CN111470778A - Calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material and preparation method thereof - Google Patents
Calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/04—Particles; Flakes
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/30—Methods of making the composites
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Abstract
The invention discloses a low-dielectric and low-temperature co-fired ceramic material based on calcium barium silicon aluminum glass and a preparation method thereof, wherein the low-temperature co-fired ceramic material is prepared from CaO-BaO-SiO2‑Al2O3The glass comprises system glass, silicon dioxide and zirconium dioxide, wherein the mass fraction of the CBSA glass is 51-58%, the mass fraction of the silicon dioxide is 28-32%, and the mass fraction of the zirconium dioxide is 13-17%. Compared with the existing material, the raw material adopted by the invention has low cost, is lead-free and nontoxic, can be sintered and compacted at 820-880 ℃, has a wider sintering temperature zone, a dielectric constant of 7.8-8.5 and a dielectric loss of 2.5 x 10‑3~3.5*10‑3Co-firing the green ceramic tape produced by casting process with gold and silver electrodesThe matching performance is good, the process operability is strong, and batch production can be realized.
Description
Technical Field
The invention relates to the technical field of low-temperature co-fired ceramics, in particular to a calcium barium silicon aluminum glass-based low-temperature co-fired ceramic material and a preparation method thereof. .
Background
Nowadays, in large-scale ultra-high speed integrated circuits, in order to reduce signal delay time, a substrate material is required to have a low dielectric constant, so that signal transmission speed can be improved. Based on these aspects, low-temperature co-fired ceramic materials with dielectric constants lower than 10 are the focus of domestic and foreign research.
The dielectric constant of the calcium barium silicon aluminum glass is about 10, the melting point of the calcium barium silicon aluminum glass is about 700 ℃, the sintering temperature of the common low-temperature co-fired ceramic material is 800-900 ℃, in order to increase the sintering temperature, one or more ceramics with lower dielectric constant and higher melting point can be added to be matched with the calcium barium silicon aluminum glass, and the low-temperature co-fired ceramic material with the dielectric constant lower than 10 can be prepared.
Disclosure of Invention
The significance of the invention is that from the practical point of view of low-temperature co-fired ceramic (L TCC), CaO-BaO-SiO with low melting point is adopted2-Al2O3The system glass (CBSA glass) is compounded with silicon dioxide and zirconium oxide to prepare a low-temperature co-fired ceramic material which can be sintered and compacted at 820-880 ℃, and the preparation method of the calcium barium silicon aluminum glass-based low-temperature co-fired ceramic material is provided.
In view of the above, the present invention provides a low temperature co-fired ceramic material, which comprises the following components:
CaO-BaO-SiO with low melting point2-Al2O3The mass fraction (wt%) of the system glass (CBSA glass) is 50-60%, the mass fraction (wt%) of the high-melting-point ceramic material silicon dioxide is 25-35%, and the mass fraction (wt%) of the zirconium oxide is 10-20%.
Further, the CaO-BaO-SiO2-Al2O3The system glass is made of CaO, BaO and SiO2、Al2O3And (4) forming.
The mass percentage of each oxide is respectively as follows:
CaO 32%~36%
SiO223%~27%
Al2O325%~30%
BaO 12%~15%
the calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material is sintered in air atmosphere and has the following preparation steps:
weighing raw materials according to the mass percent of each oxide in the CBSA glass formula, ball-milling and mixing the raw materials with alcohol, drying and sieving the mixture, melting the mixed powder into glass liquid in a high-temperature furnace, quenching the glass liquid with water, cooling and forming the glass liquid, and ball-milling and crushing glass blocks with alcohol into glass powder to obtain CaO-BaO-SiO2-Al2O3And (5) system glass powder.
And (3) ball-milling, mixing and drying the CBSA glass powder obtained in the step with silicon dioxide ceramic powder and zirconium oxide ceramic powder by alcohol to obtain the calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material.
Preferably, in the low-temperature co-fired ceramic material, CaO-BaO-SiO with low melting point2-Al2O3The mass fraction of the system glass (CBSA glass) is 51-58%, the mass fraction of the high-melting-point ceramic material silicon dioxide is 28-32%, and the mass fraction of the zirconium oxide is 13-17%.
Preferably, the CaO-BaO-SiO2-Al2O3Sintering the system glass at 1370-1430 ℃ for 2-4 hours, and performing water quenching forming.
Preferably, the particle size of the silica ceramic powder and the zirconia ceramic powder needs to be controlled, and the specific method is that water is used as a ball milling medium in an alumina ceramic tank, and the ball milling is carried out in a planetary way until the particle size is 4-6 mu m.
The invention has the advantages that the invention adopts the nontoxic and harmless CaO-BaO-SiO2-Al2O3The system glass is compounded with the ceramic, can be sintered and compacted at 820-880 ℃, has a wider sintering temperature zone, a dielectric constant of 7.8-8.5 and a dielectric loss of 2.5 x 10-3~3.5*10-3The green ceramic tape manufactured by the casting process has good co-firing matching with gold and silver electrodes and strong process operability, and can realize batch production.
Drawings
FIG. 1 is an SEM image of a sintered cross-section of a low-temperature co-fired ceramic material according to an embodiment of the invention;
FIG. 2 is an SEM image of a cross section of a low-temperature co-fired ceramic and a silver electrode after co-firing according to an embodiment of the invention.
Detailed description of the preferred embodiments
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The embodiment of the invention discloses a calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material which comprises the following components:
CaO-BaO-SiO with low melting point2-Al2O3The mass fraction of the system glass (CBSA glass) is 51-58%, the mass fraction of the high-melting-point ceramic material silicon dioxide is 28-32%, and the mass fraction of the zirconium oxide is 13-17%.
The low-melting-point glass comprises the following components: 32-36 wt% of CaO; 23wt% -27 wt% SiO2；25wt%~30wt% Al2O3；12wt%~15wt% BaO。
The invention also provides a preparation method of the low-temperature co-fired ceramic material, which comprises the following specific steps:
(1) weighing raw materials according to the mass percent of each oxide in the CBSA glass formula, ball-milling and mixing the raw materials with alcohol, drying and sieving the mixture, melting the mixed powder into glass liquid in a high-temperature furnace at 1370-1430 ℃, preserving the heat for 2-4 hours, quenching and cooling the glass liquid for forming, and then ball-milling and crushing glass blocks with alcohol into glass powder to obtain CaO-BaO-SiO2-Al2O3The granularity of the system glass powder D50 is controlled to be 3-4 mu m.
(2) The particle size of the silicon dioxide ceramic powder and the zirconium oxide ceramic powder needs to be controlled, and the specific method is that water is used as a ball milling medium in an aluminum oxide ceramic tank, planetary ball milling is carried out, and the particle size D50 is controlled to be 4-6 mu m.
(3) And (3) ball-milling, mixing and drying the CBSA glass powder obtained in the step with silicon dioxide ceramic powder and zirconium oxide ceramic powder by alcohol to obtain the calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material.
The low-temperature co-fired ceramic material can be sintered and compacted at 820-880 ℃, the sintering temperature zone is wider, the dielectric constant is 7.8-8.5, and the dielectric loss is 2.5 x 10-3~3.5*10-3The green ceramic tape manufactured by the casting process has good co-firing matching with gold and silver electrodes and strong process operability, and can realize batch production.
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Mixing CaCO346.5wt% and BaCO312.8wt%, SiO219.2wt% and Al2O3Sampling 21.5wt% of the mixed slurry according to a set proportion, putting the sampled mixed slurry into a planetary ball mill, carrying out alcohol ball milling for 1 hour, fully mixing the mixed slurry, drying the mixed slurry, and then putting the uniformly mixed powder into a platinum crucible;
placing the platinum crucible containing the mixture in a high-temperature furnace, rapidly heating to 1400 ℃, and then preserving heat for 3 hours to obtain high-temperature molten glass liquid;
pouring the obtained molten glass into deionized water for quenching to obtain glass fragments with uneven sizes, and then ball-milling the glass fragments into glass powder by alcohol to obtain CaO-BaO-SiO2-Al2O3The granularity of the system glass powder D50 is controlled to be 3-4 mu m.
Respectively putting ceramic powder silicon dioxide and zirconia in an alumina ceramic pot, taking water as a ball milling medium, carrying out planetary ball milling for 3 hours, and controlling the particle size D50 to be 4-6 mu m.
Mixing the CBSA glass powder obtained in the step with silicon dioxide ceramic powder and zirconium oxide ceramic powder according to the proportion shown in the table 1, carrying out alcohol ball milling for 2 hours, and drying the mixed slurry to obtain the calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material.
TABLE 1
| Components | CBSA glass powder | Silicon dioxide | Zirconium dioxide |
| Mass fraction | 53% | 30% | 17% |
Adding PVB with the mass fraction of 3% into the mixed powder as a binder for granulation, pressing the mixture into a cylindrical blank, discharging the binder at 450 ℃ for 1h, sintering the blank at 850 ℃ for 20min to obtain a sintered compact ceramic sample, and testing the microwave dielectric property, wherein the dielectric constant of the sample is 7.90 (@ 10.46 GHz) and the dielectric loss is 2.8 × 10-3。
Example 2
Mixing CaCO346.5wt% and BaCO312.8wt%, SiO219.2wt% and Al2O3Sampling 21.5wt% of the mixed slurry according to a set proportion, putting the sampled mixed slurry into a planetary ball mill, carrying out alcohol ball milling for 1 hour, fully mixing the mixed slurry, drying the mixed slurry, and then putting the uniformly mixed powder into a platinum crucible;
placing the platinum crucible containing the mixture in a high-temperature furnace, rapidly heating to 1400 ℃, and then preserving heat for 3 hours to obtain high-temperature molten glass liquid;
pouring the obtained molten glass into deionized water for quenching to obtain glass fragments with uneven sizes, and then ball-milling the glass fragments into glass powder by alcohol to obtain CaO-BaO-SiO2-Al2O3The granularity of the system glass powder D50 is controlled to be 3-4 mu m.
Respectively putting ceramic powder silicon dioxide and zirconia in an alumina ceramic pot, taking water as a ball milling medium, carrying out planetary ball milling for 3 hours, and controlling the particle size D50 to be 4-6 mu m.
Mixing the CBSA glass powder obtained in the step with silicon dioxide ceramic powder and zirconia ceramic powder according to the proportion shown in the table 2, carrying out alcohol ball milling for 2 hours, and drying the mixed slurry to obtain the calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material.
TABLE 2
| Components | CBSA glass powder | Silicon dioxide | Zirconium dioxide |
| Mass fraction | 56% | 27% | 17% |
Adding PVB with the mass fraction of 3% into the mixed powder as a binder for granulation, pressing the mixture into a cylindrical blank, discharging the binder at 450 ℃ for 1h, sintering the blank at 825 ℃ for 20min to obtain a sintered compact ceramic sample, and testing the microwave dielectric property, wherein the dielectric constant of the sample is 8.33(@ 11.02 GHz) and the dielectric loss is 3.25 × 10-3。
Example 3
Mixing CaCO346.5wt% and BaCO312.8wt%, SiO219.2wt% and Al2O3Sampling 21.5wt% of the mixed slurry according to a set proportion, putting the sampled mixed slurry into a planetary ball mill, carrying out alcohol ball milling for 1 hour, fully mixing the mixed slurry, drying the mixed slurry, and then putting the uniformly mixed powder into a platinum crucible;
placing the platinum crucible containing the mixture in a high-temperature furnace, rapidly heating to 1400 ℃, and then preserving heat for 3 hours to obtain high-temperature molten glass liquid;
pouring the obtained molten glass into deionized water for quenching to obtain glass fragments with uneven sizes, and then ball-milling the glass fragments into glass powder by alcohol to obtain CaO-BaO-SiO2-Al2O3The granularity of the system glass powder D50 is controlled to be 3-4 mu m.
Respectively putting ceramic powder silicon dioxide and zirconia in an alumina ceramic pot, taking water as a ball milling medium, carrying out planetary ball milling for 3 hours, and controlling the particle size D50 to be 4-6 mu m.
Mixing the CBSA glass powder obtained in the step with silicon dioxide ceramic powder and zirconia ceramic powder according to the proportion shown in the table 3, carrying out alcohol ball milling for 2 hours, and drying the mixed slurry to obtain the calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material.
TABLE 3
| Components | CBSA glass powder | Silicon dioxide | Zirconium dioxide |
| Mass fraction | 56% | 31% | 13% |
Adding PVB with the mass fraction of 3% into the mixed powder as a binder for granulation, pressing the mixture into a cylindrical blank, discharging the binder at 450 ℃ for 1h, sintering the blank at 825 ℃ for 20min to obtain a sintered compact ceramic sample, and testing the microwave dielectric property, wherein the dielectric constant of the sample is 8.02 (@ 10.18 GHz) and the dielectric loss is 3.01 × 10-3。
Example 4
Mixing CaCO346.5wt% and BaCO312.8wt%, SiO219.2wt% and Al2O3Sampling 21.5wt% according to a given proportion, putting the sample into a planetary ball mill, carrying out alcohol ball milling for 1 hour, fully mixing, drying the mixed slurry, and homogenizingThe uniformly mixed powder is placed in a platinum crucible;
placing the platinum crucible containing the mixture in a high-temperature furnace, rapidly heating to 1400 ℃, and then preserving heat for 3 hours to obtain high-temperature molten glass liquid;
pouring the obtained molten glass into deionized water for quenching to obtain glass fragments with uneven sizes, and then ball-milling the glass fragments into glass powder by alcohol to obtain CaO-BaO-SiO2-Al2O3The granularity of the system glass powder D50 is controlled to be 3-4 mu m.
Respectively putting ceramic powder silicon dioxide and zirconia in an alumina ceramic pot, taking water as a ball milling medium, carrying out planetary ball milling for 3 hours, and controlling the particle size D50 to be 4-6 mu m.
And (3) mixing the CBSA glass powder obtained in the step with silicon dioxide ceramic powder and zirconia ceramic powder according to the proportion shown in the table 4, carrying out alcohol ball milling for 2 hours, and drying the mixed slurry to obtain the calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material.
TABLE 4
| Components | CBSA glass powder | Silicon dioxide | Zirconium dioxide |
| Mass fraction | 51% | 32% | 17% |
Adding PVB with the mass fraction of 3% into the mixed powder as a binder for granulation and pressingForming a cylindrical blank, removing binder at 450 deg.C for 1h, sintering at 870 deg.C for 20min to obtain a sintered compact ceramic sample, and testing microwave dielectric properties with a dielectric constant of 8.47 (@ 10.58 GHz) and a dielectric loss of 2.97 × 10-3。
Claims (4)
1. A calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material comprises the following components:
51-58 wt% of CaO-BaO-SiO2-Al2O3The system glass comprises 28wt% to 32wt% of silicon dioxide and 13wt% to 17wt% of zirconium oxide.
2. The low dielectric and low temperature co-fired ceramic material of claim 1, wherein the CaO-BaO-SiO2-Al2O3The mass percentage of each oxide in the system glass is respectively as follows: 32% -36% of CaO; SiO2223%~27%；Al2O325%~30%；BaO 12%~15%。
3. A preparation method of a calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material comprises the following steps:
(1) CaO-BaO-SiO as claimed in claim 22-Al2O3Weighing raw materials according to mass percentage of each oxide in system glass, ball-milling and mixing the raw materials by alcohol, drying and sieving the mixture, melting mixed powder into glass liquid in a high-temperature furnace at 1370-1430 ℃, preserving heat for 2-4 hours, quenching and cooling the glass liquid for forming, and then ball-milling and crushing glass blocks into glass powder by alcohol to obtain CaO-BaO-SiO2-Al2O3The granularity D50 of the system glass powder is controlled to be between 3 and 4 mu m;
(2) the particle size of the silicon dioxide ceramic powder and the zirconium oxide ceramic powder needs to be controlled, and the specific method is that water is used as a ball milling medium in an aluminum oxide ceramic tank, planetary ball milling is carried out, and the particle size D50 is controlled to be 4-6 mu m;
(3) CaO-BaO-SiO obtained in the above step2-Al2O3System glass powder, silicon dioxide ceramic powder, zirconium oxide ceramic powder and alcohol ballGrinding, mixing and drying to obtain the calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic powder material.
4. The method for preparing the low-dielectric and low-temperature co-fired ceramic material with the calcium barium silicon aluminum glass base according to claim 3, wherein the ceramic material is CaO-BaO-SiO2-Al2O3The low-temperature co-fired ceramic material of the system glass powder can be sintered and compacted at 820-880 ℃, the dielectric constant is 7.8-8.5, and the dielectric loss is 2.5 x 10-3~ 3.5*10-3。
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| CN114477968A (en) * | 2022-03-09 | 2022-05-13 | 上海晶材新材料科技有限公司 | LTCC raw material belt material, LTCC substrate and preparation method |
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