CN108610035B - High-strength high-thermal-expansion ceramic substrate material and preparation method thereof - Google Patents

High-strength high-thermal-expansion ceramic substrate material and preparation method thereof Download PDF

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CN108610035B
CN108610035B CN201810507528.6A CN201810507528A CN108610035B CN 108610035 B CN108610035 B CN 108610035B CN 201810507528 A CN201810507528 A CN 201810507528A CN 108610035 B CN108610035 B CN 108610035B
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李波
边海勃
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University of Electronic Science and Technology of China
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Abstract

The present invention belongs to an electronic ceramic packaging materialThe field, in particular to a high-strength high-thermal-expansion ceramic substrate material and a preparation method thereof, which are suitable for ceramic packaging of large-scale integrated circuit chips, in particular for Ceramic Ball Grid Array (CBGA) packaging. The invention adopts a low-temperature co-firing process, the process is simple and easy to implement, the raw materials are green and environment-friendly, and do not contain limited pollutants in RoHS, and the material performance is stable; by redesigning the material formula, the dielectric property of the ceramic substrate material with high strength and high thermal expansion coefficient is excellent: a dielectric constant of 5 to 6 and a small dielectric loss of less than 1.0X 10‑3The bending strength is 170-190MPa, the Young's modulus is 60-70GPa, and the thermal expansion coefficient is 10-11 × 10‑6/° c; the perfect thermal matching with the PCB with the specific thermal expansion coefficient can be realized, and an excellent ceramic substrate material is provided for IC device packaging; meanwhile, the substrate material is low in production cost and has industrial popularization benefits.

Description

High-strength high-thermal-expansion ceramic substrate material and preparation method thereof
Technical Field
The invention belongs to the field of electronic ceramic packaging materials, and relates to a high-strength high-thermal-expansion ceramic substrate material and a preparation method thereof, which are suitable for ceramic packaging of large-scale integrated circuit chips, in particular for Ceramic Ball Grid Array (CBGA) packaging.
Background
The rapid development of modern electronic information technology greatly promotes the development of electronic devices in the aspects of high performance, high reliability, low cost, miniaturization, portability, popularization and the like. The development of ICs (integrated circuits) has greatly increased the density of circuits, with an IC chip carrying a density of circuit functions that is orders of magnitude greater than conventional printed circuits, particularly VLSI (very large scale integration). The advantages of ICs are only optimal when integrated with other resistors, capacitors, multi-chip hybrids, etc., and thus the circuits still need to be assembled, sometimes as well as the ICs themselves packaged into devices to handle the harsh environment. IC packaging has long developed internationally into a separate industry and constitutes, with IC design, IC manufacturing and chip testing, four major pillars of the semiconductor industry. China has independently developed a batch of novel packaging structures, but generally speaking, the electronic packaging industry of China is still quite laggard.
Ball Grid Array (BGA) technology, which was emerging in the 90 s, is a surface mount type package in which ball leads are implanted in an array on the underside of a substrate on which a chip is mounted. BGA packaging is mainly classified into PBGA (plastic encapsulated BGA) and CBGA (ceramic BGA) according to the kind of a substrate; compared with plastics, the ceramic substrate material has the advantages that: (1) the dielectric constant and the loss are low, and the transmission rate of signals can be improved; (2) the high resistivity ensures the insulation between signal lines; (3) the ceramic material has higher heat conductivity, and can better dissipate heat when a multilayer substrate is manufactured; (4) the ball planting is easier than that of plastic, and the I/O number is large; (5) the stability is good, and the air-tightness test device can be used in occasions with high requirements on air tightness; (6) the passive device integration can be realized in the multilayer ceramic substrate manufactured by utilizing the thick film hybrid circuit technology; and thus higher than PBGA packing density. However, there are a number of problems with the ceramic encapsulation materials commonly used today: the material has poor thermal matching performance with electrode materials and chips, the thermal expansion coefficient of the substrate material is too poor in serialization, and the raw materials pollute the environment.
The invention patent with application publication number CN106904953A discloses a high thermal expansion coefficient ceramic material for high density packaging and a preparation method thereof, wherein the ceramic material comprises the following components in percentage by mass: SiO 22：55～70wt％，BaO：20～30wt％，B2O3：5～10wt％，Al2O3：2～5wt％，Y2O3: 0.1 to 1 wt%, and CrO2And ZrO2The mixture is as follows: 1-3 wt%; the prepared low-temperature co-fired ceramic material with high expansion coefficient has the dielectric constant (5-6) and the dielectric loss tan delta<4.0×10-3The coefficient of thermal expansion is 12-15 ppm/DEG C, the bending strength is as high as 170-240 MPa, and the Young's modulus is 50-70 GPa. The invention patent with application publication number CN106045323A discloses a ceramic material with high thermal expansion coefficient and a preparation method thereof, wherein the formula of the ceramic material with high thermal expansion coefficient is as follows: CaO: 20 to 65 wt%, B2O3：5～15wt％，SiO2：20～55wt％，Al2O3：0～10wt％，ZrO2：0～10wt％，Cr2O3Or Co2O3: 0 to 2 wt% and 25 to 65 wt% of quartz sand. The dielectric constant of the material is 5.0-6.5, and the dielectric loss is less than 1.0 multiplied by 10-3Insulation resistivity > 1.0X 108Omega cm, thermal expansion coefficient of 8.5-12.5 x 10-6V. C. The span of the thermal expansion coefficient of the above materials is too large to be compatible with the thermal expansion coefficient of 10-11 ppm/DEG C in the futureThe novel PCB is subjected to thermal matching, and is difficult to meet the application under certain environmental conditions; and the raw materials all contain Cr element, which can cause environmental pollution.
Therefore, it is urgently needed to research a high-strength and high-thermal-expansion ceramic substrate material with a serial thermal expansion coefficient, so that the thermal expansion coefficient of the material can be 10-11 multiplied by 10 in the future-6The novel PCB board at/deg.c is thermally matched and reduces contamination of heavy metals in the raw material.
Disclosure of Invention
The invention aims to provide a high-strength high-thermal-expansion ceramic substrate material and a preparation method thereof aiming at the defects of the prior art, the ceramic substrate material has excellent dielectric property, high bending strength, high Young modulus, high thermal expansion coefficient and stable material property, and in addition, the material has small influence on human health and is beneficial to environmental protection.
In order to achieve the purpose, the invention adopts the technical scheme that:
a high-strength high-thermal-expansion ceramic substrate material is characterized in that,
the high-strength high-heat-expansion ceramic substrate material comprises the following components in percentage by weight (wt%):
B2O3：5～10wt％；
BaO：25～35wt％；
SiO2：55～65wt％；
Al2O3：1～5wt％；
ZrO2+Sm2O3: 1 to 10 wt%, wherein ZrO2And Sm2O3Mixing at any ratio.
The preparation method of the high-strength high-thermal-expansion ceramic substrate material is characterized by comprising the following steps of:
step 1: with B2O3、BaO、SiO2、Al2O3、ZrO2、Sm2O3The raw materials are calculated, weighed and uniformly mixed according to the formula proportion to obtain a mixture;
step 2: performing ball milling, drying and sieving on the mixture obtained in the step 1 to obtain uniformly dispersed powder;
and step 3: putting the powder obtained in the step 2 into a crucible, and presintering the crucible in an electric furnace at the temperature of 600-700 ℃ for 2-3 hours;
and 4, step 4: grinding and sieving the pre-sintered material obtained in the step 3 to obtain uniformly dispersed powder, granulating, and performing compression molding to obtain a blank;
and 5: and (4) placing the blank obtained by the compression molding in the step (4) in an electric furnace, and sintering for 1-2 hours at the temperature of 900-950 ℃ after removing the glue to obtain the high-strength high-thermal-expansion ceramic substrate material.
The invention has the beneficial effects that:
the invention provides a high-strength high-thermal-expansion-coefficient ceramic substrate material and a preparation process thereof, wherein a low-temperature co-firing process is adopted, the process is simple and easy to implement, the raw materials are green and environment-friendly, do not contain limited pollutants (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls and polybrominated diphenyl ethers) in RoHS, and the material performance is stable; by redesigning the material formula, the dielectric property of the ceramic substrate material with high strength and high thermal expansion coefficient is excellent: a dielectric constant of 5 to 6 and a small dielectric loss of less than 1.0X 10-3The bending strength is 170-190MPa, the Young's modulus is 60-70GPa, and the thermal expansion coefficient is 10-11 × 10-6/° c; the future coefficient of thermal expansion of 10 to 11 x 10-6Perfect thermal matching of the novel PCB at/DEG C provides an excellent ceramic substrate material for IC device packaging; by adding Sm2O3The strength of the substrate material is remarkably improved, and the thermal expansion coefficient is controlled to be 10-11 multiplied by 10-6And the substrate material has low production cost and industrial popularization benefit.
Drawings
FIG. 1 is an SEM image of a cross-section of a high-strength, high-CTE ceramic substrate material of example 2 after low-temperature co-firing.
FIG. 2 is an XRD diffraction analysis chart of the high-strength and high-thermal-expansion-coefficient ceramic substrate material of example 2 after low-temperature co-firing.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
The specific implementation manner of the invention provides 5 examples, which are respectively numbered as No. 1-5, wherein the specific components of the high-strength high-thermal-expansion-coefficient ceramic substrate material are shown in the following table:
numbering B2O3 BaO SiO2 Al2O3 ZrO2+Sm2O3
No.1 5 25 65 1 4
No.2 7 28 60 2 3
No.3 8 26 55 4 7
No.4 10 27 58 3 2
No.5 6 32 59 2 1
The preparation process comprises the following steps:
calculating the actual dosage of the raw materials of each component according to the weight percentage of the oxides used in the formula in the table 1, weighing and uniformly mixing, ball-milling, drying and sieving to obtain mixed powder, presintering for 2-3 hours at 600-950 ℃, then grinding and sieving to obtain powder, granulating the powder material, dry-pressing and molding, sintering in air at 900-950 ℃, preserving heat for 1-2 hours, and naturally cooling to obtain the high-strength high-thermal expansion coefficient ceramic substrate material;
the high strength and high thermal expansion coefficient ceramic substrate materials prepared by the above examples were tested, and the properties are shown in table 2 below, wherein the microstructure of example No.2 is shown in fig. 1, and the XRD diffraction analysis of example No.2 is shown in fig. 2:
Figure BDA0001671618790000041
as can be seen from the above table, the present invention provides a high-strength high-thermal-expansion-coefficient ceramic substrate material with excellent dielectric properties: a dielectric constant of 5 to 6 and a small dielectric loss of less than 1.0X 10-3The bending strength is 170-190MPa, the Young's modulus is 60-70GPa, and the thermal expansion coefficient is 10-11 × 10-6/° c; the thermal expansion coefficient of 10-11 x 10 can be realized in the future-6Perfect thermal matching of the novel PCB at/° C.
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 (2)

1. A high-strength high-thermal-expansion ceramic substrate material is characterized in that,
the high-strength high-heat-expansion ceramic substrate material comprises the following components in percentage by weight (wt%):
B2O3：5～10wt％；
BaO：25～35wt％；
SiO2：55～65wt％；
Al2O3：1～5wt％；
ZrO2+Sm2O3: 1 to 10 wt%, wherein ZrO2And Sm2O3Mixing in any proportion;
the thermal expansion coefficient of the high-strength high-thermal-expansion ceramic substrate material is 10-11 multiplied by 10-6/℃。
2. A method of making a high strength, high thermal expansion ceramic substrate material as defined in claim 1, comprising the steps of:
step 1: with B2O3、BaO、SiO2、Al2O3、ZrO2、Sm2O3As raw material, according toCalculating according to the formula proportion, weighing and uniformly mixing to obtain a mixture;
step 2: performing ball milling, drying and sieving on the mixture obtained in the step 1 to obtain uniformly dispersed powder;
and step 3: putting the powder obtained in the step 2 into a crucible, and presintering the crucible in an electric furnace at the temperature of 600-700 ℃ for 2-3 hours;
and 4, step 4: grinding and sieving the pre-sintered material obtained in the step 3 to obtain uniformly dispersed powder, granulating, and performing compression molding to obtain a blank;
and 5: and (4) placing the blank obtained by the compression molding in the step (4) in an electric furnace, and sintering for 1-2 hours at the temperature of 900-950 ℃ after removing the glue to obtain the high-strength high-thermal-expansion ceramic substrate material.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106045323A (en) * 2016-05-27 2016-10-26 电子科技大学 High thermal expansion coefficient ceramic material and preparation method thereof
CN106430984A (en) * 2016-09-22 2017-02-22 陕西科技大学 Method for preparing microcrystal wollastonite glass from wollastonite
CN106746676A (en) * 2017-01-19 2017-05-31 内蒙古科技大学 A kind of Surface Crystallization devitrified glass containing rare earth and preparation method and application
CN106904953A (en) * 2017-03-24 2017-06-30 电子科技大学 High-density packages high thermal expansion coefficient ceramic material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106045323A (en) * 2016-05-27 2016-10-26 电子科技大学 High thermal expansion coefficient ceramic material and preparation method thereof
CN106430984A (en) * 2016-09-22 2017-02-22 陕西科技大学 Method for preparing microcrystal wollastonite glass from wollastonite
CN106746676A (en) * 2017-01-19 2017-05-31 内蒙古科技大学 A kind of Surface Crystallization devitrified glass containing rare earth and preparation method and application
CN106904953A (en) * 2017-03-24 2017-06-30 电子科技大学 High-density packages high thermal expansion coefficient ceramic material and preparation method thereof

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