrO 2.
  • adding SnO 2 can effectively control the crystal. Excessive growth ensures the size and uniformity of the crystal grains, thereby ensuring the transparency of the glass.
  • the introduction of Y 2 O 3 into the glass-ceramic can solve the problems of melting and crystallization, and effectively improve the flexural strength of the glass.
  • the introduction of La 2 O 3 makes the crystal phase develop into complete columnar and plate-like crystals, which can increase the strength and toughness of the glass.
  • the glass-ceramic obtained by the invention has high transparency, hardness and strength, and is suitable for the use requirements of semiconductor devices, especially high-end mobile phone (including 5G) panels and backplane materials.
  • semiconductor devices especially high-end mobile phone (including 5G) panels and backplane materials.
  • the specific performance indicators are as follows:
  • the mass fraction of magnesia-aluminum spinel in the glass-ceramic material is 15-20%; the total mass fraction of tetragonal zirconia, eucryptite and quartz solid solution is 3-5%.
  • the mass fraction of tetragonal zirconia may be 1-1.5%; the mass fraction of eucryptite may be 0.5-1.5%; the mass fraction of quartz solid solution may be 0.5-1.5%.
  • magnesia-aluminum spinel, tetragonal zirconia, eucryptite and quartz solid solutions all develop into complete columnar or tabular crystals; the magnesia-aluminum spinel, tetragonal zirconia, eucryptite and quartz solid solutions are uniform and Disperse uniformly in the glass matrix.
  • the glass-ceramic material Preferably, based on the total weight of the glass-ceramic material:
  • the base glass includes the following components by weight: Li 2 O 0.5-3.2%, Al 2 O 3 25.0-35.0%, SiO 2 45.0-60.0%, MgO 2.0-14.0%, ZnO 1.0-12.0%, CaO 0.2-4.5 %, SrO 0.3 ⁇ 3.0%, BaO 0.2 ⁇ 3.0%, R 2 O 1.1 ⁇ 10.2%;
  • the crystal nucleating agent includes the following components by weight: SnO 2 0.1-1.0%, ZrO 2 1.0-5.0%, TiO 2 0.2-2.0%, P 2 O 5 0-2.0%;
  • the clarifying agent includes the following components by weight: Sb 2 O 3 0.1-0.5%, NaCl 0.2-0.6%;
  • the additive includes the following components by weight: La 2 O 3 0.1-1%, Y 2 O 3 0.1-1.0%;
  • the sum of the weight fractions of each component is 100%.
  • the base glass includes the following components by weight: Li 2 O 2.0-3.1%, Al 2 O 3 25.5-32.0%, SiO 2 45.5-57.0%, MgO 3.0 ⁇ 12.0%, ZnO 3.0 ⁇ 11.5%, CaO 0.5 ⁇ 4.0%, SrO 0.5 ⁇ 2.0%, BaO 0.5 ⁇ 2.0%, R 2 O 3.0 ⁇ 8.0%.
  • the crystal nucleating agent includes the following components by weight: SnO 2 0.2-0.7%, ZrO 2 2.0-4.7%; TiO 2 0.25-1.9%, P 2 O 5 0.1 ⁇ 1.9%.
  • the clarifying agent includes the following components by weight: Sb 2 O 3 0.2-0.48%, NaCl 0.3-0.58%.
  • the additive comprises the following components by weight: La 2 O 3 0.15-0.9%, Y 2 O 3 0.12-0.95%.
  • the R 2 O includes K 2 O, Na 2 O and Li 2 O.
  • the R 2 O includes the following weight fractions of components K 2 O 0.1-2.5% and Na 2 O 1.0-7.7%.
  • the preparation method of the above glass-ceramic material includes the following steps: mixing base glass, crystal nucleating agent, clarifying agent and additives, melting, cooling, molding, crystallization and annealing to obtain the glass-ceramic;
  • the crystallization treatment adopts multi-stage heat preservation treatment, and the temperature of each stage gradually rises.
  • the process of crystallization treatment has an important influence on the performance of glass-ceramics.
  • various crystal structures are formed by using multi-temperature sections for crystallization treatment, and the size of the crystal is controlled by different temperatures and times, that is, the micro-crystal structure is ensured.
  • the strength and hardness of crystal glass ensure its transparency.
  • the glass-ceramic of the present invention is mainly composed of a glass matrix and nanoscale crystal particles dispersed therein, and the crystal particles are composed of magnesia-aluminum spinel (mainly), eucryptite, tetragonal zirconia crystal particles and quartz crystal particles.
  • the melting temperature is 1600°C to 1660°C, and the melting time is 6 to 12 hours.
  • the cooling temperature is 1440°C to 1500°C, and the cooling time is 2 to 4 hours.
  • the following methods are used for forming: calender forming, overflow forming or float forming.
  • the crystallization treatment is a 2-stage heat preservation treatment: treatment at 600-650° C. for 1-3 hours, and then at 730-790° C. for 1-3 hours; or the crystallization treatment is a 3-stage heat preservation treatment: at 730-790° C. Treat at 600 ⁇ 650°C for 1 ⁇ 3h, then at 700 ⁇ 750°C for 1 ⁇ 3h, then at 780 ⁇ 830°C for 1 ⁇ 3h.
  • the temperature of the annealing is 550 ⁇ 580° C., and the time is 2 ⁇ 5 h.
  • the present invention has the following beneficial effects:
  • the glass-ceramic material provided by the invention has multiple crystal phases through the component polycrystalline phase system, which solves the defect of the performance of the single-crystal phase glass-ceramic, not only ensures the high hardness of the glass-ceramic, but also improves the performance of the glass-ceramic.
  • the transparency and impact strength of glass-ceramic is suitable for the use requirements of high-end mobile phone (including 5G) panels and backplane materials.
  • Fig. 1 is the X-ray diffraction pattern of a series of glass-ceramics provided in Example 1;
  • Fig. 2 is the scanning electron microscope image of a series of glass-ceramics provided in Example 1;
  • Fig. 3 is the scanning electron microscope picture of the glass-ceramic that comparative example 2 provides;
  • Mohs hardness 7.0 ⁇ 8.0 (scratch method);
  • This embodiment provides a series of glass-ceramics, which are composed of the following components (weight fraction, the same below): 2.0wt% Li 2 O, 25.5wt% A 2 lO 3 , 51.5%wt SiO 2 , 0.5wt% CaO, 0.5wt%SrO, 3.0wt%ZnO, 8.1wt %MgO, 0.5wt%BaO, 0.4wt%K2O, 1.0wt%Na2O, 5.0wt %ZrO2, 0.1wt% Y2O3 , 0.4wt % % Sb 2 O 3 , 0.4 wt % NaCl, 0.5 wt % SnO 2 , 0.3 % TiO 2 , 0.2 % P 2 O 5 , 0.1 wt % La 2 O 3 .
  • the preparation process is as follows:
  • the crystallization treatment is divided into three stages.
  • the temperature of the first stage is 640°C and the time is 2h, and the temperature of the second stage is 710°C and the time is 1h.
  • the third stage is 780 °C, the time is 2h; annealing treatment is carried out after the crystallization treatment, the temperature of the annealing treatment is 560 °C, and the time is 3h.
  • the treatment temperatures in the third stage of step (2) were adjusted to 640°C, 740°C, and 980°C, respectively, and the remaining conditions were consistent with the above operations for comparative analysis.
  • the series of glass-ceramics were characterized by means of X-ray diffraction (XRD) analysis technique supplemented by scanning electron microscopy (SEM). The results are shown in Figures 1 and 2. It can be seen from Figure 2 that when the glass-ceramic was treated at 640 °C, only a small amount of crystals were scattered sporadically. At 740 °C, the crystal particles had grown up in the glass phase, but the glass structure was still relatively loose at this time, and the strength and hardness Relatively poor. When treated at 780°C, the crystal and glass phases have been perfectly combined.
  • XRD X-ray diffraction
  • SEM scanning electron microscopy
  • the glass-ceramic has been completely devitrified due to the growth of crystal particles.
  • the analysis of the crystal phase of the glass-ceramics treated at various temperatures shows that the glass-ceramic is mainly composed of a glass matrix and nano-scale crystal particles dispersed therein.
  • the crystal particles of the glass-ceramics treated at 740°C are mainly magnesia-aluminum spinel, and the content of eucryptite, tetragonal zirconia crystal particles and quartz crystal particles is very small, and there are almost no diffraction peaks; the crystallites obtained by the treatment at 780°C
  • the crystal particles of the glass are mainly magnesia-aluminum spinel, accounting for about 18% by weight, eucryptite (about 1.5% by weight), tetragonal zirconia crystal particles (about 1% by weight) and quartz crystal particles (
  • the content of magnesia-aluminum spinel, tetragonal zirconia crystal particles and quartz crystal particles in the crystal particles of the glass-ceramic obtained by treatment at 980 ° C further increased, and the lithium
  • the content of nepheline crystal particles is greatly reduced, and there are almost no diffraction peaks. This is mainly due to the gradual transformation of eu
  • This embodiment provides a glass-ceramic, which is composed of the following components: 51.7wt% SiO 2 , 25.1wt% Al 2 O 3 , 3.0wt% ZnO, 5.0wt% ZrO 2 , 0.6wt% Y 2 O 3 , 0.3 wt% Sb 2 O 3 , 1.0 wt % BaO, 0.5 wt % SrO, 1 wt % La 2 O 3 , 5.5 wt % Na 2 O, 1.0 wt % K 2 O, 0.5 wt % Li 2 O, 0.5 wt % CaO , 0.5wt% SnO 2 , 0.3wt% TiO 2 , 0.2% P 2 O 5 , 3.0wt% MgO, 0.3wt% NaCl.
  • the preparation process is as follows:
  • Crystallizing ordinary glass to obtain glass-ceramic The crystallization treatment is divided into two stages. The temperature of the first stage is 640°C and the time is 3h, and the temperature of the second stage is 750°C and the time is 2h. , annealing treatment is carried out after crystallization treatment, the temperature of annealing treatment is 578 °C, and the time is 2.5h.
  • the X-ray diffraction pattern of the glass-ceramic is consistent with that of the glass-ceramic obtained by processing at 780°C in Fig. 1. It is mainly composed of a glass matrix and nano-scale crystal particles dispersed therein, and the crystal particles are mainly composed of magnesium aluminum spinel (weight 20%), eucryptite (about 1.2% by weight), tetragonal zirconia crystal particles (about 1.3% by weight) and quartz crystal particles (about 1% by weight).
  • This embodiment provides a glass-ceramic, which is composed of the following components: 45.2wt% SiO 2 , 33.1wt% Al 2 O 3 , 1.0wt% ZnO, 4.0wt% ZrO 2 , 0.5wt% Y 2 O 3 , 0.2 wt% Sb 2 O 3 , 0.6 wt % BaO, 0.5 wt % SrO, 0.8 wt % La 2 O 3 , 3.5 wt % Na 2 O, 1.2 wt % K 2 O, 1.5 wt % Li 2 O, 0.4 wt %
  • the composition is composed of CaO, 0.5wt% SnO 2 , 0.3wt% TiO 2 , 0.4wt% P 2 O 5 , 6.0wt% MgO, 0.3wt% NaCl.
  • the preparation process is as follows:
  • the glass-ceramic is obtained by crystallization of ordinary glass.
  • the crystallization treatment is divided into three stages.
  • the temperature of the first stage is 620°C and the time is 1.5h.
  • the temperature of the second stage is 730°C and the time is 1.5h, annealing treatment is required after the crystallization treatment.
  • the temperature of the annealing treatment is 790°C and the time is 1h.
  • the X-ray diffraction pattern of the glass-ceramic is consistent with that of the glass-ceramic obtained by processing at 780°C in Fig. 1. It is mainly composed of a glass matrix and nano-scale crystal particles dispersed therein.
  • the crystal particles are composed of magnesium aluminum spinel (weight fraction It is mainly composed of eucryptite (about 1.5% by weight), tetragonal zirconia crystal particles (about 1.2% by weight) and quartz crystal particles (about 1% by weight).
  • This embodiment provides a glass-ceramic, which is composed of the following components: 52.2wt% SiO 2 , 30.2wt% Al 2 O 3 , 6.0wt% ZnO, 2.0wt% ZrO 2 , 0.1wt% Y 2 O 3 , 0.3 wt% Sb 2 O 3 , 0.5 wt % BaO, 0.5 wt % SrO, 0.1 wt % La 2 O 3 , 1.0 wt % Na 2 O, 0.7 wt % K 2 O, 1.8 wt % Li 2 O, 0.5 wt %
  • the composition is composed of CaO, 0.2 wt% SnO 2 , 0.3 wt % TiO 2 , 0.4 wt % P 2 O 5 , 3.0 wt % MgO, 0.2 wt % NaCl.
  • the preparation process is as follows:
  • the glass-ceramic is obtained by crystallization of ordinary glass.
  • the crystallization treatment is divided into two stages.
  • the temperature of the first stage is 640°C and the time is 2.5h
  • the temperature of the second stage is 750°C and the time is 2h
  • annealing treatment is required after the crystallization treatment.
  • the temperature of the annealing treatment is 580°C and the time is 4h.
  • the X-ray diffraction pattern of the glass-ceramic is consistent with that of the glass-ceramic obtained by processing at 780°C in Fig. 1. It is mainly composed of a glass matrix and nano-scale crystal particles dispersed therein.
  • the crystal particles are composed of magnesium aluminum spinel (weight fraction It is mainly composed of eucryptite (about 1.5% by weight), tetragonal zirconia crystal particles (about 0.5% by weight) and quartz crystal particles (about 1.2% by weight).
  • This comparative example provides a glass-ceramic, which is prepared with reference to Example 1 of Patent CN110217985A, the formula is the same as Example 1 of CN110217985A, and the size of the slices is the same as each Example.
  • the preparation process is as follows: it is composed of the following weight percentages: Li 2 O: 3.7%; Al 2 O 3 : 22%; SiO 2 : 60.3%; CaO: 1.8%; MgO: 0.7%; ZnO: 2.2%; BaO: 1.0%; K 2 O: 0.5%; Na 2 O: 0.5%; TiO 2 : 1.8%; ZrO 2 : 2.0%; P 2 O 5 : 2.0%; As 2 O 3 : 0.5%; Sb 2 O 3 : 0.5%; NaCl: 0.5%.
  • the process flow includes:
  • This glass does not crystallize above 1330°C, and the cooling process is 1330°C ⁇ 600°C for 60 minutes No devitrification, heat treatment at 630°C, temperature control is shown in Figure 3 of the cooling curve; (6) Precision heat treatment and annealing, after pouring, the glass is cooled from 1330°C ⁇ 750°C within 60 minutes, and the temperature is lowered to 630°C by the following heat treatment system °C At this time, the color of the glass plate is brown and transparent; (7) Slice into the required size (consistent with the test sample) (8) Sample preparation: grinding, polishing and finishing; (9) Packing and storing for later use.
  • the glass-ceramic is mainly composed of a glass matrix and ⁇ -eucryptite crystals and ⁇ -quartz solid solution crystals dispersed therein.
  • This comparative example provides a glass-ceramic, the composition of which is the same as that of Example 2 except that it does not contain Y 2 O 3 and the content of ZrO 2 is 5.1 wt %, and the preparation method is also the same as that of Example 2.
  • the glass-ceramic is mainly composed of a glass matrix and nano-scale crystal particles dispersed in it.
  • the X-ray diffraction pattern is consistent with the glass-ceramic obtained by processing at 780 ° C in Fig. 1.
  • the crystal particles are mainly magnesium aluminum spinel (weight 20%) and eucryptite (about 1.2% by weight), tetragonal zirconia crystal particles (about 1.5% by weight) and quartz crystal particles (about 1.1% by weight).
  • Figure 3 is a scanning electron microscope image. It can be seen from the figure that ZrO 2 is refractory due to the absence of Y 2 O 3 . It can be seen that the size and distribution of zirconia crystals are uneven, and even zirconia streaks appear.
  • This comparative example provides a glass-ceramic, the composition of which is the same as that of Example 2 except that it does not contain La 2 O 3 and the content of SiO 2 is 51.6 wt %, and the preparation method is also the same as that of Example 2.
  • the X-ray diffraction pattern of the glass-ceramic is consistent with that of the glass-ceramic obtained by processing at 780°C in Fig. 1. It is mainly composed of a glass matrix and nano-scale crystal particles dispersed therein.
  • the crystal particles are composed of magnesium aluminum spinel (weight fraction It is mainly composed of eucryptite (about 1.5% by weight), tetragonal zirconia crystal particles (about 1.2% by weight) and quartz crystal particles (about 1.0% by weight).
  • La 2 O 3 has little effect on the composition of the crystal, because La 2 O 3 is conducive to the development of the crystal phase in the glass-ceramic into complete columnar and plate-like crystals, which affects the performance of the glass-ceramic.
  • This comparative example provides a glass-ceramic, the composition of which is the same as that of Example 2 except that it does not contain SnO 2 and the content of SiO 2 is 52.0 wt %, and the preparation method is also the same as that of Example 2.
  • the X-ray diffraction pattern of the glass-ceramic is consistent with that of the glass-ceramic obtained by processing at 780°C in Fig. 1. It is mainly composed of a glass matrix and nano-scale crystal particles dispersed therein.
  • the crystal particles are composed of magnesium aluminum spinel (weight fraction It is mainly composed of eucryptite (about 1.5% by weight), tetragonal zirconia crystal particles (about 0.5% by weight) and quartz crystal particles (about 1.2% by weight).
  • SnO 2 can effectively control the crystal growth too fast, ensure the size and uniformity of crystal particles, and thus ensure the transparency and strength of the glass.
  • Figure 4 is a scanning electron microscope image. As can be seen from the figure, since SnO 2 is not added, the size and uniformity of the crystal particles of the obtained glass-ceramics are relatively poor.
  • the glass-ceramics provided by the embodiments of the present invention have high transparency, hardness and strength, wherein the visible light transmittance is above 91.5%, the Mohs hardness is high, the impact resistance is excellent, and the performance is far better than Comparative Example 1.

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Abstract

La présente invention concerne un matériau vitrocéramique, son procédé de préparation et son application dans des dispositifs à semi-conducteurs. Le matériau vitrocéramique comprend un verre de base, un agent de nucléation, un agent clarifiant, et un additif. Le matériau vitrocéramique selon la présente invention présente de multiples phases cristallines formant un système de phase polycristalline spécifique, surmonte les défauts de performance de la vitrocéramique ayant une phase cristalline unique, garantit non seulement la dureté élevée de la vitrocéramique, mais améliore également la transparence et la résistance aux chocs de la vitrocéramique, et convient également aux dispositifs à semi-conducteurs, et particulièrement satisfait des exigences d'utilisation des matériaux de panneaux et de panneaux arrière de téléphones portables haut de gamme (y compris 5G).
PCT/CN2022/094351 2021-04-28 2022-05-23 Matériau vitrocéramique, procédé de préparation associé et application correspondante dans des dispositifs à semi-conducteurs WO2022228583A1 (fr)

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CN202110462754.9A CN112876083B (zh) 2021-04-28 2021-04-28 一种微晶玻璃材料及其制备方法和在半导体器件中的应用
CN202110462754.9 2021-04-28

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