CN110171972B - Low-temperature sintered ceramic material - Google Patents
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Abstract
The invention discloses a low-temperature sintered ceramic material. The invention uses 1-x-ywt% of Ba5Nb4O15Ceramic material and xwt% TiBO3+ywt％Cu9Ti2(B2O5)2(BO3)2O6And (3) co-sintering the compounds, wherein the ranges of the compound powder x and y are between 0.01% and 10wt% of x and between 0.01% and 10wt% of z. Furthermore, TiBO3Belongs to TiO2And B2O3Compound produced after co-calcination, Cu9Ti2(B2O5)2(BO3)2O6Belongs to CuO and TiO2And B2O3The compounds produced after co-calcination, both of which can form a phase at very low temperatures due to the eutectic point produced after calcination, and in addition, are added into Ba5Nb4O15After the ceramic material is sintered, the sintering temperature can be greatly reduced, and the sintering densification can be achieved within the temperature range of 700-1000 ℃.
Description
Technical Field
The invention relates to a microwave dielectric material manufactured by a low-temperature co-fired ceramic technology, in particular to a low-temperature sintered ceramic material.
Background
A common Low temperature co-fired ceramic (LTCC) process involves the addition of a ceramic plus a Low melting point oxide such as boron oxide (B)2O3) Or vanadium pentoxide (V)2O5) Mainly, the sintering temperature is reduced by melting low-melting point oxides firstly. Another way is to lower the sintering temperature by the liquid phase sintering behavior generated by the ceramic plus glass method.
Due to Ba5Nb4O15Srivastave, A.M. in "J.solid State Chem" 1997, volume 134, gave a dielectric constant ε when sintered at a high temperature of 1380 ℃r41, quality factor Qxf 57,000GHz and temperature coefficient of frequency τfThe microwave dielectric property is 50 ppm/DEG C, however, the sintering temperature is too high, so that the electrode material needs to use a silver palladium electrode. To achieve cofiring with silver at low temperatures, Kim.D.W. et al utilized B in the "Journal of the European Ceramic Society" 2003 23 curling Table2O3Addition into (1-x) Ba5Nb4O15-xBaNb2O6After that, the sintering temperature can be lowered to 900 ℃, and the quality factor Q × f becomes 28,000GHz while the temperature frequency coefficient is close to zero.
However, if B is added2O3Equal low melting point oxide due to B2O3It is easy to react with water, methanol, ethanol and commonly used adhesives such as PVA and PVB, etc. to generate a gel effect, which causes a large variation in sintering density due to uneven powder dispersion during the tape manufacturing process in the MLCC (Multi-layer Ceramic Capacitor) process. In addition B2O3High solubility in water and alcohol, and easy drying in powder filtering stage2O3Component loss, resulting in B2O3The reduction results in a reduction in the sintered density and a loss in dielectric characteristics.
Disclosure of Invention
In view of the above technical problems, an object of the present invention is to provide a low temperature sintered ceramic material. The invention uses low temperature co-fired ceramic technology to manufacture microwave dielectric material.
The technical scheme for realizing the invention is as follows:
a low-temperature sintered ceramic material is characterized by comprising the following components:
xwt％TiBO3；
ywt％Cu9Ti2(B2O5)2(BO3)2O6；
1-x-ywt％Ba5Nb4O15；
wherein the range of x and y of the compound powder is between 0.01% and 10wt% of x, and between 0.01% and 10wt% of y.
Further, the TiBO3Belongs to TiO2And B2O3The compound produced after co-calcination, Cu9Ti2(B2O5)2(BO3)2O6Belongs to CuO and TiO2And B2O3The compound produced after co-calcination.
Further, the TiBO3，Cu9Ti2(B2O5)2(BO3)2O6These two compounds can form a phase at a very low temperature because they can generate eutectic points after calcination, and are added into Ba5Nb4O15After the ceramic material is sintered, the sintering temperature can be greatly reduced, and the sintering densification can be achieved within the temperature range of 700-1000 ℃.
Furthermore, the material has the characteristics of measuring more than 1GHz high-frequency microwave, the dielectric constant is between 35 and 45, and the Q x f is more than 24000, and the material can be effectively co-sintered with silver metal and copper metal of an electrode to achieve the application of the low-temperature co-fired ceramic microwave material.
The invention provides a preparation method of a low-temperature sintered ceramic material, which comprises the following steps:
1)Ba5Nb4O15preparing the ceramic: mixing BaO 35-60 wt% and Nb 25-50 wt%2O5After the powders are mixed, the mixture is calcined at the temperature of 900-1200 ℃ for 2 hours to obtain Ba5Nb4O15A compound;
2)TiBO3preparation of oxides: mixing B in a proportion of 30-55 wt%2O3And 40-55 wt% TiO2Mixing the powders, calcining at 900 ℃ under 700-3A compound;
3)Cu9Ti2(B2O5)2(BO3)2O6preparation of oxides: mixing 50-75 wt% of CuO and 25-55 wt% of B2O3And 15-35 wt% TiO2After mixing the powders, calcining at 700-900 ℃ to obtain Cu9Ti2(B2O5)2(BO3)2O6A compound;
4) the finished product powder is prepared by mixing, and specifically comprises the following steps:
1-x-ywt% of Ba5Nb4O15Ceramic material and xwt% TiBO3+ywt％Cu9Ti2(B2O5)2(BO3)2O6Mixing the low melting point oxides in a material ratio range0.01 wt% or more and x 10wt% or more, 0.01 wt% or more and y 10wt% or more, and adding water, alcohol, dispersant or the like to the mixture to conduct wet mixing and grinding for 2 hours, wherein the grinding particle size is controlled to 1 μm, and the dried material powder is a finished powder.
Further, in the step 1), 35-60 wt% of BaO and 25-50 wt% of Nb are firstly added into the original powder2O5Carrying out wet ball milling, mixing for 24 hours, drying, filter pressing and calcining; the calcination temperature is 900-1200 ℃ per 2 hours; the calcined powder was crushed and ground to 2 μm or less.
Further, in step 2), 30-55 wt% of B is firstly added to the original powder2O3And 40-55 wt% TiO2Carrying out wet ball milling, mixing for 24 hours, drying, filter pressing and calcining; the calcination temperature is 700-900 ℃ per 2 hours; the calcined powder was crushed and ground to 2 μm or less.
Further, 50-75 wt% of CuO and 25-55 wt% of B are firstly added into the original powder in the step 3)2O3And 15-35 wt% TiO2Carrying out wet ball milling on the powder, mixing for 24 hours, drying, press filtering and calcining; the calcination temperature is 700-900 ℃ per 2 hours; the calcined powder was crushed and ground to 2 μm or less.
Further, the sample powder ground in the step 4) is manufactured into a component, the mixed material is sintered at low temperature, the sintering temperature is 700-1000 ℃, the mixed material can be co-sintered with silver and copper, the sintering time is 0.5-4 hours, the microwave dielectric material has a dielectric constant within the range of 35-45, and simultaneously has a high quality factor and a temperature frequency coefficient close to zero.
Furthermore, the material can be effectively co-fired with an electrode silver metal material, and is applied to the fields of low-temperature co-fired ceramic microwave and millimeter wave.
Compared with the prior art, the invention has the following remarkable advantages:
the invention uses CuO-TiO2-B2O3The powders are mixed and calcined at 1300 ℃ in the range 1000 ℃ to give TiBO3And Cu9Ti2(B2O5)2(BO3)2O6Compound (I) is TiBO3And Cu9Ti2(B2O5)2(BO3)2O6The compound has low melting point and high stability, can not react with water, methanol, ethanol, PVA and PVB, can not be dissolved in water and alcohol, and can achieve the effect of effective sintering densification with ceramic powder at the low temperature of 700 DEG and 1000 ℃.
The invention utilizes TiBO3And Cu9Ti2(B2O5)2(BO3)2O6Addition of Compounds into Ba5Nb4O15After ceramic powder, because of TiBO3And Cu9Ti2(B2O5)2(BO3)2O6The compound has high stability, and does not react with high molecular materials such as water, alcohol, adhesive, etc., so no gelation occurs, and in addition, the compound of the present invention only reacts with Ba5Nb4O15The ceramic powder generates liquid phase sintering characteristic, so that the material system meets the temperature of the low temperature co-fired ceramic process, can be sintered compactly at the temperature of 700-1000 ℃, and is not contacted with Ba5Nb4O15The system of the present invention can be co-fired with noble metal electrodes (silver) effectively in atmospheric environment and with base electrodes (copper) effectively in reducing atmosphere conditions, and can be applied to microwave dielectric components.
Detailed Description
The invention will be further elucidated with reference to the following specific examples. It is to be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention, which is to be given the full breadth of the appended claims and any and all equivalent modifications thereof which may occur to those skilled in the art upon reading the present specification.
The present invention is a new invented material, mainly Ba5Nb4O15Ceramic material mixed TiBO3And Cu9Ti2(B2O5)2(BO3)2O6Compound due to TiBO3And Cu9Ti2(B2O5)2(BO3)2O6The compound has high stability, is not easy to hydrolyze in water or alcohol, is not easy to react with an adhesive and the like, and does not react with ceramic to generate other secondary phases during material sintering, so the invention has high innovation.
In addition, after mixing and sintering different ceramic material compositions and different glass compositions, the dielectric properties are divided into comparative examples and examples, respectively as follows:
when 1-x-ywt% of Ba5Nb4O15Ceramic material mixed xwt% TiBO3+ywt％Cu9Ti2(B2O5)2(BO3)2O6The compounds were sintered at 750 ℃ and the results are given in table one, while the comparative examples and examples are as follows:
comparative example 1
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 0wt% of TiBO3With 0wt% of Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 750 ℃, the sintering is not compact, the dielectric constant cannot be increased to 20 due to more pores of the ceramic, and the quality factor is low to 2,752GHz because microwave signals under high frequency are lost in the pores due to more pores.
Example 1
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 1 wt% of TiBO3With 1-10 wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 750 ℃, the ceramic can be found to be dense after sintering, the dielectric constant value ranges from 35 to 37, the quality factor ranges from 26,174GHz to 33,216GHz, the temperature frequency coefficient ranges from 51 ppm/DEG C to 55 ppm/DEG C, the temperature capacitance coefficient ranges from-101 ppm/DEG C to-110 ppm/DEG C, and the insulation resistance reaches 8.5 x 1011To 3.7X 1012Omega, the material is suitable for co-firing with silver and copper.
Example 2
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 4 wt% of TiBO3With 1-10 wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 750 ℃, the ceramic can be found to be dense after sintering, the dielectric constant value ranges from 36 to 37.5, the quality factor ranges from 29,656GHz to 33,213GHz, the temperature frequency coefficient ranges from 36 to 40 ppm/DEG C, the temperature capacitance coefficient ranges from-71 to-81 ppm/DEG C, and the insulation resistance reaches 2.3 x 1012To 6.5X 1012Omega, the material is suitable for co-firing with silver and copper.
Example 3
When 1-x-ywt% of Ba5Nb4O15Ceramic material Ba5Nb4O15Ceramic material mixed with 7 wt% of TiBO3With 1-10 wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 750 ℃, the ceramic can be found to be dense after sintering, the dielectric constant value ranges from 36.5 to 38, the quality factor ranges from 24,754GHz to 32,638GHz, the temperature frequency coefficient ranges from 13 ppm/DEG C to 15 ppm/DEG C, the temperature capacitance coefficient ranges from-25 ppm/DEG C to-30 ppm/DEG C, and the insulation resistance reaches 1.7 x 1012To 3.3X 1012Omega, the material is suitable for co-firing with silver and copper.
Example 4
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 10wt% of TiBO3With 1-10 wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 750 ℃, the ceramic can be found to be dense after sintering, the dielectric constant value ranges from 36.8 to 39, the quality factor ranges from 26,052GHz to 31,595GHz, the temperature frequency coefficient ranges from 3 ppm/DEG C to-2 ppm/DEG C, the temperature capacitance coefficient ranges from 5 ppm/DEG C to-7 ppm/DEG C, and the insulation resistance reaches 2.1 x 1012To 4.1X 1012Omega, the material is suitable for co-firing with silver and copper.
(II) when 1-x-ywt% of Ba5Nb4O15Ceramic materialMixed xwt% TiBO3+ywt％Cu9Ti2(B2O5)2(BO3)2O6The compounds were sintered at 900 ℃ and the results are given in Table II, while the comparative examples and examples are as follows:
comparative example 2
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 0wt% of TiBO3With 0wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 900 ℃, the sintering is not compact, the dielectric constant cannot be increased to 24 due to more pores of the ceramic, and the quality factor is low to 2,831GHz because microwave signals under high frequency are lost in the pores due to more pores.
Example 5
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 1 wt% of TiBO3With 1-10 wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 900 ℃, it can be found that the ceramic becomes dense after sintering, the dielectric constant value ranges from 37.8 to 39.9, the quality factor ranges from 27,142GHz to 34,445GHz, the temperature frequency coefficient ranges from 47 ppm/DEG C to 51 ppm/DEG C, the temperature capacitance coefficient ranges from-94 ppm/DEG C to-101 ppm/DEG C, and the insulation resistance reaches 8.2 x 1011To 3.4X 1012Omega, the material is suitable for co-firing with silver and copper.
Example 6
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 4 wt% of TiBO3With 1-10 wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 900 ℃, the ceramic can be found to be dense after sintering, the dielectric constant value ranges from 38.8 to 42, the quality factor ranges from 30,753GHz to 34,442GHz, the temperature frequency coefficient ranges from 33 ppm/DEG C to 37 ppm/DEG C, the temperature capacitance coefficient ranges from-66 ppm/DEG C to-74 ppm/DEG C, and the insulation resistance reaches 2.8 x 1012To 6.6X 1012Omega, material and suitable for co-firing with silverCo-fired with copper.
Example 7
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 7 wt% of TiBO3With 1-10 wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 900 ℃, the ceramic can be found to be dense after sintering, the dielectric constant value ranges from 39.4 to 44, the quality factor ranges from 25,670GHz to 33,846GHz, the temperature frequency coefficient ranges from 12 ppm/DEG C to 14 ppm/DEG C, the temperature capacitance coefficient ranges from-24 ppm/DEG C to-28 ppm/DEG C, and the insulation resistance reaches 1.9 x 1012To 3.9X 1012Omega, the material is suitable for co-firing with silver and copper.
Example 8
When 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with 10wt% of TiBO3With 1-10 wt% Cu9Ti2(B2O5)2(BO3)2O6When the compound is sintered at 900 ℃, the ceramic can be found to be dense after sintering, the dielectric constant value ranges from 39.8 to 45, the quality factor ranges from 27,016GHz to 32,764GHz, the temperature frequency coefficient ranges from 3 to-2 ppm/DEG C, the temperature capacitance coefficient ranges from 4 to-6 ppm/DEG C, and the insulation resistance reaches 2.5 x 1012To 4.8X 1012Omega, the material is suitable for co-firing with silver and copper.
TABLE 1-x-ywt% of Ba5Nb4O15Ceramic material mixed with x wt% TiBO3With ywt% Cu9Ti2(B2O5)2(BO3)2O6Sintering behavior of the compound at 750 DEG C
TABLE II when 1-x-ywt% Ba5Nb4O15Ceramic material mixed with x wt% TiBO3With ywt% Cu9Ti2(B2O5)2(BO3)2O6Compound (I) in (9)00℃
Claims (4)
1. A low-temperature sintered ceramic material is characterized by comprising the following components:
xwt%TiBO3；
ywt%Cu9Ti2(B2O5)2(BO3)2O6；
1-x-ywt%Ba5Nb4O15；
wherein the range of x and y of the compound powder is between 0.01% and 10wt% of x, and between 0.01% and 10wt% of y; the TiBO3Belongs to TiO2And B2O3The compound produced after co-calcination, Cu9Ti2(B2O5)2(BO3)2O6Belongs to CuO and TiO2And B2O3The compound produced after co-calcination.
2. The low-temperature sintered ceramic material of claim 1, wherein the TiBO is3，Cu9Ti2(B2O5)2(BO3)2O6Addition into Ba5Nb4O15After the ceramic material is adopted, the Ba can be greatly reduced5Nb4O15The sintering temperature of the ceramic material reaches the sintering densification within the temperature range of 700-1000 ℃.
3. The low-temperature sintered ceramic material of claim 1, wherein the material has a dielectric constant of 35-45, measured at a frequency of 1GHz or more, and Q x f > 24000; the material can be effectively co-fired with silver metal or copper metal of an electrode to obtain the low-temperature co-fired ceramic microwave material.
4. The low-temperature sintered ceramic material as claimed in any one of claims 1 to 3, wherein the material can be co-sintered effectively with an electrode silver metal material, and is applied to the field of low-temperature co-fired ceramic microwave materials.
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