High-strength calcium-aluminum-silicon glass-ceramics and method for preparing same

Abstract

The application provides a high-strength calcium-aluminum-silicon glass-ceramics and a preparation method thereof, and belongs to the field of electronic ceramic materials. The material composition is as follows: CaO is 15-25wt%, Al2O3 is 10-15wt%, SiO2 is 50-65wt%, and ZnO+BaO is 10wt%. The high-strength calcium-aluminum-silicon glass-ceramics provided by the application has the main crystal phase of wollastonite CaSiO3, the secondary crystal phase of barium feldspar BaAl2Si2O8 and quartz SiO2. By adjusting the Zn / Ba ratio, the bending strength 193MPa and the Young's modulus 79GPa are improved, the thermal expansion coefficient 5.11ppm / ℃ is improved, and the reliability of the ultra-large scale integrated circuit package is improved. In addition, the preparation method provided by the application has the advantages of low cost, simple process and the like, is beneficial to industrialized production, and has potential application value for the ultra-large scale integrated circuit package substrate.

Description

Technical Field

[0001] This invention belongs to the field of electronic ceramic materials, specifically relating to a high-strength calcium aluminum silicon microcrystalline glass and its preparation method; it can be applied to ultra-large-scale integrated circuit packaging substrates. Background Technology

[0002] Calcium-aluminum-silicon microcrystalline glass possesses advantages such as good mechanical strength and chemical corrosion resistance, and was widely used as a building material in the early days. For example, invention patent CN101973709A utilizes nano-silicon calcium glass waste to prepare calcium-aluminum-silicon nanocrystalline glass, with the following composition: SiO2: 55%–70%, CaO: 15%–22%, Al2O3: 3%–11%, Na2O+K2O: 8%–12%, B2O3: 0–1%, TiO2: 1%–2%, and P2O5: 1.5%–2.5%. However, the flexural strength of this material is too low, only 50–70 MPa, making it difficult to meet the mechanical performance requirements of ultra-large-scale integrated circuit packaging substrate materials.

[0003] Based on this, the present invention provides a high-strength calcium aluminum silicon microcrystalline glass and its preparation method. Summary of the Invention

[0004] This invention provides a high-strength calcium aluminum silicon microcrystalline glass and its preparation method, the technical solution of which is as follows:

[0005] The formula consists of 15-25 wt% CaO, 10-15 wt% Al2O3, 50-65 wt% SiO2, and 10 wt% ZnO+BaO.

[0006] Furthermore, the preparation method of the above-mentioned high-strength calcium aluminum silicon microcrystalline glass includes the following steps:

[0007] Step 1. Calculate and weigh the actual amount of each raw material based on the mass percentage of CaO, Al2O3, SiO2, ZnO, and BaO in the formula;

[0008] Step 2. After mixing and drying, pour the mixture into a crucible and place it in an electric furnace to melt at 1500-1600℃ for 1-2 hours;

[0009] Step 3. Pour the molten glass into deionized water and quench it to obtain glass slag, then grind it to obtain glass powder;

[0010] Step 4. Ball mill with zirconium balls and deionized water as the medium for 6-8 hours, then dry and sieve to obtain powder with uniform particle size;

[0011] Step 5. After granulation, the material is dry-pressed and sintered in an electric furnace at 900-950℃ for 1-2 hours to obtain high-strength calcium aluminum silicon microcrystalline glass.

[0012] Furthermore, the beneficial effects of the present invention are as follows:

[0013] This invention provides a high-strength calcium aluminum silicon microcrystalline glass, with wollastonite (CaSiO3) as the main crystalline phase and barium feldspar (BaAl2Si2O8) and quartz (SiO2) as the secondary crystalline phases. By adjusting the Zn / Ba ratio, the flexural strength is increased to 193 MPa and the Young's modulus to 79 GPa, and the coefficient of thermal expansion is improved to 5.11 ppm / ℃, thereby enhancing the reliability of integrated circuit packaging.

[0014] Furthermore, the present invention provides a high-strength calcium aluminum silicon microcrystalline glass with a dielectric constant of 6.5–7.3 (@1MHz) and a dielectric loss of 2.7–3.7 × 10⁻⁶. -3 (@1MHz) can improve signal transmission speed and reduce loss;

[0015] Furthermore, the high-strength calcium aluminum silicon microcrystalline glass provided by this invention has low preparation cost and simple process, which is conducive to industrial production and has potential application value for ultra-large-scale integrated circuit packaging substrates. Attached Figure Description

[0016] Figure 1 The image shows the XRD pattern of a high-strength calcium aluminum silicon microcrystalline glass in Example 2.

[0017] Figure 2 This is a SEM image of a high-strength calcium aluminum silicon microcrystalline glass of Example 2. Detailed Implementation

[0018] The present invention will be further described in detail below with reference to the embodiments.

[0019] The present invention provides four embodiments, and the formulation composition and process parameters of each embodiment are shown in Table 1.

[0020] Table 1

[0021]

[0022] Furthermore, in this embodiment, the specific preparation process of the high-strength calcium aluminum silicon microcrystalline glass is as follows:

[0023] Step 1. Calculate and weigh the actual amount of each raw material based on the mass percentage of CaO, Al2O3, SiO2, ZnO, and BaO in the formula;

[0024] Step 2. After mixing and drying, pour the mixture into a crucible and place it in an electric furnace to melt at 1500-1600℃ for 1-2 hours;

[0025] Step 3. Pour the molten glass into deionized water and quench it to obtain glass slag, then grind it to obtain glass powder;

[0026] Step 4. Ball mill with zirconium balls and deionized water as the medium for 6-8 hours, then dry and sieve to obtain powder with uniform particle size;

[0027] Step 5. After granulation, the material is dry-pressed and sintered in an electric furnace at 900-950℃ for 1-2 hours to obtain high-strength calcium aluminum silicon microcrystalline glass.

[0028] The mechanical, thermal, and dielectric properties of the four embodiments described above are detailed in Table 2.

[0029] Table 2

[0030]

[0031] As shown in Table 2, the high-strength calcium aluminum silicon microcrystalline glass provided by this invention has good mechanical properties: bending strength of 164–193 MPa and Young's modulus of 64–79 GPa; good thermal properties: coefficient of thermal expansion of 5.11–6.20 ppm / ℃; and good dielectric properties: dielectric constant of 6.5–7.3 (@1MHz) and dielectric loss of 2.7–3.7 × 10⁻⁶. -3 (@1MHz).

[0032] The above description is merely a specific embodiment of the present invention. Any feature disclosed in this specification may be replaced by other equivalent or similar features unless otherwise specified. All disclosed features, or steps in all methods or processes, may be combined in any way except for mutually exclusive features and / or steps.

Claims

1. A high-strength calcium-aluminum-silicon glass-ceramic, characterized in that, Composition: CaO 15-25 wt%, Al203 10-15 wt%, Si02 50-65 wt%, containing ZnO and BaO, ZnO+BaO 10 wt%, characterized in that the main crystal phase is wollastonite, the secondary crystal phase is celsian and quartz, characterized in that the bending strength is 164-193 MPa, the Young's modulus is 64-79 GPa, the thermal expansion coefficient is 5.11-6.20 ppm / °C, the dielectric constant is 6.5-7.3 @ 1 MHz, the dielectric loss is 2.7-3.7 x 10 -3 @ 1 MHz, characterized in that the preparation method comprises the following steps: Step 1. According to the mass percentage of CaO, Al2O3, SiO2, ZnO and BaO in the formula, the actual amount of each raw material is calculated and weighed; Step 2. After mixing and drying, pour into a crucible, and place in an electric furnace at 1500-1600℃ for 1-2 hours; Step 3. Pour the glass liquid into deionized water for water quenching to obtain glass slag, and grind to obtain glass powder; Step 4. Ball mill for 6-8 hours with zirconium balls and deionized water as the medium, dry, sieve and obtain powder with uniform particle size; Step 5. After granulation, dry pressing and sintering in an electric furnace at 900-950℃ for 1-2 hours, high-strength calcium-aluminum-silicon microcrystalline glass is obtained.

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