CN103613369A - Silicate low-temperature co-fired ceramic substrate material and preparation method thereof - Google Patents
Silicate low-temperature co-fired ceramic substrate material and preparation method thereof Download PDFInfo
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- CN103613369A CN103613369A CN201310499020.3A CN201310499020A CN103613369A CN 103613369 A CN103613369 A CN 103613369A CN 201310499020 A CN201310499020 A CN 201310499020A CN 103613369 A CN103613369 A CN 103613369A
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Abstract
The invention discloses a silicate low-temperature co-fired ceramic substrate material and a preparation method thereof. The principal crystalline phase of the ceramic substrate material is Zn2SiO4, and the paracrystalline phase is CaTiO3. The dielectric constant [epsilon]r of the ceramic substrate material is 6.1-8.2, the quality factor Q*f is 9600-16000 GHz, and the resonance frequency temperature coefficient [Tau]f is -52 ppm/DEG C to 28 ppm/DEG C. The preparation method includes grinding the Zn2SiO4 and the CaTiO3 respectively into powder, mixing the CaTiO3 and the Zn2SiO4 with Bi2O3-CuO-B2O3 or Li2CO3-Bi2O3-CuO-B2O3 according to a ratio, adding absolute ethanol or deionized water, ball milling, drying, granulating, and sintering at 900-975 DEG C in a furnace. According to the preparation method, a product has the advantages of high purity, good quality, simple technology and low sintering temperature, and can be co-fired with Ag having high conductivity.
Description
Technical field
The present invention relates to a kind of ceramic substrate material and preparation method thereof, relate in particular to a kind of silicate low-temperature co-fired ceramic substrate material and preparation method thereof, belong to electronic substrate field.
Background technology
Low-temperature co-burning ceramic material is as the key foundation material in low temperature co-fired technology, and its performance requriements is more stricter than common microwave-medium ceramics, for example, mainly contain:
(1) there is good microwave dielectric property: there is the specific inductivity (2~2000) that can adapt to multi-purpose seriation, and as baseplate material, conventionally require material to there is low-k, the time of lag of propagating to shorten signal between chip; There is high quality factor, to guarantee good selecting frequency characteristic and to reduce the insertion loss under high frequency; There is nearly zero temperature coefficient of resonance frequency, to guarantee the thermostability of device.
(2) at process aspect, need lower sintering temperature, generally lower than 950 ℃, to realize low temperature co-fired with some electrode materialss.(Zeng Qun, Huo Liang, Zhou Yongheng, material Leader: a summary piece of writing, 2010,24(5)).
The people such as Yiping Guo in 2005 have just reported after 1350 ℃ of sintering of high temperature, Zn
2siO
4dielectric properties better, it can reach DIELECTRIC CONSTANT ε respectively
r=6.6, quality factor q * f=219,000GHz, temperature coefficient of resonance frequency τ
f=-61ppm/ ℃, and utilize the TiO with larger forward temperature coefficient of resonance frequency
2to Zn
2siO
4τ
fregulate, and finally τ
fvalue is successfully adjusted to zero.
But the sintering temperature of its matrix material is still very high, up to 1,250 ℃.(Y.Guo,H.Ohsato,et?al.Characterization?and?dielectric?behavior?of?willemite?and?TiO2-doped?willemite?ceramics?at?millimeter-wave?frequency.J.Eur.Ceram.Soc.,2006,26:1827-1830.)
Because the stupalith system being applied in LTCC technology is wanted built-in metal electrode, therefore stupalith system and metal electrode material must have good chemical compatibility between the two, take Ag electrode as example, its fusing point is 961 ℃, this just requires the optimal sintering temperature of LTCC stupalith lower than this fusing point, and can in its sintering range, burn altogether with Ag.
The people such as Kim pass through to Zn
2siO
4the middle V with low melting point that adds respectively
2o
5and B
2o
3, successfully ceramic sintering temperature is reduced to 875 ℃ and 900 ℃.
But the temperature coefficient of resonance frequency of prepared stupalith and 0 deviation are larger, be respectively-28ppm/ ℃ and-21.9ppm/ ℃.Therefore, prepared stupalith cannot guarantee high stability and the high reliability of device, can not meet the dielectric properties requirement of high-frequency high-speed circuit to baseplate material.(J.S.Kim,M.E.Song,et?al.Effect?of?B
2O
3addition?on?the?sintering?temperature?and?microwave?dielectric?properties?of?Zn
2SiO
4ceramics.J.Eur.Ceram.Soc.,2010,30:375-379.;J.S.Kim,M.E.Song,et?al.Low-Temperature?Sintering?and?Microwave?Dielectric?Properties?of?V
2O
5-Added?Zn
2SiO
4Ceramics.J.Am.Ceram.Soc.,2008,91(12):4133-4136)。
Summary of the invention
One of object of the present invention is, a kind of baseplate material of LTCC is provided, and this baseplate material can meet the dielectric properties requirement of high-frequency high-speed circuit to baseplate material, and its sintering temperature is low, have the features such as microwave dielectric property is good.
The technical scheme that the present invention adopts is for achieving the above object, a kind of low-temperature co-fired ceramic substrate material, is characterized in that, principal crystalline phase is Zn
2siO
4, paracrystalline phase is CaTiO
3, DIELECTRIC CONSTANT ε
r=6.1~8.2, quality factor q * f=9600~16000GHz, temperature coefficient of resonance frequency τ
f=-52~28ppm/ ℃.
The technique effect of technique scheme is that this low-temperature co-fired ceramic substrate material can meet the dielectric properties requirement of high-frequency high-speed circuit to baseplate material.
As preferably, above-mentioned low-temperature co-fired ceramic substrate material, is characterized in that, by zinc silicate Zn
2siO
4powder, calcium titanate CaTiO
3powder, Bi
2o
3-CuO-B
2o
3or Li
2cO
3-Bi
2o
3-CuO-B
2o
3powder powder adds in proportion, mixes, at 900~975 ℃, sintering forms, wherein:
Described CaTiO
3the add-on of powder accounts for CaTiO
3powder and Zn
2siO
4the molar percentage of both total amounts of powder is 3.0~10.0mol%;
Described Bi
2o
3-CuO-B
2o
3or Li
2cO
3-Bi
2o
3-CuO-B
2o
3the add-on of powder accounts for 5.0~10.0wt% of ceramic total mass.
The technique effect that above-mentioned optimal technical scheme produces is that sintering temperature is low, and can burn altogether with the Ag of high conductivity.
Can also be preferably, above-mentioned Zn
2siO
4powder is with SiO
2with ZnO be raw material, through 1100~1300 ℃ of calcinings, make; Described CaTiO
3powder is with CaCO
3and TiO
2for raw material, through 1000~1200 ℃ of calcinings, make.
The technique effect that adopts above-mentioned optimization technique to produce is, technique is simple, raw material is easy to get and with low cost.
In sum, low temperature co-fired pottery baseplate material of the present invention, it has good dielectric properties, the low (ε of specific inductivity
r=6.1~8.2), the quality factor high (Q * f=9600~16000GHz) under microwave frequency, temperature coefficient of resonance frequency is adjustable (τ in containing zero scope
f=-52~28ppm/ ℃).
Two of object of the present invention is, a kind of preparation method of low-temperature co-fired ceramic substrate material is provided, and the method technique is simple, cost is low, prepared low temperature co-fired pottery baseplate material, it has good dielectric properties, can meet the dielectric properties requirement of high-frequency high-speed circuit to baseplate material.
The technical scheme that the present invention adopts is for achieving the above object, a kind of preparation method of low-temperature co-fired ceramic substrate material, and it comprises the following steps successively:
The 1st step: by SiO
2with ZnO 1:2 batching in molar ratio, to put into ball grinder and add dehydrated alcohol or deionized water carries out ball milling, Ball-milling Time is 2~3 hours, then dries, sieving for standby.
The 2nd step: by CaCO
3and TiO
21:1 batching in molar ratio, puts into ball grinder and adds dehydrated alcohol or deionized water carries out ball milling, and Ball-milling Time is 2~3 hours, then dries, sieving for standby.
The 3rd step: by SiO
2with ZnO compound from room temperature the temperature rise rate with 3~5 ℃/min, be warming up to 1100~1300 ℃ and be incubated 1~5 hour; By CaCO
3and TiO
2compound is the temperature rise rate with 3~5 ℃/min from room temperature, is warming up to 1000~1200 ℃, is incubated 1~5 hour; Make respectively Zn
2siO
4and CaTiO
3.
The 4th step: the Zn that the 3rd step is made
2siO
4and CaTiO
3pulverize respectively, and press CaTiO
3the add-on of powder accounts for CaTiO
3powder and Zn
2siO
4the molar percentage of both total amounts of powder is 3.0~10.0mol%, Bi
2o
3-CuO-B
2o
3or Li
2cO
3-Bi
2o
3-CuO-B
2o
3the add-on of powder accounts for the ratio of 5.0~10.0wt% of ceramic total mass mixes, and puts into ball grinder and adds dehydrated alcohol or deionized water carries out ball milling, and Ball-milling Time is 2~3 hours, then dries, grinding, sieving for standby.
The 5th step: adopt massfraction be 5~15wt% polyvinyl alcohol solution as binding agent, the add-on of binding agent is to treat 5~10wt% of granulation mixture quality, granulation, sieve, compression moulding.
The 6th step: the sample after compression moulding is entered to stove calcining, be incubated 1~5 hour to sintering at 900~975 ℃.
The technique effect that technique scheme produces is that sintering temperature is low, technique is simply easy to control.
As preferably, above-mentioned oven dry is carried out at 80~110 ℃, described in the sieve adopting that sieves be 40 orders.
The technique effect that above-mentioned optimal technical scheme produces is, is conducive to fully mixing of material, is conducive to carrying out smoothly of subsequent chemical reaction.
Can also be preferably, above-mentioned compression moulding adopts dry pressing, pressure 30~100MPa, and described sample is that diameter is 25mm, is highly the right cylinder of 14~17mm.
The technique effect that above-mentioned optimal technical scheme produces is, mixture is pressed into the sample that size is reasonable, structure is closely knit, be conducive to that the control of follow-up calcination process and reaction carry out thoroughly.
Can also be preferably, above-mentionedly enter stove calcining, its detailed process is that the speed with 3 ℃/min rises to 550 ℃ from room temperature in retort furnace, and is incubated 30~60 minutes; Then after continuing to be warming up to 900~975 ℃ with the speed of 5 ℃/min, be incubated 1~5 hour to sintering.
Adopt above-mentioned optimal technical scheme, its technique effect directly producing is, first with the speed of 3 ℃/min, from room temperature, rises to 550 ℃ and be incubated 30~60 minutes, and this is conducive to binding agent polyvinyl alcohol composition all to be got rid of; Then with the speed of 5 ℃/min, rise to 900~975 ℃, this is conducive to guarantee final sintering quality.
In sum, adopt the ceramic substrate material of preparation method's acquisition of low-temperature co-fired ceramic substrate material of the present invention, there is following technique effect:
(1) baseplate material of the present invention has good dielectric properties, the low (ε of specific inductivity
r=6.1~8.2), the quality factor high (Q * f=9600~16000GHz) under microwave frequency, temperature coefficient of resonance frequency is adjustable (τ in containing zero scope
fthereby can meet the dielectric properties requirement of high-frequency high-speed circuit to baseplate material=-52~28ppm/ ℃).
(2) raw material that the present invention adopts all adopts cheap oxide compound, and technique is simple, has significantly reduced the cost of product.
(3) fully demonstrated the advantage of LTCC Technology, can realize altogether and burning with the metal A g of high conductivity, and then the loss can significantly reduce Circuits System operation time.
Accompanying drawing explanation
Fig. 1, for pressing embodiment 10 batchings, adds respectively (a) Bi
2o
3-CuO-B
2o
3(b) Li
2cO
3-Bi
2o
3-CuO-B
2o
3after, through being incubated after 3 hours at 950 ℃, the XRD figure of the ceramic substrate material sample obtaining spectrum;
Fig. 2, for pressing embodiment 10 batchings, adopts respectively Bi
2o
3-CuO-B
2o
3and Li
2cO
3-Bi
2o
3-CuO-B
2o
3as the ceramics sample of sintering agent, after 950 ℃ are incubated 3 hours, the SEM collection of illustrative plates of the ceramic substrate material sample obtaining;
Fig. 3, for pressing embodiment 10 batchings, adopts Li
2cO
3-Bi
2o
3-CuO-B
2o
3the 20.0wt%Ag that adulterates in ceramics powder as sintering agent is incubated the XRD figure spectrum after 3 hours at 950 ℃.
Embodiment
Below in conjunction with example, the specific embodiment of the present invention is described further.
Embodiments of the invention 1-12 is all prepared by the method for being prepared as follows, and described preparation method comprises the following steps successively:
1, by SiO
2with ZnO 1:2 batching in molar ratio, to put into ball grinder and add dehydrated alcohol or deionized water carries out ball milling, Ball-milling Time is 2~3 hours, then at 80~110 ℃, dries, to cross 40 mesh sieves standby;
2, by CaCO
3with TiO
21:1 batching in molar ratio, puts into ball grinder and adds dehydrated alcohol or deionized water carries out ball milling, and Ball-milling Time is 2~3 hours, then at 80~110 ℃, dries, to cross 40 mesh sieves standby;
3, by SiO
2with ZnO compound from room temperature the temperature rise rate with 3~5 ℃/min, be warming up to 1100~1300 ℃ and be incubated 1~5 hour; By CaCO
3and TiO
2compound is the temperature rise rate with 3~5 ℃/min from room temperature, is warming up to 1000~1200 ℃, is incubated 1~5 hour; Make respectively Zn
2siO
4and CaTiO
3.
4, the Zn the 3rd step being made
2siO
4and CaTiO
3grind to form respectively powder, by Zn
2siO
4powder, CaTiO
3powder and Bi
2o
3-CuO-B
2o
3or Li
2cO
3-Bi
2o
3-CuO-B
2o
3powder is in the ratio batching shown in table 1, after put into ball grinder, add appropriate dehydrated alcohol or deionized water, ball milling 2~3 hours is dried after discharging, to cross 40 mesh sieves standby at 80~110 ℃.
5, adopt the solution of the polyvinyl alcohol that massfraction is 5~15wt% as tackiness agent, granulation, crosses 40 mesh sieves.
6, under 30~100MPa pressure, it is 25mm that dry pressing is pressed into diameter, is highly the right cylinder of 14~17mm, enters calcining in retort furnace, with the speed of 3 ℃/min, from room temperature, rises to 550 ℃, is incubated 30~60 minutes; Then with the speed of 5 ℃/min, rise to 900~975 ℃, be incubated 1~5 hour, then with furnace temperature, be cooled to room temperature, obtain the ceramics sample after sintering.
In embodiment 1~12, the raw material of each embodiment and formula are as shown in table 1; The dielectric properties of each laboratory sample adopt AgilentE5701C type network analyzer to measure, and detected result is as shown in table 2:
The composition of raw materials of table 1 low-temperature co-fired ceramic substrate material
The dielectric properties of table 2 laboratory sample
As can be seen from the above table, low-temperature co-fired ceramic substrate material of the present invention, can meet the dielectric properties requirement of high-frequency high-speed circuit to baseplate material, its DIELECTRIC CONSTANT ε
r=6.1~8.2, quality factor q * f=9600~16000GHz, temperature coefficient of resonance frequency τ
f=-52~28ppm/ ℃.
For a better understanding of the present invention, existing by reference to the accompanying drawings to the further explanation of the present invention's do.
Fig. 1, for pressing embodiment 10 batchings, adds respectively (a) Bi
2o
3-CuO-B
2o
3(b) Li
2cO
3-Bi
2o
3-CuO-B
2o
3after, through being incubated after 3 hours at 950 ℃, the XRD figure of the ceramic substrate material sample obtaining spectrum.
As shown in Figure 1, through 950 ℃ of insulations, after 3 hours, in sample, only contain Zn
2siO
4and CaTiO
3two kinds of phases, in the ratio of embodiment 10, add respectively Bi
2o
3-CuO-B
2o
3and Li
2cO
3-Bi
2o
3-CuO-B
2o
3the phase that does not affect sample as sintering agent forms.
Fig. 2, for pressing embodiment 10 batchings, adopts respectively Bi
2o
3-CuO-B
2o
3and Li
2cO
3-Bi
2o
3-CuO-B
2o
3as the ceramics sample of sintering agent, after 950 ℃ are incubated 3 hours, the SEM collection of illustrative plates of the ceramic substrate material sample obtaining.In figure, left side a adopts Bi
2o
3-CuO-B
2o
3the ceramics sample obtaining as sintering agent, the right b adopts the Li obtaining
2cO
3-Bi
2o
3-CuO-B
2o
3the ceramics sample obtaining as sintering agent.
As shown in Figure 2, add respectively Bi
2o
3-CuO-B
2o
3and Li
2cO
3-Bi
2o
3-CuO-B
2o
3as sintering agent, after 3 hours, all very fine and close at obtained ceramic substrate material sample structure through 950 ℃ of insulations, and homogeneous grain size, grain-size concentrates within the scope of 3-5um.
Fig. 3, for pressing embodiment 10 batchings, adopts Li
2cO
3-Bi
2o
3-CuO-B
2o
3the 20.0wt% metal A of adulterating in ceramics powder as sintering agent g is incubated the XRD figure spectrum after 3 hours at 950 ℃.
As shown in Figure 3, in the ceramic substrate material sample obtaining, the main diffraction peak of metal A g can clearly be observed in the drawings, and containing the phase of Ag compound, in XRD figure, does not occur.Therefore, Zn
2siO
4-CaTiO
3ceramics sample and Ag have good chemical compatibility, burn altogether theoretically and can realize with Ag electrode.
In sum, the preparation method of low-temperature co-fired ceramic substrate material of the present invention, its product purity is high, quality good, technique is simple, sintering temperature is low and can burn altogether with the Ag of high conductivity; And because its raw material is easy to get and cheap, correspondingly, preparation method's low cost of manufacture of low-temperature co-fired ceramic substrate material of the present invention.
Claims (7)
1. a low-temperature co-fired ceramic substrate material, is characterized in that, principal crystalline phase is Zn
2siO
4, paracrystalline phase is CaTiO
3, DIELECTRIC CONSTANT ε
r=6.1~8.2, quality factor q * f=9600~16000GHz, temperature coefficient of resonance frequency τ
f=-52~28ppm/ ℃.
2. low-temperature co-fired ceramic substrate material according to claim 1, is characterized in that, by zinc silicate Zn
2siO
4powder, calcium titanate CaTiO
3powder, Bi
2o
3-CuO-B
2o
3or Li
2cO
3-Bi
2o
3-CuO-B
2o
3powder adds in proportion, mixes, at 900~975 ℃, sintering forms, wherein:
Described CaTiO
3the add-on of powder accounts for CaTiO
3powder and Zn
2siO
4the molar percentage of both total amounts of powder is 3.0~10.0mol%;
Described Bi
2o
3-CuO-B
2o
3or Li
2cO
3-Bi
2o
3-CuO-B
2o
3the add-on of powder accounts for 5.0~10.0wt% of ceramic total mass.
3. low-temperature co-fired ceramic substrate material according to claim 1, is characterized in that, described Zn
2siO
4powder is with SiO
2with ZnO be raw material, through 1100~1300 ℃ of calcinings, make;
Described CaTiO
3powder is with CaCO
3and TiO
2for raw material, through 1000~1200 ℃ of calcinings, make.
4. a preparation method for low-temperature co-fired ceramic substrate material described in claim 1, is characterized in that, comprises the following steps successively:
The 1st step: by SiO
2with ZnO 1:2 batching in molar ratio, to put into ball grinder and add dehydrated alcohol or deionized water carries out ball milling, Ball-milling Time is 2~3 hours, then dries, sieving for standby;
The 2nd step: by CaCO
3and TiO
21:1 batching in molar ratio, puts into ball grinder and adds dehydrated alcohol or deionized water carries out ball milling, and Ball-milling Time is 2~3 hours, then dries, sieving for standby;
The 3rd step: by SiO
2with ZnO compound from room temperature the temperature rise rate with 3~5 ℃/min, be warming up to 1100~1300 ℃ and be incubated 1~5 hour; By CaCO
3and TiO
2compound is the temperature rise rate with 3~5 ℃/min from room temperature, is warming up to 1000~1200 ℃, is incubated 1~5 hour; Make respectively Zn
2siO
4and CaTiO
3.
The 4th step: the Zn that the 3rd step is made
2siO
4and CaTiO
3pulverize respectively, and press CaTiO
3the add-on of powder accounts for CaTiO
3powder and Zn
2siO
4the molar percentage of both total amounts of powder is 3.0~10.0mol%, Bi
2o
3-CuO-B
2o
3or Li
2cO
3-Bi
2o
3-CuO-B
2o
3the add-on of powder accounts for the ratio of 5.0~10.0wt% of ceramic total mass mixes, and puts into ball grinder and adds dehydrated alcohol or deionized water carries out ball milling, and Ball-milling Time is 2~3 hours, then dries, grinding, sieving for standby;
The 5th step: adopt massfraction be 5~15wt% polyvinyl alcohol solution as binding agent, the add-on of binding agent is to treat 5~10wt% of granulation mixture quality, granulation, sieve, compression moulding;
The 6th step: the sample after compression moulding is entered to stove calcining, be incubated 1~5 hour to sintering at 900~975 ℃.
5. the preparation method of low-temperature co-fired ceramic substrate material described in a kind of claim 1 according to claim 3, is characterized in that, described oven dry is carried out at 80~110 ℃, described in the sieve adopting that sieves be 40 orders.
6. the preparation method of low-temperature co-fired ceramic substrate material described in a kind of claim 1 according to claim 3, it is characterized in that, the method of described compression moulding adopts dry pressing, pressure 30~100MPa, and described sample is that diameter is 25mm, is highly the right cylinder of 14~17mm.
7. the preparation method of low-temperature co-fired ceramic substrate material described in a kind of claim 1 according to claim 3, it is characterized in that, describedly enter stove calcining, its detailed process is that the speed with 3 ℃/min rises to 550 ℃ from room temperature in retort furnace, and is incubated 30~60 minutes; Then after continuing to be warming up to 900~975 ℃ with the speed of 5 ℃/min, be incubated 1~5 hour to sintering.
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