CN102173755A - Low-temperature co-fired ceramic material, raw materials and preparation process thereof - Google Patents
Low-temperature co-fired ceramic material, raw materials and preparation process thereof Download PDFInfo
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Abstract
The invention discloses a low-temperature co-fired ceramic material which has low manufacturing cost, high contraction consistency, and is very suitable for low temperature co-fired ceramic (LTCC) curtain coating process production and in which glass is not needed to be founded, and raw materials and a preparation method thereof. The low-temperature co-fired ceramic material is a mixed presintered body which comprises 30 to 55 weight parts of Al2O3, 30 to 55 weight parts of powder a and 5 to 20 weight parts of powder b; the powder a is the presintered body which comprises 10 to 25 weight parts of CaO, 1 to 4 weight parts of MgO, 1 to 5 weight parts of LiO2, 40 to 60 weight parts of SiO2, and 10 to 30 weight parts of B2O3; and the powder b is the presintered body which comprises ZnO and SiO2 in a molar ratio of 2 to 1.
Description
Technical field
The present invention relates to field of electronic materials, relate in particular to a kind of low-temperature co-burning ceramic material and raw material thereof and preparation technology.
Background technology
LTCC (low temperature co-fired ceramics, write a Chinese character in simplified form LTCC) be the type material technology of nineteen eighty-two Hughes Electronics's exploitation, be that low temperature co-fired structural ceramics powder is made the accurate and fine and close green band of thickness, on the green band, utilize laser boring, micropore slip casting, technologies such as accurate conductor paste printing are made the circuitry needed figure, and with a plurality of passive blocks (as low appearance value electric capacity, resistance, wave filter, impedance transducer, coupling mechanism etc.) imbed in the multilayer ceramic substrate, overlap together then, internal and external electrode can use silver respectively, copper, metals such as gold, at 900 ℃ of following sintering, make the non-interfering high-density circuit of three-dimensional space, also can be made into the three-dimensional circuit substrate of built-in passive element, can mount IC and active part on its surface, make passive/active integrated functional module, can be particularly suitable for high frequency communication assembly further with circuit miniaturization and densification.
The low-temperature co-fired ceramic medium baseplate material of current use mainly contains following two classes:
1, stupalith is a matrix, by adding sintering aid (supporting fusing point oxide compound or low melting glass), the sintering temperature of stupalith is reduced to below 900 ℃, the low-temperature sintering dielectric material that electric property is had relatively high expectations generally is to adopt this mode to prepare stupalith, as laminated medium electric capacity, laminated medium antenna and filter in laminated medium etc.;
2, be matrix with the glass composition, earlier with glass melting, pulverize after quenching, form devitrified glass by crystallization in the sintering process at last, part Study person also adds pottery as machinery and the electric property of weighting agent to improve material before sintering, this material is mainly used in to the less demanding low-temperature sintering medium substrate of electric property, as the high frequency laminated inductance.
In these " glass+ceramic stopping composition " compound systems and " pottery+glass " system, also there is very big deficiency: 1. production cost height, owing to need high temperature melting glass, heat treatment time is long, power consumption is big, vaporization at high temperature causes prescription to change, this has all caused the manufacturing process complexity, and is not suitable for producing in enormous quantities; 2. to the equipment requirements height, behind the glass melting, it is big to equipment loss to quench; 3. the glass slag hardness height after quenching is difficult to levigately, not only increased manufacturing cost, and glass shape is poor, and Technological adaptability is bad.
Summary of the invention
The technical problem that the present invention mainly solves provides a kind of low-temperature co-burning ceramic material and raw material and preparation technology without fusion cast glass, low cost of manufacture, contraction high conformity, very suitable LTCC casting technique production.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of low-temperature co-burning ceramic material is provided, and described low-temperature co-burning ceramic material is the Al of 30～55 weight parts
2O
3, 30～55 weight parts powder a and 5～20 weight parts powder b mix the pre-burning body;
Described powder a is the pre-burning body, and its component is:
The CaO of 10～25 weight parts,
The MgO of 1～4 weight part,
The Li of 1～5 weight part
2O,
The SiO of 40～60 weight parts
2,
The B of 10～30 weight parts
2O
3
Described powder b is the pre-burning body, and its component is that mol ratio is 2: 1 ZnO and SiO
2
The present invention is with respect to prior art, and its beneficial effect is as follows:
1) the present invention is by regulating Al
2O
3, CaO, MgO, Li
2O, ZnO, SiO
2And B
2O
3Composition, the sintering temperature of material is controlled at below 900 ℃.
2) material of the present invention can make with Ag, Ag/Pd, Cu electrode matching co-firing, and (ε=5-8,1MHz), low-loss (D≤0.002) is applicable to lamination components and parts, medium substrate and semi-conductor and microelectronic packaging material field to have low specific inductivity.
3) material of the present invention is a kind of without fusion cast glass, and manufacture craft is simple, and cost is low, and high conformity is shunk in energy-conserving and environment-protective, is fit to very much the production of LTCC casting technique.
For realizing second goal of the invention, the invention provides a kind of low-temperature co-burning ceramic material preparation raw material, the described low-temperature co-burning ceramic material preparation Al of raw material by 30～55 weight parts
2O
3, the powder a of 30～55 weight parts and the powder b of 5～20 weight parts mix;
Described powder a is the pre-burning body, and its component is:
The CaO of 10～25 weight parts,
The MgO of 1～4 weight part,
The Li of 1～5 weight part
2O,
The SiO of 40～60 weight parts
2,
The B of 10～30 weight parts
2O
3
Described powder b is the pre-burning body, and its component is that mol ratio is 2: 1 ZnO and SiO
2
Use this raw material can under the sintering temperature below 900 ℃, make as the present invention above-mentioned low-temperature co-burning ceramic material.
The present invention also provides a kind of low-temperature co-burning ceramic material preparation raw material, and described low-temperature co-burning ceramic material preparation is the pre-burning body with raw material, and its component is:
The CaO of 10～25 weight parts,
The MgO of 1～4 weight part,
The Li of 1～5 weight part
2O,
The SiO of 40～60 weight parts
2,
The B of 10～30 weight parts
2O
3
The present invention provides a kind of low-temperature co-burning ceramic material preparation raw material again, and described low-temperature co-burning ceramic material preparation is the pre-burning body with raw material, and its component is that mol ratio is 2: 1 ZnO and SiO
2
Above-mentioned two kinds of material-mix aluminum oxide use, and can make as the present invention above-mentioned low-temperature co-burning ceramic material under the sintering temperature below 900 ℃.
For reaching the 3rd goal of the invention, the invention provides the preparation technology of a kind of low-temperature co-burning ceramic material preparation with raw material, may further comprise the steps:
Step 1: preparation powder a and powder b
The preparation of powder a may further comprise the steps:
A1: take by weighing the CaO of 10～25 weight parts, the MgO of 1～4 weight part is converted into 1～5 weight part Li
2The Li of O
2CO
3, the SiO of 40～60 weight parts
2Be converted into 10～30 weight part B
2O
3H
3BO
3, be processed into less than 20 purpose mixed powders;
A2: the calcining under 500～800 ℃ of step a1 gained mixed powder is obtained powder a;
The preparation of powder b may further comprise the steps;
B1: took by weighing ZnO and SiO in 2: 1 in molar ratio
2Be processed into less than 20 purpose mixed powders;
B2: the calcining under 1000～1100 ℃ of step b1 gained mixed powder is obtained powder b;
The Al of step 2:30～55 weight parts
2O
3, the powder a of 30～55 weight parts and the powder b of 5～20 weight parts mix, and obtains low-temperature co-burning ceramic material.
Technology of the present invention is applicable to and Ag, Ag/Pd, Cu electrode matching co-firing, and (ε=5-8,1MHz), low-loss (D≤0.002) is applicable to lamination components and parts, medium substrate and semi-conductor and microelectronic packaging material field to have low specific inductivity.
And technology of the present invention is a kind of without fusion cast glass, and manufacture craft is simple, and cost is low, and high conformity is shunk in energy-conserving and environment-protective, is fit to very much the material preparation process that the LTCC casting technique is produced.
Wherein, be processed among step a1, the b1 20 purpose mixed powders can for: dry after starting material and deionized water placed the ball mill ball milling, cross 20 mesh sieves then.
In the step 2 with Al
2O
3, powder a and powder b mix and be specially: with Al
2O
3, powder a and powder b dry after placing the ball mill Ball milling together with deionized water.
Wherein, aluminum oxide, powder a, b mixing granulation, moulding with in the present invention and the improvement technology thereof place 900 ℃ sintering temperature then, obtain described low-temperature co-burning ceramic material.
Wherein, sintering process can for: the temperature rise rate with 5 ℃/min is warmed up to 550 ℃, insulation 30min, the temperature rise rate with 2.5 ℃/min is warmed up to 870～900 ℃ then, and is incubated 2～4 hours, adopts air atmosphere, cools to room temperature with the furnace.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, realized purpose and effect, give explanation below in conjunction with embodiment is detailed.
Embodiment 1:
1, CaO 25%, MgO 4%, SiO by weight percentage
240%, B
2O
3(with H
3BO
3Form is introduced) 30%, Li
2O is (with Li
2CO
3The form introducing) powder of 1% weighing gross weight 100Kg, together with deionized water 200Kg, mixing and ball milling 24 ± 4hr obtains powder again after dry down in 150 ± 5 ℃, crossing 20 mesh sieves;
2, step (1) gained powder is promptly got powder a at 500 ± 50 ℃ of temperature lower calcination 2 ± 1hr;
3, ZnO: SiO in molar ratio
2Prepare powder 100Kg at=2: 1, and together with deionized water 200Kg, mixing and ball milling 24 ± 4hr obtains powder again after dry down in 150 ± 5 ℃, crossing 20 mesh sieves;
4, step (3) gained powder is promptly being got powder b at 1050 ± 50 ℃ of temperature lower calcination 2 ± 1hr;
5, powder a 30%, powder b 15%, Al by weight percentage
2O
355% weighing gross weight 100Kg powder together with deionized water 80Kg, is put into ball mill and is disperseed 30 ± 4hr, then through promptly getting described LTCC medium substrate material preparation raw material in 150 ± 5 ℃ of oven dry;
6, get step (5) LTCC medium substrate material preparation raw material, the polyvinyl alcohol solution that adds massfraction 5% is made binding agent, granulation;
7, moulding.Green compact diameter 14.2mm, height 3～4mm, pressure is 1 ton, pressurize 10 seconds;
8, sintering adopts the normal sintering method, is warmed up to 550 ℃ with 5 ℃/min, and insulation 30min is warmed up to 870～900 ℃ with 2.5 ℃/min then, and is incubated 2～4 hours, adopts air atmosphere, cools to room temperature with the furnace;
9, use the miking radial shrinkage ratio, the drainage measuring density adopts TH2828 impedance instrument Measuring Dielectric Constant and dielectric loss, and performance sees Table 1
Table 1
Embodiment two
1, CaO 20%, MgO 3%, SiO by weight percentage
250%, B
2O
3(with H
3BO
3Form is introduced) 25%, Li
2O is (with Li
2CO
3The form introducing) powder of 2% weighing gross weight 100Kg, together with deionized water 200Kg, mixing and ball milling 24 ± 4hr obtains powder again after dry down in 150 ± 5 ℃, crossing 20 mesh sieves;
2, step (1) gained powder is promptly got powder a at 600 ± 50 ℃ of temperature lower calcination 2 ± 1hr;
3, ZnO: SiO in molar ratio
2Prepare powder 100Kg at=2: 1, and together with deionized water 200Kg, mixing and ball milling 24 ± 4hr obtains powder again after dry down in 150 ± 5 ℃, crossing 20 mesh sieves;
4, step (3) gained powder is promptly being got powder b at 1050 ± 50 ℃ of temperature lower calcination 2 ± 1hr;
5, powder a 55%, powder b 15%, Al by weight percentage
2O
330% weighing gross weight 100Kg powder together with deionized water 80Kg, is put into ball mill and is disperseed 30 ± 4hr, then through promptly getting described LTCC medium substrate material preparation raw material in 150 ± 5 ℃ of oven dry;
6, get step (5) LTCC medium substrate material preparation raw material, the polyvinyl alcohol solution that adds massfraction 5% is made binding agent, granulation;
7, moulding.Green compact diameter 14.2mm, height 3～4mm, pressure is 1 ton, pressurize 10 seconds;
8, sintering adopts the normal sintering method, is warmed up to 550 ℃ with 5 ℃/min, and insulation 30min is warmed up to 870～900 ℃ with 2.5 ℃/min then, and is incubated 2-4 hour, adopts air atmosphere, cools to room temperature with the furnace;
9, use the miking radial shrinkage ratio, the drainage measuring density adopts TH2828 impedance instrument Measuring Dielectric Constant and dielectric loss, and performance sees Table 2
Table 2
Embodiment three
1, CaO 25%, MgO 2%, SiO by weight percentage
260%, B
2O
3(with H
3BO
3Form is introduced) 10%, Li
2O is (with Li
2CO
3The form introducing) powder of 3% weighing gross weight 100Kg, together with deionized water 200Kg, mixing and ball milling 24 ± 4hr obtains powder again after dry down in 150 ± 5 ℃, crossing 20 mesh sieves;
2, step (1) gained powder is promptly got powder a at 800 ± 50 ℃ of temperature lower calcination 2 ± 1hr;
3, ZnO: SiO in molar ratio
2Prepare powder 100Kg at=2: 1, and together with deionized water 200Kg, mixing and ball milling 24 ± 4hr obtains powder again after dry down in 150 ± 5 ℃, crossing 20 mesh sieves;
4, step (3) gained powder is promptly being got powder b at 1050 ± 50 ℃ of temperature lower calcination 2 ± 1hr;
5, powder a 45%, powder b 5%, Al by weight percentage
2O
350% weighing gross weight 100Kg powder together with deionized water 80Kg, is put into ball mill and is disperseed 30 ± 4hr, then through promptly getting described LTCC medium substrate material preparation raw material in 150 ± 5 ℃ of oven dry;
6, get step (5) LTCC medium substrate material preparation raw material, the polyvinyl alcohol solution that adds massfraction 5% is made binding agent, granulation;
7, moulding.Green compact diameter 14.2mm, height 3～4mm, pressure is 1 ton, pressurize 10 seconds;
8, sintering adopts the normal sintering method, is warmed up to 550 ℃ with 5 ℃/min, and insulation 30min is warmed up to 870～900 ℃ with 2.5 ℃/min then, and is incubated 2-4 hour, adopts air atmosphere, cools to room temperature with the furnace;
9, use the miking radial shrinkage ratio, the drainage measuring density adopts TH2828 impedance instrument Measuring Dielectric Constant and dielectric loss, and performance sees Table 3
Table 3
Embodiment four
1, CaO 10%, MgO 1%, SiO by weight percentage
260%, B
2O
3(with H
3BO
3Form is introduced) 24%, Li
2O is (with Li
2CO
3The form introducing) powder of 5% weighing gross weight 100Kg, together with deionized water 200Kg, mixing and ball milling 24 ± 4hr obtains powder again after dry down in 150 ± 5 ℃, crossing 20 mesh sieves;
2, step (1) gained powder is promptly got powder a at 700 ± 50 ℃ of temperature lower calcination 2 ± 1hr;
3, ZnO: SiO in molar ratio
2Prepare powder 100Kg at=2: 1, and together with deionized water 200Kg, mixing and ball milling 24 ± 4hr obtains powder again after dry down in 150 ± 5 ℃, crossing 20 mesh sieves;
4, step (3) gained powder is promptly being got powder b at 1050 ± 50 ℃ of temperature lower calcination 2 ± 1hr;
5, powder a 40%, powder b 20%, Al by weight percentage
2O
340% weighing gross weight 100Kg powder together with deionized water 80Kg, is put into ball mill and is disperseed 30 ± 4hr, then through promptly getting described LTCC medium substrate material preparation raw material in 150 ± 5 ℃ of oven dry;
6, get step (5) LTCC medium substrate material preparation raw material, the polyvinyl alcohol solution that adds massfraction 5% is made binding agent, granulation;
7, moulding.Green compact diameter 14.2mm, height 3～4mm, pressure is 1 ton, pressurize 10 seconds;
8, sintering adopts the normal sintering method, is warmed up to 550 ℃ with 5 ℃/min, and insulation 30min is warmed up to 870～900 ℃ with 2.5 ℃/min then, and is incubated 2-4 hour, adopts air atmosphere, cools to room temperature with the furnace;
9, use the miking radial shrinkage ratio, the drainage measuring density adopts TH2828 impedance instrument Measuring Dielectric Constant and dielectric loss, and performance sees Table 4
Table 4
The above only is embodiments of the invention; be not so limit claim of the present invention; every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (8)
1. a low-temperature co-burning ceramic material is characterized in that, described low-temperature co-burning ceramic material is the Al of 30～55 weight parts
2O
3, 30～55 weight parts powder a and 5～20 weight parts powder b mix the pre-burning body;
Described powder a is the pre-burning body, and its component is:
The CaO of 10～25 weight parts,
The MgO of 1～4 weight part,
The Li of 1～5 weight part
2O,
The SiO of 40～60 weight parts
2,
The B of 10～30 weight parts
2O
3
Described powder b is the pre-burning body, and its component is that mol ratio is 2: 1 ZnO and SiO
2
2. raw material is used in a low-temperature co-burning ceramic material preparation, it is characterized in that, the described low-temperature co-burning ceramic material preparation Al of raw material by 30～55 weight parts
2O
3, the powder a of 30～55 weight parts and the powder b of 5～20 weight parts mix;
Described powder a is the pre-burning body, and its component is:
The CaO of 10～25 weight parts,
The MgO of 1～4 weight part,
The Li of 1～5 weight part
2O,
The SiO of 40～60 weight parts
2,
The B of 10～30 weight parts
2O
3
Described powder b is the pre-burning body, and its component is that mol ratio is 2: 1 ZnO and SiO
2
3. raw material is used in a low-temperature co-burning ceramic material preparation, it is characterized in that, described low-temperature co-burning ceramic material preparation is the pre-burning body with raw material, and its component is:
The CaO of 10～25 weight parts,
The MgO of 1～4 weight part,
The Li of 1～5 weight part
2O,
The SiO of 40～60 weight parts
2,
The B of 10～30 weight parts
2O
3
4. raw material is used in a low-temperature co-burning ceramic material preparation, it is characterized in that, described low-temperature co-burning ceramic material preparation is the pre-burning body with raw material, and its component is that mol ratio is 2: 1 ZnO and SiO
2
5. a low-temperature co-burning ceramic material prepares the preparation technology who uses raw material, it is characterized in that, may further comprise the steps:
Step 1: preparation powder a and powder b
The preparation of powder a may further comprise the steps:
A1: take by weighing the CaO of 10～25 weight parts, the MgO of 1～4 weight part is converted into 1～5 weight part Li
2The Li of O
2CO
3, the SiO of 40～60 weight parts
2Be converted into 10～30 weight part B
2O
3H
3BO
3, be processed into less than 20 purpose mixed powders;
A2: the calcining under 500～800 ℃ of step a1 gained mixed powder is obtained powder a;
The preparation of powder b may further comprise the steps;
B1: took by weighing ZnO and SiO in 2: 1 in molar ratio
2Be processed into less than 20 purpose mixed powders;
B2: the calcining under 1000～1100 ℃ of step b1 gained mixed powder is obtained powder b;
The Al of step 2:30～55 weight parts
2O
3, the powder a of 30～55 weight parts and the powder b of 5～20 weight parts mix, and obtains low-temperature co-burning ceramic material preparation raw material.
6. the low-temperature co-burning ceramic material preparation according to claim 5 preparation technology of raw material, it is characterized in that, being processed into 20 purpose mixed powders among step a1, the b1 is specially: dry after starting material and deionized water are placed the ball mill ball milling, cross 20 mesh sieves then.
In the step 2 with Al
2O
3, powder a and powder b mix and be specially: with Al
2O
3, powder a and powder b dry after placing the ball mill Ball milling together with deionized water.
7. the preparation technology of a low-temperature co-burning ceramic material is characterized in that, claim 5 or the preparation of 6 gained low-temperature co-burning ceramic materials are used the raw material granulation, and moulding places 900 ℃ sintering temperature then, obtains described low-temperature co-burning ceramic material.
8. the preparation technology of low-temperature co-burning ceramic material according to claim 7, it is characterized in that, sintering process is specially: the temperature rise rate with 5 ℃/min is warmed up to 550 ℃, insulation 30min, temperature rise rate with 2.5 ℃/min is warmed up to 870～900 ℃ then, and be incubated 2～4 hours, and adopt air atmosphere, cool to room temperature with the furnace.
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| CN102503137A (en) * | 2011-10-13 | 2012-06-20 | 天津大学 | Calcium-aluminum-boron-silicon glass and fused quartz low-temperature co-fired ceramic material and preparation method thereof |
| CN102863221A (en) * | 2012-09-20 | 2013-01-09 | 广东风华高新科技股份有限公司 | Method, sintering aid and materials for preparation of low-temperature cofired medium ceramic and application |
| CN102898145A (en) * | 2012-10-09 | 2013-01-30 | 天津大学 | Li2O-Al2O3-SiO2-B2O3, CaO-Al2O3-SiO2-B2O3 crystallizable glass low-temperature co-fired composite material and preparation method thereof |
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| CN112592160B (en) * | 2020-12-23 | 2022-05-24 | 嘉兴佳利电子有限公司 | Complex-phase low-temperature co-fired ceramic material and preparation method thereof |
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| CN115894002B (en) * | 2022-12-06 | 2023-09-22 | 中国科学院合肥物质科学研究院 | Diphase ceramic reinforced low-temperature cofiring ceramic material and preparation method and application thereof |
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