CN110156455B - Bismuth oxide-niobium oxide based LTCC substrate material and preparation method thereof - Google Patents

Bismuth oxide-niobium oxide based LTCC substrate material and preparation method thereof Download PDF

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CN110156455B
CN110156455B CN201910600438.6A CN201910600438A CN110156455B CN 110156455 B CN110156455 B CN 110156455B CN 201910600438 A CN201910600438 A CN 201910600438A CN 110156455 B CN110156455 B CN 110156455B
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ltcc substrate
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zno
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窦占明
张二甜
应建
庞锦标
叶萍
杜玉龙
班秀峰
张秀
陈凯
褚涛
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Guizhou Zhenhua Electronic Information Industry Technology Research Co ltd
China Zhenhua Group Yunke Electronics Co Ltd
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China Zhenhua Group Yunke Electronics Co Ltd
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Abstract

The invention discloses a bismuth oxide-niobium oxide based LTCC substrate material and a preparation method thereof, wherein the preparation raw materials comprise the following components in parts by mass: bi2O3‑Nb2O595.4-99.1 parts of ceramic powder and ZnO-B2O3‑SiO20.01 to 1.5 parts of microcrystalline glass, and CuO-V2O51-3.5 parts of sintering aid. According to the LTCC substrate material, the problems that precious metal slurry volatilizes or diffuses due to high sintering temperature and long sintering time of a high-dielectric-constant dielectric ceramic material and an LTCC substrate is warped due to shrinkage characteristic difference during low-temperature co-firing are solved by adding trace glass and a low-melting-point oxide sintering aid in preparation raw materials and adjusting the particle size of the material, and the LTCC substrate material meeting the requirements is prepared.

Description

Bismuth oxide-niobium oxide based LTCC substrate material and preparation method thereof
Technical Field
The invention relates to the technical field of LTCC substrate materials, and particularly relates to a bismuth oxide-niobium oxide based LTCC substrate material and a preparation method thereof.
Background
The LTCC substrate material is a general name of the low-temperature co-fired ceramic as the substrate in the LTCC technology, the dielectric constant of the LTCC substrate material can change in a large range, and the LTCC substrate material with the flexibility of circuit design is subjected to the development processes from simple to composite, from low dielectric constant to high dielectric constant, continuous increase of the use frequency band and the like. Currently, LTCC technology is the mainstream technology of passive integration, evaluated from the perspective of technology maturity, industrialization degree, application breadth, and the like. LTCC belongs to a leading-edge product of high and new technologies, is widely applied to various fields of the microelectronic industry, and has very wide application market and development prospect. Meanwhile, the LTCC technology will also face competition and challenge from different technologies, and must continue to enhance the development of the technology and greatly reduce the manufacturing cost, so that the related technologies are continuously perfected or urgently needed to be developed.
At present, LTCC substrate materials are already in the stages of industrialization, serialization, and material design in developed countries such as japan and the usa. For example, the united states (ITRI) is actively leading to the development of PCB technologies that can embed resistors and capacitors, and is expected to reach the mature stage after 2-3 years, at which time it will become a strong competitor in the field of high frequency communication modules with the LTCC/MLC technology in the form of MCM-L. As for the manufacture of high frequency communication modules by MCM-D technology developed with the core of microelectronics, it is actively developing in the united states, the days, and the europe. How to continuously maintain the mainstream status of the LTCC technology in the field of wireless communication components, the development of the LTCC technology must be continuously enhanced and the manufacturing cost must be greatly reduced, so as to continuously improve or urgently develop the related technologies, such as solving the problems of co-firing matching with heterogeneous materials in the integrated device manufacturing process, chemical compatibility, electromechanical properties, interface behavior, and the like.
The technical difficulty of LTCC lies in that the ceramic substrate is matched and co-fired with noble metal conductor slurry such as gold, silver and the like, so that the phenomena of cracking, layering, warping and the like do not occur on the basis of ensuring the dielectric property of the ceramic substrate. Therefore, the ceramic powder which is well matched with the noble metal slurry and has the dielectric property meeting the requirement is obtained by heat preservation for 30min at the temperature of 850-930 ℃ and is the main direction for solving the LTCC substrate. Although the existing ceramic material can meet the requirements on dielectric property, the sintering temperature is too high or the sintering time is too long on the sintering property, so that the noble metal slurry is diffused or volatilized in a large amount, and the microwave property of the device is seriously influenced. Meanwhile, the matching co-firing effect is poor, the phenomena of layering, warping and the like of the substrate occur, and a lot of constraints are imposed on processing devices.
Therefore, it is urgently needed to prepare an LTCC substrate material meeting the requirements.
Disclosure of Invention
The invention aims to provide a bismuth oxide-niobium oxide based LTCC substrate material and a preparation method thereof, which solve the problems of volatilization or diffusion of noble metal slurry caused by high sintering temperature and long sintering time of a high-dielectric-constant dielectric ceramic material and the problems of warping of an LTCC substrate caused by shrinkage characteristic difference during low-temperature co-firing and the like, and have processability.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a bismuth oxide-niobium oxide based LTCC substrate material which is prepared from the following raw materials in parts by mass: bi2O3-Nb2O595.4-99.1 parts of ceramic powder and ZnO-B2O3-SiO20.01 to 1.5 parts of microcrystalline glass, and CuO-V2O51-3.5 parts of sintering aid.
The invention also provides a preparation method of the bismuth oxide-niobium oxide based LTCC substrate material, which comprises the following steps:
adding Bi2O3-Nb2O5Ceramic powder, ZnO-B2O3-SiO2Microcrystalline glass and CuO-V2O5Mixing the sintering aids in proportion, and carrying out tape casting, laminating hot pressing and sintering treatmentTo produce Bi2O3-Nb2O5A base LTCC substrate material.
The invention has the beneficial effects that:
the invention provides a bismuth oxide-niobium oxide based LTCC substrate material and a preparation method thereof, through the optimized design of raw materials in a formula, particularly through adding microcrystalline glass and a sintering aid, the shrinkage characteristic of a main crystal phase can be effectively adjusted while the sintering temperature of a green body is effectively reduced, the sintering time is shortened, the shrinkage characteristic is ensured to be approximately the same as that of noble metal conductor slurry, and the good co-firing matching with gold slurry is realized.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a process flow diagram for preparing an LTCC substrate material in embodiment 1 of the present invention;
FIG. 2 is a graph showing the co-firing effect of the LTCC substrate material matched with gold in embodiment 1 of the present invention;
FIG. 3 is a graph showing the co-firing effect of the LTCC substrate material of comparative example 1 of the present invention matching with gold;
FIG. 4 is a graph showing the co-firing effect of the LTCC substrate material of comparative example 2 of the present invention matched with gold.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The bismuth oxide-niobium oxide based LTCC substrate material and the preparation method thereof provided by the embodiments of the present invention are specifically described below.
The embodiment of the invention provides a bismuth oxide-niobium oxide based LTCC substrate material, which comprises the following raw materials in parts by mass: bi2O3-Nb2O595.4-99.1 parts of ceramic powder and ZnO-B2O3-SiO20.01 to 1.5 parts of microcrystalline glass, and CuO-V2O51-3.5 parts of sintering aid.
The embodiment of the invention provides a bismuth oxide-niobium oxide based LTCC substrate material, which comprises the following raw materials in parts by mass: bi2O3-Nb2O595.4-99.1 parts of ceramic powder and ZnO-B2O3-SiO20.01 to 1.5 parts of microcrystalline glass, and CuO-V2O51-3.5 parts of sintering aid, prepared by adding Bi into2O3-Nb2O5Adding ZnO-B into the main crystal phase of ceramic2O3-SiO2Microcrystalline glass and CuO-V2O5The sintering aid is optimally designed in formula, so that the sintering temperature and the sintering time of a green body can be effectively reduced, the noble metal conductor slurry is prevented from volatilizing and diffusing in a ceramic substrate during high-temperature long-time sintering, the shrinkage characteristic of the LTCC substrate is effectively adjusted, the ceramic shrinkage time of the ceramic substrate in the densification process is shortened, the shrinkage rate and the shrinkage rate are basically the same as those of the metal conductor slurry, and the ceramic substrate and the metal conductor slurry are matched and co-fired.
Meanwhile, the mixing ratio not only directly determines the dielectric property of the LTCC substrate material, but also is a key process for regulating and controlling the shrinkage starting time, shrinkage rate and shrinkage rate of the LTCC substrate material to be matched with the co-firing of the metal conductor slurry. If the formula proportion is not suitable, the dielectric property of the substrate cannot meet the design requirement of the LTCC assembly, and the substrate can generate the problems of warping, layering, conductor paste diffusion and the like when being matched with the conductor paste and co-fired.
In some embodiments, Bi2O3-Nb2O5Bi in ceramic powder2O3：Nb2O5In a molar ratio of 0.8 to 1.2: 1, ZnO-B2O3-SiO2ZnO in the glass ceramics: b is2O3：SiO2In a molar ratio of 45 to 75: 20-40: 5-15, CuO-V2O5CuO in the sintering aid: v2O5In a molar ratio of 1.8-2.6: 1.
in some embodiments, the bismuth oxide-niobium oxide based LTCC substrate material has a dielectric constant of 40 ≦ εrLess than or equal to 49@8GHz, and the dielectric loss tan delta is (3-8) × 10-4@8GHz。
The embodiment of the invention also provides a preparation method of the bismuth oxide-niobium oxide based LTCC substrate material, which comprises the following steps:
adding Bi2O3-Nb2O5Ceramic powder, ZnO-B2O3-SiO2Microcrystalline glass and CuO-V2O5The sintering aids are mixed in proportion, and the Bi is prepared by tape casting, laminated hot pressing and sintering treatment2O3-Nb2O5A base LTCC substrate material.
The embodiment of the invention also provides a preparation method of the bismuth oxide-niobium oxide based LTCC substrate material, which comprises the following steps: bi to be prepared2O3-Nb2O5Ceramic powder, ZnO-B2O3-SiO2Microcrystalline glass and CuO-V2O5Mixing the sintering aid to obtain a mixture, in particular by adding ZnO-B2O3-SiO2Microcrystalline glass and low-melting-point oxide sintering aid CuO-V2O5Can effectively reduce the sintering temperature of a green body and simultaneously effectively adjust the shrinkage characteristic of a main crystal phase, ensures that the prepared ceramic substrate has good microwave dielectric property and has good co-firing matching property with gold conductor slurry,
the mixed material and an organic casting system are mixed to prepare a casting material, the casting material is subjected to casting forming to prepare a raw porcelain band, the shrinkage characteristic of the material can be slightly adjusted by the particle size selection and the adding process of the amount of the organic casting solvent, and the matching co-firing is further optimized.
In some embodiments, Bi2O3-Nb2O5The ceramic powder is prepared by the following steps: according to Bi2O3：Nb2O50.8-1.2: 1, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, and calcining for 3-5 hours at 880 +/-30 ℃.
In some embodiments, ZnO-B2O3-SiO2The microcrystalline glass is prepared by the following steps: according to the ZnO: b is2O3：SiO2In a molar ratio of 45 to 75: 20-40: 5-15, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, smelting at 1200-1400 ℃ for 2-5 hours, crushing, ball milling and grinding into powder.
In some embodiments, CuO-V2O5The sintering aid is prepared by the following steps: according to the formula of CuO: v2O5In a molar ratio of 1.8-2.6: 1, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, and calcining for 30-120min at 580 +/-30 ℃.
In some embodiments, the casting comprises the steps of: grinding the mixed material into powder with the particle size of 1.5-3.0 mu m, mixing the powder with an adhesive, a plasticizer and an organic solvent to obtain a casting material, and casting the casting material to obtain the ceramic green tape with the thickness of 35-120 mu m.
In some embodiments, the stack hot pressing comprises the steps of: after printing a gold wire circuit pattern on the surface of the ceramic green tape, carrying out warm water isostatic pressing, wherein the isostatic pressing conditions are as follows: the pressure is 20MPa-50MPa, and the pressure maintaining time is 30min-90 min.
In some embodiments, sintering comprises the steps of: sintering at 880 + -40 deg.C, and keeping the temperature for 40 + -25 min.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
Referring to fig. 1, a method for preparing a bismuth oxide-niobium oxide based LTCC substrate material includes the following steps:
1) bi is added2O3、Nb2O5According to Bi2O3：Nb2O51: 1 molar ratioProportioning, mixing, ball milling, calcining at 880 ℃ for 4 hours to obtain Bi2O3-Nb2O5Ceramic powder (BN);
2)、ZnO、B2O3、SiO2according to mol ratio ZnO: b is2O3：SiO245-75: 20-40: 5-15 preparing materials, namely mixing the following materials: ball: the mass ratio of the deionized water is 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, screening by a screen, drying, crushing uniformly, melting glass at 1400 ℃, crushing the prepared glass slag, ball-milling into powder to prepare ZnO-B2O3-SiO2A glass ceramics (ZBS);
3) CuO and V are mixed2O5According to the formula of CuO: v2O51.8-2.6: 1, preparing materials according to a molar ratio; according to the material: ball: deionized water according to the mass ratio of 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, sieving by a screen, drying, crushing uniformly, calcining for 30min at 600 ℃ to prepare CuO-V2O5A sintering aid (VC);
4) and mixing BN: ZBS: VC is 98.1: 0.3: 1.6, mixing, crushing and ball-milling according to the mass ratio to obtain a mixed material with the particle size of 1.8 mu m;
5) adding the mixed material into an organic solvent system to prepare a casting material, and preparing a ceramic green tape with the thickness of 45 mu m by adopting a casting process; then, laminating ceramic green porcelain tapes, printing gold conductor slurry on the surface, drying, and then performing warm water isostatic pressing under the isostatic pressing condition: pressure 45MPa, dwell time: and (3) 30 min. Finally sintering the product in a box furnace, wherein the sintering temperature of the material is 900 ℃, and the temperature is kept for 30min to prepare Bi2O3-Nb2O5A base LTCC substrate material.
Referring to FIG. 2, FIG. 2 is a graph showing the co-firing effect of the Bi material prepared in example 12O3-Nb2O5The co-firing effect of the base LTCC substrate material is good.
The dielectric property test result of the prepared bismuth oxide-niobium oxide based LTCC substrate is as follows: the dielectric constant is 47.32@8GHz, and the dielectric loss tan delta is approximately equal to 5.48 multiplied by 10-4@8GHz, co-fired simultaneouslyThe matching performance is good, and the phenomena of warping, cracking and the like do not occur.
Example 2
A preparation method of a bismuth oxide-niobium oxide based LTCC substrate material comprises the following steps:
1) bi is added2O3、Nb2O5According to Bi2O3：Nb2O51: 1 mol ratio, ball milling, calcining at 900 ℃ for 4 hours to prepare Bi2O3-Nb2O5Ceramic powder (BN);
2)、ZnO、B2O3、SiO2according to mol ratio ZnO: b is2O3：SiO245-75: 20-40: 5-15 preparing materials, namely mixing the following materials: ball: the mass ratio of the deionized water is 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, screening by a screen, drying, crushing uniformly, melting glass at 1400 ℃, crushing the prepared glass slag, ball-milling into powder to prepare ZnO-B2O3-SiO2A glass ceramics (ZBS);
3) CuO and V are mixed2O5According to the formula of CuO: v2O51.8-2.6: 1, preparing materials according to a molar ratio; according to the material: ball: deionized water according to the mass ratio of 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, sieving by a screen, drying, crushing uniformly, calcining for 30min at 600 ℃ to prepare CuO-V2O5A sintering aid (VC);
4) and mixing BN: ZBS: VC is 98.5: 0.1: 1.4, mixing, crushing and ball-milling according to the mass ratio to obtain a mixed material with the particle size of 2.1 mu m;
5) adding the mixed material into an organic solvent system to prepare a casting material, and preparing a ceramic green tape with the thickness of 95 microns by adopting a casting process; then, laminating ceramic green porcelain tapes, printing gold conductor slurry on the surface, drying, and then performing warm water isostatic pressing under the isostatic pressing condition: pressure 45MPa, dwell time: and (3) 30 min. Finally sintering the product in a box furnace, wherein the sintering temperature of the material is 870 ℃, and the temperature is kept for 30min to prepare Bi2O3-Nb2O5A base LTCC substrate material.
The dielectric property test result of the bismuth oxide-niobium oxide based LTCC substrate prepared by the method is as follows: the dielectric constant is 43.62@8GHz, and the dielectric loss tan delta is approximately equal to 3.45 multiplied by 10-4@8GHz, good co-firing matching performance, no phenomena of warping, cracking and the like.
Example 3
A preparation method of a bismuth oxide-niobium oxide based LTCC substrate material comprises the following steps:
1) bi is added2O3、Nb2O5According to Bi2O3：Nb2O50.8: 1 mol ratio, ball milling, calcining at 900 ℃ for 4 hours to prepare Bi2O3-Nb2O5Ceramic powder (BN);
2)、ZnO、B2O3、SiO2according to mol ratio ZnO: b is2O3：SiO245-75: 20-40: 5-15 preparing materials, namely mixing the following materials: ball: the mass ratio of the deionized water is 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, screening by a screen, drying, crushing uniformly, melting glass at 1400 ℃, crushing the prepared glass slag, ball-milling into powder to prepare ZnO-B2O3-SiO2A glass ceramics (ZBS);
3) CuO and V are mixed2O5According to the formula of CuO: v2O51.8-2.6: 1, preparing materials according to a molar ratio; according to the material: ball: deionized water according to the mass ratio of 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, sieving by a screen, drying, crushing uniformly, calcining for 30min at 600 ℃ to prepare CuO-V2O5A sintering aid (VC);
4) and mixing BN: ZBS: VC is 97.5: 1.5: 1, mixing, crushing and ball-milling according to a mass ratio to obtain a mixed material with the particle size of 2.1 mu m;
5) adding the mixed material into an organic solvent system to prepare a casting material, and preparing a ceramic green tape with the thickness of 75 microns by adopting a casting process; then, laminating ceramic green porcelain tapes, printing gold conductor slurry on the surface, drying, and then performing warm water isostatic pressing under the isostatic pressing condition: pressure 45MPa, dwell time: and (3) 30 min. Finally, theSintering the product in a box furnace at 850 ℃ for 20min to obtain Bi2O3-Nb2O5A base LTCC substrate material.
The bismuth oxide-niobium oxide based LTCC substrate prepared by the method has good co-firing matching performance with metal conductor slurry, and does not have the phenomena of warping, cracking and the like.
Example 4
A preparation method of a bismuth oxide-niobium oxide based LTCC substrate material comprises the following steps:
1) bi is added2O3、Nb2O5According to Bi2O3：Nb2O51: proportioning the raw materials according to the molar ratio of 1.2, mixing the raw materials, ball-milling, calcining at 900 ℃ for 4 hours to prepare Bi2O3-Nb2O5Ceramic powder (BN);
2)、ZnO、B2O3、SiO2according to mol ratio ZnO: b is2O3：SiO245-75: 20-40: 5-15 preparing materials, namely mixing the following materials: ball: the mass ratio of the deionized water is 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, screening by a screen, drying, crushing uniformly, melting glass at 1400 ℃, crushing the prepared glass slag, ball-milling into powder to prepare ZnO-B2O3-SiO2A glass ceramics (ZBS);
3) CuO and V are mixed2O5According to the formula of CuO: v2O51.8-2.6: 1, preparing materials according to a molar ratio; according to the material: ball: deionized water according to the mass ratio of 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, sieving by a screen, drying, crushing uniformly, calcining for 30min at 600 ℃ to prepare CuO-V2O5A sintering aid (VC);
4) and mixing BN: ZBS: VC 96.49: 0.01: 3.5, mixing, crushing and ball-milling according to the mass ratio to obtain a mixed material with the particle size of 2.5 mu m;
5) adding the mixed material into an organic solvent system to prepare a casting material, and preparing a ceramic green tape with the thickness of 65 mu m by adopting a casting process; then laminating ceramic green ceramic tapes, printing gold conductor slurry on the surface, drying, and thenCarrying out warm water isostatic pressing, wherein the isostatic pressing condition is as follows: pressure 45MPa, dwell time: and (3) 30 min. Finally sintering the product in a box furnace, wherein the sintering temperature of the material is 850 ℃, and the heat preservation is carried out for 15min to prepare Bi2O3-Nb2O5A base LTCC substrate material.
The bismuth oxide-niobium oxide based LTCC substrate prepared by the method has good co-firing matching performance with metal conductor slurry, and does not have the phenomena of warping, cracking and the like.
Comparative example 1
The main preparation method and procedure in this example are the same as in the previous example 3, except that: change BN in step 4) on the basis of example 3: ZBS: VC proportion is BN: ZBS: and VC is 95: 1.5: 3.5.
as shown in FIG. 3, the Bi prepared above was examined2O3-Nb2O5The substrate dielectric gold conductor slurry has no warpage after sintering, but has poor co-firing effect, and has the surface phenomena of gold diffusion and VC floating, which is particularly shown in that the gold surface is darker.
Comparative example 2
This example provides a method for preparing a bismuth oxide-niobium oxide-based substrate material unmatched with a gold paste by co-firing, wherein the main preparation method and steps are the same as those in the previous embodiment, mainly different from CuO-V2O5The amount of sintering aid used is outside the range claimed in the present invention, and comprises the following steps:
1) bi is added2O3、Nb2O5According to Bi2O3：Nb2O51: 1 mol ratio, ball milling, calcining at 880 ℃ for 3.5 hours to prepare Bi2O3-Nb2O5Ceramic powder (BN);
2)、ZnO、B2O3、SiO2according to mol ratio ZnO: b is2O3：SiO2＝45％-75％ZnO：20％-40％B2O3：5％-15％SiO2Preparing materials, namely preparing the following raw materials: ball: the mass ratio of the deionized water is 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, screening by a screen, drying, crushing uniformly, and thenThen melting glass at 1400 ℃, crushing and ball-grinding the prepared glass slag into powder to prepare ZnO-B2O3-SiO2A glass ceramics (ZBS);
3) CuO and V are mixed2O5According to the formula of CuO: v2O5Burdening according to the mol ratio of 1.8-2.6; according to the material: ball: deionized water according to the mass ratio of 1: 3: 2 mixing, ball milling for 6-8 hours by a planetary ball mill, sieving by a screen, drying, crushing uniformly, calcining for 30min at 600 ℃ to prepare CuO-V2O5A sintering aid (VC);
4) and mixing BN: ZBS: VC is 98.5: 0.2: 4, preparing materials according to the mass ratio, crushing and ball-milling to obtain a mixed material with the particle size of 2 mu m;
5) adding the mixed material into an organic solvent system to prepare a casting material, and preparing a ceramic green tape with the thickness of 65 mu m by adopting a casting process; then, laminating ceramic green porcelain tapes, printing gold conductor slurry on the surface, drying, and then performing warm water isostatic pressing under the isostatic pressing condition: pressure 45MPa, dwell time: and (3) 30 min. Finally sintering the product in a box furnace, wherein the sintering temperature of the material is 880 ℃, and the heat preservation is carried out for 30min to prepare Bi2O3-Nb2O5A base LTCC substrate material.
The dielectric property test result of the bismuth oxide-niobium oxide base plate prepared by the method is as follows: the dielectric constant is 46.82@8GHz, and the dielectric loss tan delta is approximately equal to 6.96 multiplied by 10-4@8GHz, as can be seen from FIG. 4, the co-firing effect with the gold conductor paste is slightly poor, and the warping phenomenon occurs, and the warping degree is about 1%.
To sum up, the embodiment of the invention provides a bismuth oxide-niobium oxide based LTCC substrate material and a preparation method thereof, wherein the preparation raw materials comprise the following components in parts by mass: bi2O3-Nb2O595.4-99.1 parts of ceramic powder and ZnO-B2O3-SiO20.01 to 1.5 parts of microcrystalline glass, and CuO-V2O51-3.5 parts of sintering aid. The preparation raw materials comprise ZnO-B which can reduce the sintering temperature and the sintering time and can regulate and control the shrinkage characteristics (shrinkage starting time, shrinkage rate and shrinkage rate) of the ceramic during the densification process of the ceramic substrate2O3-SiO2Microcrystalline glass and low-melting-point oxide sintering aid CuO-V2O5The components are used as the raw materials, the shrinkage characteristics of the prepared raw materials are almost the same as those of the noble metal conductor slurry in the sintering process, the prepared raw materials and the gold slurry can be subjected to heat preservation for 40 +/-25 min at the temperature of 880 +/-40 ℃ to realize matching co-firing, the conductor slurry does not volatilize or diffuse, and the substrate does not warp. The prepared LTCC substrate material has good microwave dielectric property, and has good co-firing matching property with gold slurry.
Meanwhile, as the applicability of the LTCC substrate material mainly lies in the low-temperature rapid matching co-firing with the metal conductor slurry, the matching co-firing effect of the material is influenced by the main crystal phase, the glass crystallites, the oxide sintering aid, the particle size and the like in each formula, and thus, the problem of mismatching of co-firing can be caused by only changing one or two variables.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. 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.

Claims (10)

1. The bismuth oxide-niobium oxide based LTCC substrate material is characterized by comprising the following raw materials in parts by mass: bi2O3-Nb2O595.4-99.1 parts of ceramic powder and ZnO-B2O3-SiO20.01 to 1.5 parts of microcrystalline glass, and CuO-V2O51-3.5 parts of sintering aid, wherein,
the Bi2O3-Nb2O5The ceramic powder is prepared by the following steps: according to Bi2O3：Nb2O5In a molar ratio of 0.8 to 1.2: 1, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, and calcining at 880 +/-30 DEG CThe mixture is burnt for 3 to 5 hours,
the ZnO-B2O3-SiO2The microcrystalline glass is prepared by the following steps: according to the ZnO: b is2O3：SiO2In a molar ratio of 45 to 75: 20-40: 5-15, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, smelting at 1200-1400 ℃ for 2-5 hours, crushing, ball milling into powder,
the CuO-V2O5The sintering aid is prepared by the following steps: according to the formula of CuO: v2O5In a molar ratio of 1.8-2.6: 1, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, and calcining for 30-120min at 580 +/-30 ℃.
2. The bismuth oxide-niobium oxide based LTCC substrate material of claim 1, wherein the Bi is2O3-Nb2O5Bi in ceramic powder2O3：Nb2O5In a molar ratio of 0.8 to 1.2: 1, said ZnO-B2O3-SiO2ZnO in the glass ceramics: b is2O3：SiO2In a molar ratio of 45 to 75: 20-40: 5 to 15, said CuO-V2O5CuO in the sintering aid: v2O5In a molar ratio of 1.8-2.6: 1.
3. the bismuth oxide-niobium oxide-based LTCC substrate material according to claim 1 or 2, wherein the dielectric constant of the bismuth oxide-niobium oxide-based LTCC substrate material is 40 ≤ epsilonrLess than or equal to 49@8GHz, and the dielectric loss tan delta is 3-8 multiplied by 10-4@8GHz。
4. A method for producing a bismuth oxide-niobium oxide based LTCC substrate material according to any one of claims 1 to 3, comprising the steps of:
the Bi is added2O3-Nb2O5Ceramic powder and said ZnO-B2O3-SiO2Microcrystalline glass and CuO-V2O5Mixing the sintering aids in proportion, and casting,Laminated hot pressing and sintering treatment to obtain the Bi2O3-Nb2O5A base LTCC substrate material.
5. The method according to claim 4, wherein said Bi2O3-Nb2O5The ceramic powder is prepared by the following steps: according to Bi2O3：Nb2O5In a molar ratio of 0.8 to 1.2: 1, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, and calcining for 3-5 hours at 880 +/-30 ℃.
6. The production method according to claim 4, wherein the ZnO-B is2O3-SiO2The microcrystalline glass is prepared by the following steps: according to the ZnO: b is2O3：SiO2In a molar ratio of 45 to 75: 20-40: 5-15, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, smelting at 1200-1400 ℃ for 2-5 hours, crushing, ball milling and grinding into powder.
7. The method according to claim 4, wherein said CuO-V is2O5The sintering aid is prepared by the following steps: according to the formula of CuO: v2O5In a molar ratio of 1.8-2.6: 1, ball milling for 6-8 hours, screening by a screen, drying, crushing uniformly, and calcining for 30-120min at 580 +/-30 ℃.
8. The production method according to claim 4, wherein the casting includes the steps of: grinding the preparation raw materials into powder with the particle size of 1.5-3.0 microns, mixing the powder with an adhesive, a plasticizer and an organic solvent to obtain a casting material, and casting the casting material to obtain the ceramic green tape with the thickness of 35-120 microns.
9. The method of claim 8, wherein the stack hot pressing comprises the steps of: after printing a gold wire circuit pattern on the surface of the ceramic green tape, carrying out warm water isostatic pressing, wherein the isostatic pressing conditions are as follows: the pressure is 20MPa-50MPa, and the pressure maintaining time is 30min-90 min.
10. The method of manufacturing according to claim 4, wherein the sintering comprises: sintering at 880 + -40 deg.C, and keeping the temperature for 40 + -25 min.
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