CN111908797A - Low-thermal-expansion cordierite-based microcrystalline glass material and preparation method thereof - Google Patents
Low-thermal-expansion cordierite-based microcrystalline glass material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of electronic ceramic materials, and provides a low-thermal-expansion cordierite-based microcrystalline glass material and a preparation method thereof, which are used for packaging a very large scale integrated circuit. The microcrystalline glass material comprises the following components in percentage by mass: 15 to 19 wt% of MgO and Al2O326 to 30 wt% of SiO246 to 50 wt% of ZrO22 to 6 wt%, B2O31 to 5 wt%, K2O is 1-3 wt%; by introducing K2O as a modifier, ZrO2As a nucleating agent, B2O3As a burning reducing agent, part of (MgAl) is suppressed2Si3O10)0.6Phase conversion to Mg2Al4Si5O18Phase, thereby adjusting the coefficient of thermal expansion toward that of a Si chip (3.5X 10)‑6/deg.C) and is in the range of 2.5 to 3.5X 10‑6The temperature per DEG C is adjustable, and the thermal stability is good; at the same time, bending resistanceThe strength can reach 150 to 200MPa, the Young modulus can reach 80 to 95GPa, the dielectric constant is low by 5 to 6(@1MHz), the dielectric loss is low by 0.5 to 1 multiplied by 10‑3The (@1MHz) can improve the signal transmission speed and greatly reduce the power consumption; in conclusion, the low thermal expansion cordierite based glass-ceramic material is suitable for packaging a super large scale integrated circuit, can obviously reduce signal transmission delay and power consumption, and is well matched with a silicon chip.
Description
Technical Field
The invention belongs to the field of electronic ceramic materials, and relates to a low-thermal-expansion cordierite-based microcrystalline glass material and a preparation method thereof; especially suitable for very large scale integrated circuit package.
Background
In recent years, with the rapid development of information technology, the ultra-large scale and the multi-functionalization of integrated circuits are promoted, and the focus of people for seeking packaging materials with excellent performance becomes the focus of attention; MgO-Al2O3-SiO2The glass ceramics have the characteristics of low thermal expansion coefficient, excellent dielectric property and the like, but have the problems of poor mechanical property, high sintering temperature and the like.
For example, Journal of Non-Crystalline Solids, 2015, 419: 16-26 report, K2The influence of O on the performance of the magnesium-aluminum-silicon microcrystalline glass is that the microcrystalline glass comprises the following components in percentage by mass: 21.60 mol% of MgO and Al2O321.61 mol% of SiO254.00 mol% and K2O is 2.79 mol%; melting and insulating the mixed materials at 1550 ℃ for 6h, granulating and molding by using PVA (polyvinyl alcohol), and sintering at 925 ℃ for 6h to obtain the material with optimal comprehensive performance; the bending strength is 145MPa, and the thermal expansion coefficient is 5.63 multiplied by 10-6Dielectric constant of 7.51(@10 MHz)/° C, and dielectric loss of 14X 10-3(@10MHz), the disadvantages are low bending strength, high thermal expansion coefficient and high dielectric loss.
In view of the above problems, the inventor of the present invention discloses "a cordierite-based microcrystalline glass material and a method for producing the same" in the invention patent application No. 201810507515.9, wherein the microcrystalline glass composition is as follows by mass percent: 10 to 20 wt% of MgO and Al2O325 to 35 wt% of SiO 240 to 50 wt% of ZrO25 to 10 wt%, B2O31 to 5 wt%; melting and preserving heat for 1-2 h at 1400-1450 ℃ of the mixed material, granulating and molding by using acrylic acid, and sintering for 1-2 h at 875-925 ℃, wherein the finally obtained material has the following properties: bending strength of 160-230 MPa, Young's modulus of 80-100 GPa, dielectric constant of 4.5-5.0 (@1MHz), dielectric loss of 0.5-0.6 × 10-3(@1MHz) and a thermal expansion coefficient of 1.5 to 2.5X 10-6/℃；The disadvantages are that the dielectric constant is low, the thermal expansion coefficient is low, and the silicon chip can not be well matched with heat.
Disclosure of Invention
Aiming at the problems of poor mechanical property, mismatched thermal expansion coefficient, large dielectric loss and the like of the existing ceramic material in the background technology, which cause larger signal transmission delay, higher power consumption and the like, the invention provides a low-thermal-expansion cordierite-based microcrystalline glass material and a preparation method thereof, which can realize good thermal matching with a silicon chip, and also have higher bending strength and Young modulus and excellent dielectric property.
In order to achieve the purpose, the invention adopts the technical scheme that:
a low thermal expansion cordierite based microcrystalline glass material and a preparation method thereof are characterized in that the material comprises the following components by mass percent:
15-19 wt% of MgO,
Al2O326-30 wt%,
SiO246-50 wt%,
ZrO22-6 wt%,
B2O31 to 5wt percent,
K2O is 1 to 3 wt%.
The low thermal expansion cordierite based microcrystalline glass material and the preparation method thereof comprise the following steps:
step 1: with MgO, Al2O3、SiO2、ZrO2、B2O3、K2O is a component design formula, the actual dosage of the raw materials corresponding to each oxide is calculated according to the proportion, and the raw materials are uniformly mixed;
step 2: ball-milling for 2-4 hours, drying, placing the mixture in a crucible, melting at 1400-1450 ℃ for 1-2 hours, and pouring into deionized water to obtain transparent glass slag;
and step 3: ball-milling the obtained glass slag in a ceramic pot for 1-1.5 hours, and drying to obtain glass powder;
and 4, step 4: ball-milling the obtained glass powder in a nylon tank for 6-8 hours, and drying to obtain uniformly dispersed powder;
and 5: and adding acrylic acid into the powder for granulation, performing dry pressing molding, sintering at 900-950 ℃, and preserving heat for 1-2 hours to obtain the low-thermal-expansion cordierite-based microcrystalline glass.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a low-thermal expansion cordierite-based microcrystalline glass material, which belongs to a magnesium-aluminum-silicon system and is prepared by introducing K2O as a modifier, ZrO2As a nucleating agent, B2O3As a burning reducing agent, part of (MgAl) is suppressed2Si3O10)0.6Phase conversion to Mg2Al4Si5O18Phase, by calculation, Mg in the final material2Al4Si5O18The content of phase (MgAl) is 65.2-76.5%2Si3O10)0.6The content of the phase is 18.3-25.7%; the coefficient of thermal expansion of the glass-ceramic is mainly determined by the kind and content of the crystalline phase, since Mg2Al4Si5O18The coefficient of thermal expansion of the phases being 1.5X 10-6/℃，(MgAl2Si3O10)0.6The coefficient of thermal expansion of the phases is about 5.0X 10-6The content of different crystal phases can change the thermal stress in the material, thereby adjusting the thermal expansion coefficient to be close to that of a Si chip (3.5 multiplied by 10℃)-6/deg.C) and is in the range of 2.5 to 3.5X 10-6The temperature per DEG C is adjustable, and the thermal stability is good; meanwhile, the bending strength can reach 150-200 MPa, the Young modulus can reach 80-95 GPa, the dielectric constant is low by 5-6 (@1MHz), and the dielectric loss is low by 0.5-1 × 10-3(@1MHz), improve the signal transmission speed, has greatly reduced the power consumption; in conclusion, the low thermal expansion cordierite based glass-ceramic material is suitable for packaging a super large scale integrated circuit, can obviously reduce signal transmission delay and power consumption, and is well matched with a silicon chip. In addition, the sintering temperature of the invention is further reduced to below 950 ℃, the energy consumption is reduced, and the preparation method has simple process flow and rich raw material sources, and has important significance for industrial production.
Drawings
FIG. 1 is an XRD pattern of a low thermal expansion cordierite-based glass-ceramic of example 2.
FIG. 2 is an SEM image of a cross-section of a low thermal expansion cordierite-based crystallized glass of example 2.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
According to the formula: 15 wt% of MgO and Al2O326 wt% of SiO 250 wt% of ZrO26 wt% of B2O3Is 1 wt%, K2The O accounts for 2 wt%, the weight of the corresponding raw materials is accurately calculated, and after accurate weighing, ball milling is carried out for 2 hours to ensure that the raw materials are uniformly mixed; after drying, placing the mixture in a crucible for melting, heating to 1400 ℃, preserving heat for 1.5 hours, and performing water quenching after complete melting; then ball-milling the obtained glass slag by a wet method, drying to obtain glass powder, ball-milling for 6 hours by taking deionized water as a medium, and drying to obtain uniformly dispersed powder; the powder is sintered at 900 ℃ and kept warm for 1 hour after granulation and dry pressing forming, and the low thermal expansion cordierite based microcrystalline glass material is obtained.
The low thermal expansion cordierite based microcrystalline glass material, Mg, produced in this example2Al4Si5O18Phase content 73.4%, (Mg Al)2Si3O10)0.6The content of phase was 19.1%. The performance indexes are as follows: dielectric constant of 5.54(@1MHz), dielectric loss of 0.75X 10-3(@1MHz), coefficient of thermal expansion 2.72X 10-6/° c, flexural strength 175MPa, and young's modulus 92 Gpa.
Example 2
According to the formula: 16 wt% of MgO and Al2O327 wt% SiO249 wt% of ZrO25 wt%, B2O3Is 2 wt%, K2The O accounts for 1 wt%, the weight of the corresponding raw materials is accurately calculated, and after accurate weighing, ball milling is carried out for 2 hours to ensure that the raw materials are uniformly mixed; after drying, placing the mixture in a crucible for melting, heating to 1400 ℃, preserving heat for 2 hours, and completely meltingWater quenching is carried out; then ball-milling the obtained glass slag by a wet method, drying to obtain glass powder, ball-milling for 6 hours by taking deionized water as a medium, and drying to obtain uniformly dispersed powder; the powder is sintered at 900 ℃ and kept warm for 1.5 hours after granulation and dry pressing forming, and the low thermal expansion cordierite based glass ceramics material is obtained.
The XRD pattern of the low thermal expansion cordierite-based microcrystalline glass material prepared in this example is shown in FIG. 1, wherein the main crystal phase is Mg2Al4Si5O18The secondary crystal phase is (MgAl)2Si3O10)0.6And ZrO2(ii) a As shown in fig. 2, the darker region a is a crystalline phase, the bright region B is a glass phase, and the black region C is a hole, so that it can be seen that the crystalline phase accounts for a higher proportion and the hole is less, so that the material has a low thermal expansion coefficient and a higher mechanical property; more specifically, Mg2Al4Si5O18The content of phase (MgAl) is 65.2%2Si3O10)0.6The content of phase was 25.7%. The performance indexes are as follows: dielectric constant of 5.39(@1MHz), electric loss of 0.63X 10-3(@1MHz), coefficient of thermal expansion 3.32X 10-6/° c, bending strength 196MPa, and young's modulus 95 Gpa.
Example 3
According to the formula: 17 wt% of MgO and Al2O3Is 28 wt% SiO247 wt% of ZrO24 wt% of B2O3Is 1 wt%, K2The O accounts for 3 wt%, the weight of the corresponding raw materials is accurately calculated, and after accurate weighing, ball milling is carried out for 3 hours to ensure that the raw materials are uniformly mixed; after drying, placing the mixture in a crucible for melting, heating to 1450 ℃, preserving heat for 1 hour, and performing water quenching after complete melting; then ball-milling the obtained glass slag by a wet method, drying to obtain glass powder, ball-milling for 7 hours by taking deionized water as a medium, and drying to obtain uniformly dispersed powder; the powder is sintered at 925 ℃ and is kept warm for 1.5 hours after granulation and dry pressing forming, and the low thermal expansion cordierite based glass ceramics material is obtained.
The low thermal expansion cordierite based microcrystalline glass material, Mg, produced in this example2Al4Si5O18Phase content 68.4%, (MgAl)2Si3O10)0.6The content of phase was 22.6%. The performance indexes are as follows: dielectric constant of 5.43(@1MHz), dielectric loss of 0.77X 10-3(@1MHz), coefficient of thermal expansion 3.13X 10-6/° c, bending strength 173MPa, and young's modulus 90 Gpa.
Example 4
According to the formula: 15 wt% of MgO and Al2O330 wt% of SiO246 wt% of ZrO 23 wt% of B2O3Is 4 wt%, K2The O accounts for 2 wt%, the weight of the corresponding raw materials is accurately calculated, and after accurate weighing, ball milling is carried out for 4 hours to ensure that the raw materials are uniformly mixed; after drying, placing the mixture in a crucible for melting, heating to 1450 ℃, preserving heat for 1.5 hours, and performing water quenching after complete melting; then ball-milling the obtained glass slag by a wet method, drying to obtain glass powder, ball-milling for 8 hours by taking deionized water as a medium, and drying to obtain uniformly dispersed powder; the powder is sintered at 925 ℃ and is kept warm for 2 hours after granulation and dry pressing forming, and the low-thermal-expansion cordierite-based microcrystalline glass material is obtained.
The low thermal expansion cordierite based microcrystalline glass material, Mg, produced in this example2Al4Si5O18The content of phase (Mg Al) was 70.6%2Si3O10)0.6The content of phase was 21.5%. The performance indexes are as follows: dielectric constant of 5.62(@1MHz), dielectric loss of 0.86X 10-3(@1MHz), coefficient of thermal expansion 2.97X 10-6/° c, flexural strength 162MPa, and young's modulus 83 Gpa.
Example 5
According to the formula: 19 wt% of MgO and Al2O326 wt% of SiO247 wt% of ZrO2Is 2 wt%, B2O35 wt%, K2The O accounts for 1 wt%, the weight of the corresponding raw materials is accurately calculated, and after accurate weighing, ball milling is carried out for 4 hours to ensure that the raw materials are uniformly mixed; after drying, placing the mixture in a crucible for melting, heating to 1450 ℃, preserving heat for 2 hours, and performing water quenching after complete melting; then ball-milling the obtained glass slag by a wet method, and drying to obtain glass powderBall milling for 8 hours by taking deionized water as a medium, and drying to obtain uniformly dispersed powder; the powder is sintered at 950 ℃ and kept warm for 1 hour after granulation and dry pressing molding, and the low thermal expansion cordierite based microcrystalline glass material is obtained.
The low thermal expansion cordierite based microcrystalline glass material, Mg, produced in this example2Al4Si5O18The content of phase (MgAl) is 76.5%2Si3O10)0.6The content of phase was 18.3%. The performance indexes are as follows: dielectric constant of 5.77(@1MHz), dielectric loss of 0.88X 10-3(@1MHz), coefficient of thermal expansion 2.58X 10-6/° c, flexural strength 153MPa, and young's modulus 81 Gpa.
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 low thermal expansion cordierite based microcrystalline glass material is characterized in that the composition is as follows:
MgO：15～19wt％；
Al2O3：26～30wt％；
SiO2：46～50wt％；
ZrO2：2～6wt％；
B2O3：1～5wt％；
K2O：1～3wt％。
2. the method for producing a low thermal expansion cordierite-based microcrystalline glass material as defined in claim 1, comprising the steps of:
step 1: with MgO, Al2O3、SiO2、ZrO2、B2O3、K2O is a component design formula, and raw materials corresponding to the oxides are calculated according to the proportionThe actual amount of the raw materials is used, and the raw materials are uniformly mixed;
step 2: ball-milling for 2-4 hours, drying, placing the mixture in a crucible, melting at 1400-1450 ℃ for 1-2 hours, and pouring into deionized water to obtain transparent glass slag;
and step 3: ball-milling the obtained glass slag in a ceramic pot for 1-1.5 hours, and drying to obtain glass powder;
and 4, step 4: ball-milling the obtained glass powder in a nylon tank for 6-8 hours, and drying to obtain uniformly dispersed powder;
and 5: and adding acrylic acid into the powder for granulation, performing dry pressing molding, sintering at 900-950 ℃, and preserving heat for 1-2 hours to obtain the low-thermal-expansion cordierite-based microcrystalline glass.
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Cited By (5)
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| CN112939471A (en) * | 2021-03-15 | 2021-06-11 | 武汉理工大学 | High-thermal-conductivity low-expansion low-dielectric microcrystalline glass and preparation method thereof |
| CN113277852A (en) * | 2021-05-21 | 2021-08-20 | 景德镇陶瓷大学 | Cordierite-based microcrystalline glass combined silicon carbide ceramic material and preparation method thereof |
| CN113354288A (en) * | 2021-06-21 | 2021-09-07 | 向承刚 | Microcrystalline glass plate and preparation method thereof |
| CN113754296A (en) * | 2021-10-09 | 2021-12-07 | 南京琅璃材料有限公司 | Continuous glass fiber containing cordierite microcrystals |
| CN114031297A (en) * | 2021-11-24 | 2022-02-11 | 中建材蚌埠玻璃工业设计研究院有限公司 | Cordierite-based porous glass ceramic and preparation method thereof |
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|---|---|---|---|---|
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| CN113277852A (en) * | 2021-05-21 | 2021-08-20 | 景德镇陶瓷大学 | Cordierite-based microcrystalline glass combined silicon carbide ceramic material and preparation method thereof |
| CN113277852B (en) * | 2021-05-21 | 2022-08-02 | 景德镇陶瓷大学 | Cordierite-based microcrystalline glass combined silicon carbide ceramic material and preparation method thereof |
| CN113354288A (en) * | 2021-06-21 | 2021-09-07 | 向承刚 | Microcrystalline glass plate and preparation method thereof |
| CN113354288B (en) * | 2021-06-21 | 2023-02-03 | 向承刚 | Microcrystalline glass plate and preparation method thereof |
| CN113754296A (en) * | 2021-10-09 | 2021-12-07 | 南京琅璃材料有限公司 | Continuous glass fiber containing cordierite microcrystals |
| CN114031297A (en) * | 2021-11-24 | 2022-02-11 | 中建材蚌埠玻璃工业设计研究院有限公司 | Cordierite-based porous glass ceramic and preparation method thereof |
| CN114031297B (en) * | 2021-11-24 | 2023-08-22 | 中建材玻璃新材料研究院集团有限公司 | Cordierite-based porous glass ceramic and preparation method thereof |
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