Low-expansion zinc-aluminum-silicon microcrystalline glass and preparation method thereof

Abstract

The invention provides low-expansion zinc-aluminum-silicon microcrystalline glass and a preparation method thereof, and belongs to the field of electronic ceramic materials. The material is prepared from the following components in percentage by weight: 15 to 25 percent of ZnO, 23 to 25 percent of Al2O3, 37 to 45 percent of SiO2, 10 to 15 percent of B2O3, 0 to 3 percent of MgO and 0 to 5 percent of K2O. The main crystalline phase of the zinc-aluminum-silicon microcrystalline glass provided by the invention is zinc-aluminum spinel ZnAl2O4, and the zinc-aluminum-silicon microcrystalline glass has the thermal expansion coefficient of 4.47-5.28 ppm / DEG C, the bending strength of 130-155 MPa, the Young modulus of 73-83 GPa, the dielectric constant of 5.24-6.91 and the dielectric loss of 2.3-2.9 * 10 <-3 >. The preparation method provided by the invention is low in cost, simple in process, beneficial to industrial production and suitable for a super-large-scale integrated circuit packaging substrate.

Description

Technical Field

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

[0002] Zinc-aluminum-silicon microcrystalline glass possesses excellent mechanical properties and has the potential to serve as a substrate for integrated circuit packaging. For example, invention patent CN202311204316.8 describes the preparation of zinc-aluminum-silicon microcrystalline glass using casting and other forming processes with ZnO: 5%~13%, Al2O3: 12%~22%, and SiO2: 40%~65%, exhibiting high transparency and high strength. However, it does not address thermal expansion properties, while very large-scale integrated circuits require packaging substrates with low coefficients of thermal expansion.

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

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

[0005] The formula consists of 15-25 wt% ZnO, 23-25 ​​wt% Al2O3, 37-45 wt% SiO2, 10-15 wt% B2O3, 0-3 wt% MgO, and 0-5 wt% K2O.

[0006] Furthermore, the preparation method of the above-mentioned low-expansion zinc-aluminum-silicon microcrystalline glass includes the following steps:

[0007] Step 1. Calculate and weigh the actual amount of each raw material based on the percentages of ZnO, Al2O3, SiO2, B2O3, MgO, and K2O in the formula;

[0008] Step 2. After mixing, pour the mixture into a crucible and place it in a lifting furnace to melt at 1500℃ for 1 hour;

[0009] Step 3. Use water quenching to make glass slag, then grind it to obtain glass powder;

[0010] Step 4. After ball milling for 2 hours, dry to obtain powder with uniform particle size;

[0011] Step 5. Granulate and dry press the mixture, then sinter it at 900~950℃ for 2 hours to obtain low-expansion zinc-aluminum-silicon microcrystalline glass.

[0012] The beneficial effects of this invention are as follows:

[0013] The present invention provides a zinc-aluminum-silicon microcrystalline glass with zinc-aluminum spinel ZnAl2O4 as the main crystalline phase and a low coefficient of thermal expansion of 4.47~5.28ppm / ℃.

[0014] The present invention provides a zinc-aluminum-silicon microcrystalline glass with a low dielectric constant of 5.24~6.91 and a low dielectric loss of 2.3~2.9×10⁻⁶. -3 This can improve the speed of signal transmission and reduce losses during transmission;

[0015] This invention improves the flexural strength to over 150 MPa by adding MgO or K2O, thereby enhancing packaging reliability. The addition of B2O3 or K2O lowers the sintering temperature to below 950°C, meeting the technical requirements of LTCC.

[0016] Furthermore, the low-expansion zinc-aluminum-silicon microcrystalline glass provided by this invention has low preparation cost and simple process, which is conducive to industrial production and suitable for use as a packaging substrate for ultra-large-scale integrated circuits. Attached Figure Description

[0017] Figure 1 The image shows the XRD pattern of a low-expansion zinc-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 three embodiments, and the formulation composition and process parameters of each embodiment are shown in Table 1.

[0020] Table 1

[0021] Furthermore, in the embodiments, the specific preparation process of the low-expansion zinc-aluminum-silicon microcrystalline glass is as follows:

[0022] Step 1. Calculate and weigh the actual amount of each raw material based on the percentages of ZnO, Al2O3, SiO2, B2O3, MgO, and K2O in the formula;

[0023] Step 2. After mixing, pour the mixture into a crucible and place it in a lifting furnace to melt at 1500℃ for 1 hour;

[0024] Step 3. Use water quenching to make glass slag, then grind it to obtain glass powder;

[0025] Step 4. After ball milling for 2 hours, dry to obtain powder with uniform particle size;

[0026] Step 5. Granulate and dry press the mixture, then sinter it at 900~950℃ for 2 hours to obtain low-expansion zinc-aluminum-silicon microcrystalline glass.

[0027] The thermal, mechanical, and dielectric properties of the three embodiments described above are detailed in Table 2.

[0028] Table 2

[0029] As shown in Table 2, the low-expansion zinc-aluminum-silicon microcrystalline glass provided by this invention has a thermal expansion coefficient of 4.47~5.28ppm / ℃, a bending strength of 130~155MPa, a Young's modulus of 73~83GPa, a dielectric constant of 5.24~6.91, and a dielectric loss of 2.3~2.9×10⁻⁶. -3 .

[0030] 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 low-expansion zinc-aluminum-silicon microcrystalline glass, characterized in that, It includes the following composition: ZnO 15~25wt%, Al2O3 23~25wt%, SiO2 37~45wt%, B2O3 10~15wt%, MgO 0~3wt%, K2O 0~5wt%.

2. The zinc-aluminum-silicon microcrystalline glass according to claim 1, characterized in that, The main crystalline phase is zinc aluminum spinel ZnAl2O4.

3. The zinc-aluminum-silicon microcrystalline glass according to claim 1, characterized in that, Thermal expansion coefficient 4.47~5.28ppm / ℃, flexural strength 130~155MPa, Young's modulus 73~83GPa, dielectric constant 5.24~6.91, dielectric loss 2.3~2.9×10 -3 .

4. The method for preparing zinc-aluminum-silicon microcrystalline glass according to claim 1, characterized in that, Includes the following steps: Step 1. Calculate and weigh the actual amount of each raw material based on the percentages of ZnO, Al2O3, SiO2, B2O3, MgO, and K2O in the formula; Step 2. After mixing, pour the mixture into a crucible and place it in a lifting furnace to melt at 1500℃ for 1 hour; Step 3. Use water quenching to make glass slag, then grind it to obtain glass powder; Step 4. After ball milling for 2 hours, dry to obtain powder with uniform particle size; Step 5. Granulate and dry press the mixture, then sinter it at 900~950℃ for 2 hours to obtain low-expansion zinc-aluminum-silicon microcrystalline glass.

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