CN111732426A - Calcium-aluminum-silicon-based ceramic material for high-density packaging and preparation method thereof - Google Patents

Calcium-aluminum-silicon-based ceramic material for high-density packaging and preparation method thereof Download PDF

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CN111732426A
CN111732426A CN202010547961.XA CN202010547961A CN111732426A CN 111732426 A CN111732426 A CN 111732426A CN 202010547961 A CN202010547961 A CN 202010547961A CN 111732426 A CN111732426 A CN 111732426A
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李波
赵翔浔
高陈熊
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University of Electronic Science and Technology of China
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    • C04B35/22—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in calcium oxide, e.g. wollastonite
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention belongs to the technical field of electronic ceramic materials, and particularly provides a calcium-aluminum-silicon-based ceramic material for high-density packaging and a preparation method thereof, aiming at solving the problem of thermal mismatch between a ceramic substrate and a PCB (printed Circuit Board) under high-density packaging. In the invention, the calcium-aluminum-silicon-based ceramic material comprises the following components: al (Al)2O3：4～15wt％，B2O3：2～10wt％，CaO：20～50wt％，SiO2：40～70wt％，CeO2: 1 to 5 wt%. The calcium-aluminum-silicon-based ceramic material has stable and excellent performance, low dielectric constant and low dielectric loss, and is beneficial to efficient transmission of signals; the high bending strength (158-205 MPa) and the high Young modulus (69-72 GPa) provide enough stable support protection for the chip; the high thermal expansion coefficient (10.3-12.4 ppm/DEG C) and the PCB reach a proper matchThe matching degree reduces the thermal stress among materials, and prolongs the service life of the chip; in addition, the substrate material is low in preparation cost, relatively simple in process and stable in performance, and completely meets the requirement of high-density packaging.

Description

Calcium-aluminum-silicon-based ceramic material for high-density packaging and preparation method thereof
Technical Field
The invention belongs to the technical field of electronic ceramic materials, particularly relates to a ceramic material with a high thermal expansion coefficient, and particularly provides a calcium-aluminum-silicon-based ceramic material for high-density packaging and a preparation method thereof.
Background
At present, the ceramic packaging material is mainly Al2O3Its advantages are high moisture resistance, mechanical strength and thermal conductivity, and mature technology. Ceramic Ball Grid Array (CBGA) packaging structures are widely adopted for high-density packaging, but the problem of thermal mismatch can occur when ceramic packaging modules are installed on a PCB through a ball mounting technology; therefore, a packaging material with high thermal expansion coefficient, high bending strength and low dielectric constant is designed to meet the urgent need of high-density packaging.
In recent years, microcrystalline glass has been receiving much attention and research, for example, a magnesium aluminum silicon system has cordierite as a main crystal phase and a thermal expansion coefficient thereof<3 ppm/DEG C and the bending strength is more than or equal to 130 MPa; the main crystal phase of the calcium-boron-silicon system is wollastonite, the thermal expansion coefficient of the calcium-boron-silicon system is 5-6 ppm/DEG C, the bending strength of the calcium-boron-silicon system is 150MPa, and a representative product is A6 series of Ferro company in the United states; for example, in patent document CN108341662A, a method for preparing a low dielectric constant, low loss, high frequency ceramic substrate material is provided, which comprises the following components: al (Al)2O395-96% of SiO20.6 to 1.5 percent of CaO, 0.6 to 1.5 percent of CoO, 0.5 to 1.5 percent of CoO, the dielectric constant of the material is 6 to 7, and the dielectric loss is less than or equal to 0.0003; however, the patent document does not note thermal expansion coefficient and bending strength, which are two important indexes for measuring the thermal and mechanical properties of the substrate material; in addition, the melting temperature of the material reaches 1400-1600 ℃, the energy consumption in the preparation process is huge, and the production cost is high.
Based on the above, the invention provides the calcium-aluminum-silicon-based ceramic material for high-density packaging, which has high thermal expansion coefficient, excellent mechanical property and excellent electrical property and is used for meeting the requirement of secondary packaging of ceramic ball grid arrays in integrated circuits.
Disclosure of Invention
The invention aims to solve the problem of thermal mismatch between a ceramic substrate and a PCB (printed circuit board) under high-density packaging, and provides a calcium-aluminum-silicon-based ceramic material for high-density packaging; the material has high thermal expansion coefficient, is matched with a PCB (printed Circuit Board), has high bending strength, low dielectric constant and low dielectric loss, has stable performance, and can meet the requirements of high-density packaging in large-scale integrated circuits.
In order to achieve the purpose, the invention adopts the technical scheme that:
the calcium-aluminum-silicon-based ceramic material for high-density packaging is characterized by comprising the following components in percentage by mass: al (Al)2O3：4～15wt％，B2O3：2～10wt％，CaO：20～50wt％，SiO2：40～70wt％，CeO2：1～5wt％。
Furthermore, the main crystal phases of the calcium aluminum silicon-based ceramic material for high-density packaging are wollastonite, cristobalite and quartz.
The preparation method of the calcium-aluminum-silicon-based ceramic material for high-density packaging comprises the following steps:
step 1: calculating Al according to the formula2O3、B2O3、CaO、SiO2、CeO2Accurately weighing and mixing the raw materials according to the mass of the raw materials;
step 2: performing ball milling, drying and sieving on the mixture obtained in the step 1 to obtain uniformly dispersed dry powder;
and step 3: putting the dried powder obtained in the step 2 into a crucible, and presintering the crucible in an electric furnace at the temperature of 600-770 ℃ for 1-3 hours;
and 4, step 4: performing ball milling, drying and sieving on the pre-sintered material obtained in the step 3 again to obtain uniformly dispersed powder;
and 5: granulating the powder obtained in the step (4) by using acrylic acid, and performing dry pressing to obtain a blank;
step 6: and (4) placing the blank obtained by the press forming in the step (5) in an electric furnace, removing the glue, and sintering at 880-980 ℃ for 1-3 hours to obtain the calcium-aluminum-silicon-based ceramic material for high-density packaging.
The invention has the beneficial effects that:
the invention provides a calcium-aluminum-silicon-based ceramic material for high-density packaging, which has excellent stabilityThe performance is low in dielectric constant and dielectric loss, and high-efficiency transmission of signals is facilitated; doping with right amount of rare earth oxide CeO2The crystallization activation energy can be effectively reduced, and the crystallinity is increased, so that the bending strength (to 158-205 MPa) and the Young modulus (to 69-72 GPa) of the material are improved, and sufficient and stable support protection is provided for the chip; as the cristobalite phase has high thermal expansion coefficient (50 ppm/DEG C), the increase of the content can improve the thermal expansion coefficient (10.3-12.4 ppm/DEG C), achieve the thermal matching degree with a PCB (printed Circuit Board), reduce the thermal stress among materials and prolong the service life of a chip. Meanwhile, the substrate material is low in preparation cost, relatively simple in process and stable in performance, and completely meets the requirement of high-density packaging.
Drawings
Fig. 1 is an XRD pattern of the calcium aluminum silicon-based ceramic material for high density packaging prepared in example 4.
Fig. 2 is an SEM image of the high-density calcium-aluminum-silicon-based ceramic material for encapsulation prepared in example 4.
Detailed Description
The invention is further described below with reference to specific examples.
The present invention provides 4 embodiments; the actual proportions and the preparation processes of the components of the calcium-aluminum-silicon-based ceramic material for high-density packaging in the embodiments 1 to 4 are shown in the table 1, and the performance test results of the embodiments 1 to 4 are shown in the table 2;
in the embodiment, the preparation process of the calcium-aluminum-silicon-based ceramic material for high-density packaging is as follows:
step 1: calculating Al according to the formula2O3、B2O3、CaO、SiO2、CeO2Accurately weighing and mixing the raw materials according to the mass of the raw materials;
step 2: performing ball milling, drying and sieving on the mixture obtained in the step 1 to obtain uniformly dispersed dry powder;
and step 3: putting the dried powder obtained in the step 2 into a crucible, and presintering the crucible in an electric furnace at the temperature of 600-770 ℃ for 1-3 hours;
and 4, step 4: performing ball milling, drying and sieving on the pre-sintered material obtained in the step 3 again to obtain uniformly dispersed powder;
and 5: granulating the powder obtained in the step (4) by using acrylic acid, and performing dry pressing to obtain a blank;
step 6: and (3) placing the blank obtained by the press forming in the step (5) in an electric furnace, removing the glue, and sintering at 880-980 ℃ for 1-3 hours to obtain the calcium-aluminum-silicon-based ceramic material for high-density packaging, wherein the test results are shown in Table 2.
TABLE 1
Figure BDA0002541425760000031
TABLE 2
Figure BDA0002541425760000032
The XRD and SEM images of the calcium-aluminum-silicon-based ceramic material for high-density packaging prepared in example 2 are shown in figure 1 and figure 2 respectively; as can be seen from fig. 1, the calcium aluminum silicon-based ceramic material for high density packaging mainly comprises three crystal phases: wollastonite, cristobalite and quartz phase, wherein the increase of the content of the cristobalite phase improves the thermal expansion coefficient of the material; as can be seen from FIG. 2, a number of white wollastonite grains are contained in the amorphous glass phase with appropriate amounts of CeO2The incorporation reduces the crystallization activation energy and increases the wollastonite crystallization, and the wollastonite grains improve the work of fracture by bending and passivating the crack tips in the material, which prevents the cracks from passing through the crystalline phase and improves the flexural strength of the material.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.

Claims (3)

1. The calcium-aluminum-silicon-based ceramic material for high-density packaging is characterized by comprising the following components in percentage by mass: al (Al)2O3：4～15wt％，B2O3：2～10wt％，CaO：20～50wt％，SiO2：40～70wt％，Ce O2：1～5wt％。
2. The calcium aluminum silicon-based ceramic material for high-density packaging as claimed in claim 1, wherein the main crystal phases of the calcium aluminum silicon-based ceramic material for high-density packaging are wollastonite, cristobalite and quartz.
3. The method for preparing a calcium aluminum silicon-based ceramic material for high-density packaging according to claim 1, comprising the steps of:
step 1: calculating Al according to the formula2O3、B2O3、CaO、SiO2、CeO2Accurately weighing and mixing the raw materials according to the mass of the raw materials;
step 2: performing ball milling, drying and sieving on the mixture obtained in the step 1 to obtain uniformly dispersed dry powder;
and step 3: putting the dried powder obtained in the step 2 into a crucible, and presintering the crucible in an electric furnace at the temperature of 600-770 ℃ for 1-3 hours;
and 4, step 4: performing ball milling, drying and sieving on the pre-sintered material obtained in the step 3 again to obtain uniformly dispersed powder;
and 5: granulating the powder obtained in the step (4) by using acrylic acid, and performing dry pressing to obtain a blank;
step 6: and (4) placing the blank obtained by the press forming in the step (5) in an electric furnace, removing the glue, and sintering at 880-980 ℃ for 1-3 hours to obtain the calcium-aluminum-silicon-based ceramic material for high-density packaging.
CN202010547961.XA 2020-06-16 2020-06-16 Calcium-aluminum-silicon-based ceramic material for high-density packaging and preparation method thereof Pending CN111732426A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06227858A (en) * 1993-02-02 1994-08-16 Sumitomo Metal Ind Ltd Ceramic substrate
CN1718641A (en) * 2005-06-21 2006-01-11 沈阳工业大学 Enamel powder for electrophoresis coating and its preparation
CN110342915A (en) * 2019-08-01 2019-10-18 电子科技大学 A kind of high thermal expansion calcium borosilicate base ceramic packaging material and preparation method thereof
CN110357597A (en) * 2019-08-01 2019-10-22 电子科技大学 High thermal expansion ceramic baseplate material of a kind of calcium borosilicate system and preparation method thereof
EP3632875A1 (en) * 2013-05-20 2020-04-08 Corning Incorporated Porous ceramic article and method of manufacturing the same

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06227858A (en) * 1993-02-02 1994-08-16 Sumitomo Metal Ind Ltd Ceramic substrate
CN1718641A (en) * 2005-06-21 2006-01-11 沈阳工业大学 Enamel powder for electrophoresis coating and its preparation
EP3632875A1 (en) * 2013-05-20 2020-04-08 Corning Incorporated Porous ceramic article and method of manufacturing the same
CN110342915A (en) * 2019-08-01 2019-10-18 电子科技大学 A kind of high thermal expansion calcium borosilicate base ceramic packaging material and preparation method thereof
CN110357597A (en) * 2019-08-01 2019-10-22 电子科技大学 High thermal expansion ceramic baseplate material of a kind of calcium borosilicate system and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
成钧等: "氧化铈对CaO-Al2O3-SiO2系微晶玻璃烧结和性能的影响", 《中国有色金属学报》 *
王艺慈: "《包钢高炉渣制备微晶玻璃的析晶行为》", 31 January 2014, 北京：冶金工业出版社 *

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