CN102173587A - Glass ceramic material for electronic substrate and preparation method thereof - Google Patents
Glass ceramic material for electronic substrate and preparation method thereof Download PDFInfo
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- CN102173587A CN102173587A CN 201110051412 CN201110051412A CN102173587A CN 102173587 A CN102173587 A CN 102173587A CN 201110051412 CN201110051412 CN 201110051412 CN 201110051412 A CN201110051412 A CN 201110051412A CN 102173587 A CN102173587 A CN 102173587A
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Abstract
The invention discloses a glass ceramic material for an electronic substrate and a preparation method thereof and relates to the technology of electronic materials. The glass ceramic material comprises the following components: 33 to 50 molar percent of CaO, 12 to 30 molar percent of B2O3, 30 to 50 molar percent of SiO2, 0 to 2 molar percent of ZnO, 0 to 2 molar percent of P2O5, 0 to 2 molar percent of ZrO2, and 0 to 2 molar percent of TiO2. The prepared glass ceramic material has a low dielectric constant epsilon which is equal to 6.5 to 7.2, 1MHz, and low dielectric losses tgdelta which is less than 0.003, 1 MHz.
Description
Technical field
The present invention relates to electronic material technology.
Background technology
Along with miniaturization, slimming, the integrated and high frequency development of electronics, more and more stricter requirement has been proposed in aspects such as the low-k of miniaturization, densification, low resistanceization and the baseplate material of integrated circuit wiring, low-thermal-expansion rate, high heat conductance.The traditional ceramics substrate adopts Al usually
2O
3, material such as mullite, AlN, but because its sintering temperature is at 1500～1900 ℃, if adopt sintering method simultaneously, conductor material can only be selected insoluble metal Mo and W etc., certainly will cause a series of insoluble problems like this: (1) burning altogether need carry out in reducing atmosphere, increased technology difficulty, sintering temperature is too high, needs to adopt the special sintering stove; (2) because the resistivity of Mo and W itself is higher, and the cloth line resistance is big, the signal transmission causes distortion easily, and loss increases, and the wiring miniaturization is restricted; (3) specific inductivity of dielectric material is all bigger than normal, therefore can increase signal transmission delay time, particularly is not suitable for the ultra-high frequency circuit.In order to address the above problem, nineteen eighty-two by Hughes Electronics developed glass mixes with pottery altogether the low-temperature co-fired ceramic substrate of burning (Low Temperature Co-fired Ceramic, LTCC).Because its firing temperature is about in the of 900 ℃, the conductor wiring material can adopt the low Au of resistivity, Ag, Cu, Ag-Pd etc., can realize the miniaturization wiring.And,, must reduce signal delay time, and signal transmission delay time is with the square root of dielectric material specific inductivity for adapting to the needs of high speed circuit
Be directly proportional.For this reason, for baseplate material, must reduce the specific inductivity of dielectric material.Therefore, the low temperature co-fired low-k ceramic substrate material of exploitation has broad application prospects.
At present, the LTCC material has been realized industrialization in developed countries such as Japan, the U.S..Many LTCC material produce producer can provide supporting series product.But still belong to the starting stage at home, the material system and the device that have independent intellectual property right almost are blank.Domestic urgent need is developed LTCC porcelain and pdm substrate seriation, that independent intellectual property right is arranged.Low-temperature sintering low-k stupalith can be divided into three major types: devitrified glass system (also claiming glass-ceramic), glass add compound system, the amorphous glass system of ceramic stopping composition.In recent years, people have carried out a large amount of research on devitrified glass, have developed many sintering temperature and low low-k ceramic systems.The devitrified glass system is the equally distributed matrix material of microcrystal and glassy phase, generally constitutes glass reticulattion by boron and silicon, and the formation thing of these glass adds the reticulattion that the oxide-based element of reductive can be rebuild glass that is difficult to of unit price or two valency alkalescence.Many LTCC are based on and prepare on the borosilicate glass basis, as CaO-B
2O
3-SiO
2Microcrystalline glass in series.
United States Patent (USP) (US Patent 5258335) has been invented the low temperature co-fired CaO-B of a kind of low-k by Ferro company
2O
3-SiO
2The system glass ceramic material, each is formed proportioning and is: CaO 35～65wt%, B
2O
30～50wt%, SiO
210～65wt%.Adopt this glass ceramic material of traditional glass prepared, be about to the material powder mixing and ball milling, drying, in alumina crucible in 1400～1500 ℃ of complete fusions and homogenizing.800～950 ℃ of sintering.The kind of crystalline that this glass-ceramic can be separated out is CaOSiO
2And CaOB
2O
3Gained glass-ceramic DIELECTRIC CONSTANT≤7.9 (1KHz), dielectric loss tg δ＜0.003 (1KHz).Which kind of feedstock production vitreum of the undeclared employing of this patent.
Chinese invention patent (application number 02124131.7) has been invented a kind of used for high-frequency chip inductor glass-ceramic by Tsing-Hua University, by CaO, B
2O
3, SiO
2, ZnO, P
2O
5Five kinds of one-tenth are grouped into, and the proportioning of each composition is: CaO 25～60wt%, B
2O
310～50wt%, SiO
210～60wt%, ZnO 1～10wt%, P
2O
51～5wt%.The preparation method of this glass ceramic material adopts traditional glass technology, is about to CaO, B
2O
3, SiO
2, ZnO, P
2O
5The powder mixing and ball milling, drying, in alumina crucible in 1300～1400 ℃ of complete fusions and homogenizing.Melts is obtained glass cullet through shrend, obtain the glass powder that median size is 0.5～2.0 μ m through wet ball grinding, again through glass-ceramic DIELECTRIC CONSTANT=4.9～5.5 (1MHz) of sintering preparation, dielectric loss tg δ=0.001～0.0025 (1MHz), and sintering temperature lower (750～850 ℃) can be burnt altogether with silver electrode.
Summary of the invention
Technical problem to be solved by this invention provides the electric substrate microcrystal glass material of a kind of low-k and low-dielectric loss.
The technical scheme that the present invention solve the technical problem employing is, a kind of microcrystal glass material is provided, and component comprises: CaO:33～50mol%, B
2O
3: 12～30mol%, SiO
2: 30～50mol%, ZnO:0～2mol%, P
2O
5: 0～2mol%, ZrO
2: 0～2mol%, TiO
2: 0～2mol%.
The present invention also provides a kind of preparation method of microcrystal glass material, may further comprise the steps:
(1) accurately takes by weighing quartz sand, lime carbonate, borocalcite and ZnO, P by predetermined formulation
2O
5, ZrO
2, TiO
2Ball milling 0.5～3 hour mixes it, drying;
(2) compound is joined in the platinum crucible that is incubated in the high temperature silicon molybdenum rod furnace in batches, be warming up to 1380～1450 ℃ of insulations 2～5 hours, found evenly, used quartz glass bar to stir once every 1 hour in order to make it;
(3) the fusion clarification back cooling of waiting to prepare burden is poured melts into that shrend obtains transparent glass cullet body in the distilled water;
(4) gained glass cullet body obtains the glass powder of median size at 0.8～5.2 μ m through wet ball grinding;
(5) after the repressed moulding of gained glass powder, at 850～950 ℃ of sintering and be incubated 1～4 hour, promptly get microcrystal glass material.
Described predetermined formulation means the composition of raw materials according to following component conversion:
CaO：33～50mol％，B
2O
3：12～30mol％，SiO
2：30～50mol％，ZnO：0～2mol％，P
2O
5：0～2mol％，ZrO
2：0～2mol％，TiO
2：0～2mol％。
The microcrystal glass material of the present invention's preparation has following characteristics:
(1) this microcrystal glass material can be at 850～950 ℃ of dense sinterings, and the microtexture of sintered compact is made up of a large amount of fine-grains, more glassy phase and a small amount of pore, is a kind of typical devitrified glass, as shown in Figure 1.
(2) the prepared devitrified glass of the present invention have low-k (ε=6.0～7.2,1MHz) and low-dielectric loss (tg δ＜0.003,1MHz).
(3) the present invention adopts ZnO, P
2O
5, ZrO
2, TiO
2As the nucleus agent, can promote the glass nucleus to form, help crystalline phase and generate.
(4) the present invention is defined as the low boron high calcium district of low silicon with glass formula.By increasing the content of CaO in the prescription, help improving wollastonite principal crystalline phase content, reduce sintering temperature.
(5) the microcrystal glass material sintering temperature lower (850～950 ℃) of the present invention's preparation can be burnt with the silver electrode of low-resistivity well altogether.
(6) microcrystal glass material of the present invention's preparation is applicable to and makes low temperature co-fired multilayer ceramic substrate.
The invention will be further described below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is differential thermal analysis (DTA) curve of microcrystal glass material of the present invention.
Fig. 2 is the scanning electron microscope of devitrified glass section of the present invention micro-(SEM) photo.
Embodiment
Embodiment 1
CaO (38mol%) in molar ratio, B
2O
3(20mol%), SiO
2(42mol%), can convert and obtain CaCO
3, CaB
2O
4, SiO
2Consumption, accurately take by weighing CaCO according to the consumption that calculates gained
3, CaB
2O
4, SiO
2After batch mixing is even, the platinum crucible of packing into, fusion cast glass (1420 ℃, insulation 2h) obtains transparent glass cullet body with the melten glass shrend.The glass cullet body obtains the glass powder that median size is 5.1 μ m through wet ball grinding (with deionized water, zirconium ball is medium, 12 hours time).After granulation (glass powder and 8% polyvinyl alcohol), dry-pressing formed under 20MPa pressure.Raw cook is warmed up to 950 ℃ of sintering and is incubated 30 minutes behind 550 ℃ of binder removals, promptly obtains devitrified glass, and performance is as shown in table 1.
Embodiment 2
CaO (43mol%) in molar ratio, B
2O
3(18mol%), SiO
2(39mol%), can convert and obtain CaCO
3, CaB
2O
4, SiO
2Consumption, accurately take by weighing CaCO according to the consumption that calculates gained
3, CaB
2O
4, SiO
2After batch mixing is even, the platinum crucible of packing into, fusion cast glass (1400 ℃, insulation 3h) obtains transparent glass cullet body with the melten glass shrend.The glass cullet body obtains the glass powder that median size is 2.4 μ m through wet ball grinding (with deionized water, zirconium ball is medium, 48 hours time).After granulation (glass powder and 8% polyvinyl alcohol), dry-pressing formed under 20MPa pressure.Raw cook is warmed up to 850 ℃ of sintering and is incubated 60 minutes behind 550 ℃ of binder removals, promptly obtains devitrified glass, and performance is as shown in table 1.
Embodiment 3
CaO (46mol%) in molar ratio, B
2O
3(16mol%), SiO
2(36mol%), ZnO (2mol%) can convert and obtain CaCO
3, CaB
2O
4, SiO
2, ZnO consumption, accurately take by weighing CaCO according to the consumption that calculates gained
3, CaB
2O
4, SiO
2After batch mixing is even, the platinum crucible of packing into, fusion cast glass (1450 ℃, insulation 2h) obtains transparent glass cullet body with the melten glass shrend.The glass cullet body obtains the glass powder that median size is 0.9 μ m through wet ball grinding (with deionized water, zirconium ball is medium, 72 hours time).After granulation (glass powder and 8% polyvinyl alcohol), dry-pressing formed under 20MPa pressure.Raw cook is warmed up to 900 ℃ of sintering and is incubated 120 minutes behind 550 ℃ of binder removals, promptly obtains devitrified glass, and performance is as shown in table 1.
Embodiment 4
CaO (47mol%) in molar ratio, B
2O
3(13mol%), SiO
2(39mol%), ZrO
2(1mol%), can convert and obtain CaCO
3, CaB
2O
4, SiO
2, ZrO
2Consumption, accurately take by weighing CaCO according to the consumption that calculates gained
3, CaB
2O
4, SiO
2, ZrO
2After batch mixing is even, the platinum crucible of packing into, fusion cast glass (1380 ℃, insulation 4h) obtains transparent glass cullet body with the melten glass shrend.The glass cullet body obtains the glass powder that median size is 1.3 μ m through wet ball grinding (with deionized water, zirconium ball is medium, 60 hours time).After granulation (glass powder and 8% polyvinyl alcohol), dry-pressing formed under 20MPa pressure.Raw cook is warmed up to 850 ℃ of sintering and is incubated 30 minutes behind 550 ℃ of binder removals, promptly obtains devitrified glass, and performance is as shown in table 1.
Embodiment 5
CaO (47mol%) in molar ratio, B
2O
3(12mol%), SiO
2(39mol%), TiO
2(2mol%) can convert and obtain CaCO
3, CaB
2O
4, SiO
2, TiO
2Consumption, accurately take by weighing CaCO according to the consumption that calculates gained
3, CaB
2O
4, SiO
2, TiO
2After batch mixing is even, the platinum crucible of packing into, fusion cast glass (1390 ℃, insulation 3h) obtains transparent glass cullet body with the melten glass shrend.The glass cullet body obtains the glass powder that median size is 3.5 μ m through wet ball grinding (with deionized water, zirconium ball is medium, 36 hours time).After granulation (glass powder and 8% polyvinyl alcohol), dry-pressing formed under 20MPa pressure.Raw cook is warmed up to 950 ℃ of sintering and is incubated 180 minutes behind 550 ℃ of binder removals, promptly obtains devitrified glass, and performance is as shown in table 1.
Embodiment 6
CaO (47mol%) in molar ratio, B
2O
3(13mol%), SiO
2(39mol%), P
2O
5(1mol%) can convert and obtain CaCO
3, CaB
2O
4, SiO
2, P
2O
5Consumption, accurately take by weighing CaCO according to the consumption that calculates gained
3, CaB
2O
4, SiO
2, P
2O
5After batch mixing is even, the platinum crucible of packing into, fusion cast glass (1410 ℃, insulation 2h) obtains transparent glass cullet body with the melten glass shrend.The glass cullet body obtains the glass powder that median size is 4.2 μ m through wet ball grinding (with deionized water, zirconium ball is medium, 24 hours time).After granulation (glass powder and 8% polyvinyl alcohol), dry-pressing formed under 20MPa pressure.Raw cook is warmed up to 900 ℃ of sintering and is incubated 240 minutes behind 550 ℃ of binder removals, promptly obtains devitrified glass, and performance is as shown in table 1.
The performance of sintered sample in each example of table 1
Claims (4)
1. the electric substrate microcrystal glass material is characterized in that, comprises following component:
CaO：33～50mol％，B
2O
3：12～30mol％，SiO
2：30～50mol％，ZnO：0～2mol％，P
2O
5：0～2mol％，ZrO
2：0～2mol％，TiO
2：0～2mol％。
2. electric substrate is characterized in that with the preparation method of microcrystal glass material, may further comprise the steps:
(1) accurately takes by weighing quartz sand, lime carbonate, borocalcite and ZnO, P by predetermined formulation
2O
5, ZrO
2, TiO
2Ball milling 0.5～3 hour mixes it, drying;
(2) compound is warming up to 1380～1450 ℃ of insulations 2～5 hours, used quartz glass bar to stir once every 1 hour;
(3) the fusion clarification back cooling of waiting to prepare burden is poured melts into that shrend obtains transparent glass cullet body in the distilled water;
(4) gained glass cullet body obtains the glass powder of median size at 0.8～5.2 μ m through wet ball grinding;
(5) after the repressed moulding of gained glass powder, at 850～950 ℃ of sintering and be incubated 1～4 hour, promptly get microcrystal glass material;
Described predetermined formulation means the composition of raw materials according to following component conversion:
CaO：33～50mol％，B
2O
3：12～30mol％，SiO
2：30～50mol％，ZnO：0～2mol％，P
2O
5：0～2mol％，ZrO
2：0～2mol％，TiO
2：0～2mol％。
3. electric substrate as claimed in claim 2 is characterized in that with the preparation method of microcrystal glass material described predetermined formulation means the composition of raw materials according to following component conversion:
CaO：47mol％，B
2O
3：13mol％，SiO
2：39mol％，ZrO
2：1mol％。
4. electric substrate as claimed in claim 2 is characterized in that with the preparation method of microcrystal glass material described predetermined formulation means the composition of raw materials according to following component conversion:
CaO：47mol％，B
2O
3：12mol％，SiO
2：39mol％，TiO
2：2mol％。
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|---|---|---|---|
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Family
ID=44516885
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| CN103395994A (en) * | 2013-07-29 | 2013-11-20 | 云南云天化股份有限公司 | Low-temperature co-fired ceramic material and preparation method thereof |
| CN104003731A (en) * | 2014-06-09 | 2014-08-27 | 云南云天化股份有限公司 | Dielectric paste for thick-film process and preparation method thereof |
| CN106007387A (en) * | 2016-07-05 | 2016-10-12 | 电子科技大学 | Low-thermal-expansion high-strength glass-ceramic material and preparation method thereof |
| CN106187141A (en) * | 2016-07-12 | 2016-12-07 | 深圳顺络电子股份有限公司 | A kind of CBS system LTCC material and preparation method thereof |
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| CN101973709A (en) * | 2010-10-28 | 2011-02-16 | 南昌航空大学 | Method for preparing calcium aluminosilicate nanometer microcrystal glass by utilizing natrium silica calcium glass waste slag |
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| CN101973709A (en) * | 2010-10-28 | 2011-02-16 | 南昌航空大学 | Method for preparing calcium aluminosilicate nanometer microcrystal glass by utilizing natrium silica calcium glass waste slag |
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| CN103395994B (en) * | 2013-07-29 | 2015-11-25 | 云南云天化股份有限公司 | A kind of low-temperature co-burning ceramic material and preparation method thereof |
| CN104003731A (en) * | 2014-06-09 | 2014-08-27 | 云南云天化股份有限公司 | Dielectric paste for thick-film process and preparation method thereof |
| CN106007387A (en) * | 2016-07-05 | 2016-10-12 | 电子科技大学 | Low-thermal-expansion high-strength glass-ceramic material and preparation method thereof |
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| US10160689B2 (en) | 2016-07-12 | 2018-12-25 | Shenzhen Sunlord Electronics Co., Ltd. | CBS-based LTCC material and preparation method thereof |
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| CN110372217A (en) * | 2018-04-13 | 2019-10-25 | 上海晶材新材料科技有限公司 | A kind of low-temperature co-burning ceramic material and preparation method thereof |
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| CN112062473A (en) * | 2020-07-28 | 2020-12-11 | 电子科技大学 | High-strength mullite-based microcrystalline glass material and preparation method thereof |
| CN112062473B (en) * | 2020-07-28 | 2021-10-26 | 电子科技大学 | High-strength mullite-based microcrystalline glass material and preparation method thereof |
| CN115210195A (en) * | 2020-09-14 | 2022-10-18 | 冈本硝子株式会社 | Composition for low-temperature co-fired substrate |
| CN115210195B (en) * | 2020-09-14 | 2023-03-21 | 冈本硝子株式会社 | Composition for low-temperature co-fired substrate |
| CN114671614A (en) * | 2022-04-14 | 2022-06-28 | 电子科技大学 | Low-dielectric low-calcium low-loss aluminum boron silicon-based microcrystalline glass material and preparation method thereof |
| CN114671614B (en) * | 2022-04-14 | 2022-11-18 | 电子科技大学 | Low-dielectric low-loss calcium-boron-silicon-based microcrystalline glass material and preparation method thereof |
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Application publication date: 20110907 |