CN102173587A - Microcrystalline glass material for electronic substrate and preparation method thereof - Google Patents
Microcrystalline glass 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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- 239000011521 glass Substances 0.000 title claims abstract description 88
- 239000000463 material Substances 0.000 title claims abstract description 28
- 239000000758 substrate Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 19
- 238000005245 sintering Methods 0.000 claims description 19
- 239000006063 cullet Substances 0.000 claims description 17
- 239000013081 microcrystal Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 11
- 229910052796 boron Inorganic materials 0.000 claims description 10
- 230000004927 fusion Effects 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000009472 formulation Methods 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 239000006004 Quartz sand Substances 0.000 claims description 2
- 238000005352 clarification Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000012776 electronic material Substances 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- 238000002156 mixing Methods 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000005469 granulation Methods 0.000 description 6
- 230000003179 granulation Effects 0.000 description 6
- 238000012856 packing Methods 0.000 description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 description 6
- 238000003825 pressing Methods 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- 239000002241 glass-ceramic Substances 0.000 description 5
- 239000003989 dielectric material Substances 0.000 description 3
- 239000006112 glass ceramic composition Substances 0.000 description 3
- 230000008054 signal transmission Effects 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000004455 differential thermal analysis Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
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Abstract
A microcrystalline glass material for a circuit substrate and a preparation method thereof relate to the electronic material technology. The microcrystalline glass material comprises the following components: CaO: 33 to 50 mol%, B2O3:12~30mol%,SiO2:30~50mol%,ZnO:0~2mol%,P2O5:0~2mol%,ZrO2:0~2mol%,TiO2: 0 to 2 mol%. The microcrystalline glass prepared by the invention has low dielectric constant (epsilon is 6.5-7.2, 1MHz) and dielectric loss (tg delta 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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