CN106995312B - Preparation method of multilayer heterogeneous ceramic high-temperature co-fired L C filter - Google Patents
Preparation method of multilayer heterogeneous ceramic high-temperature co-fired L C filter Download PDFInfo
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- CN106995312B CN106995312B CN201710305323.5A CN201710305323A CN106995312B CN 106995312 B CN106995312 B CN 106995312B CN 201710305323 A CN201710305323 A CN 201710305323A CN 106995312 B CN106995312 B CN 106995312B
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- 229910052573 porcelain Inorganic materials 0.000 claims description 24
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 16
- 229910052709 silver Inorganic materials 0.000 claims description 16
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- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 4
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- SWPMTVXRLXPNDP-UHFFFAOYSA-N 4-hydroxy-2,6,6-trimethylcyclohexene-1-carbaldehyde Chemical compound CC1=C(C=O)C(C)(C)CC(O)C1 SWPMTVXRLXPNDP-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
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- ZFZQOKHLXAVJIF-UHFFFAOYSA-N zinc;boric acid;dihydroxy(dioxido)silane Chemical compound [Zn+2].OB(O)O.O[Si](O)([O-])[O-] ZFZQOKHLXAVJIF-UHFFFAOYSA-N 0.000 description 3
- 229910017518 Cu Zn Inorganic materials 0.000 description 2
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- 229910052788 barium Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 2
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- 239000002131 composite material Substances 0.000 description 2
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
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- 238000010030 laminating Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
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- 229910052712 strontium Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- RPEUFVJJAJYJSS-UHFFFAOYSA-N zinc;oxido(dioxo)niobium Chemical compound [Zn+2].[O-][Nb](=O)=O.[O-][Nb](=O)=O RPEUFVJJAJYJSS-UHFFFAOYSA-N 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
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- 238000007599 discharging Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
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- 239000002241 glass-ceramic Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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Abstract
The invention provides a preparation method of a multilayer heterogeneous ceramic high-temperature co-fired L C filter, which can effectively solve the technical problems of poor heat dispersion and high-frequency electrical property, excessive product layer number, overlarge volume and the like of a L C filter in the prior art due to the adoption of a homogeneous microwave dielectric material as a raw material by designing a raw material formula and a casting material formula of a microwave ferrite material and a microwave dielectric ceramic and adjusting casting and co-firing processes, and realizes the development of a multilayer sheet type L C filter product to the direction of microminiaturization, light weight, high frequency and high quality, thereby having great significance and good market application prospect.
Description
Technical Field
The invention relates to the field of filter manufacturing, in particular to a preparation method of a multilayer heterogeneous ceramic high-temperature co-fired L C filter.
Background
With the progress of science and technology, the requirements of the fields of aerospace and aviation on wireless communication technology are gradually increased, and further higher requirements on the integration level, the electrical performance, the volume, the weight, the reliability, the amplitude-phase consistency and the like of microwave electronic components are provided. The multilayer co-fired ceramic (including low-temperature and high-temperature multilayer co-fired ceramics) becomes a preferred material of a Multi-Chip Module (MCM) with excellent electrical, mechanical and thermal characteristics, the MCM can realize high integration of various low-power radio frequency and microwave functional modules and even systems in a 3D (three-dimensional) multilayer circuit structure, has excellent high-frequency characteristics, and is widely applied to the fields of aerospace, wireless communication and the like.
At present, many production process lines of low-Temperature Co-fired ceramics (L TCC, <tttranslation = 'L' >tl <t/t >tow thermal Ceramic Co-fired Ceramic) are in China, the adopted materials are mainly from 951 series (Ceramic material dielectric constant 7.8) of U.S. Dupont company and A6 series (Ceramic material dielectric constant 5.9) of Ferro company, the series of materials comprise green Ceramic tapes, series resistance paste, series gold paste, series silver paste, encapsulation paste and the like, the TCC Temperature is 850 ℃, the green Ceramic tapes are homogeneous low-dielectric microwave ceramics, the High-Temperature Co-fired ceramics (HTCC, High-Temperature Co-fired Ceramic) are not limited by sintering Temperature, the Ceramic substrate can adopt pure microwave Ceramic phase without adding glass phase, the dielectric constant is larger than that of glass ceramics for L, the loss tangent is High, the heat dissipation performance is good, the mechanical strength is High, the L mechanical strength is High, and the Ceramic substrate has the advantages of single Ceramic substrate, and the like.
L C filters developed at home and abroad at present are also concentrated on L TCC filters, the used materials are the same kind of microwave dielectric materials or microwave ferrite materials and gold and silver paste which are co-fired, the defects are that the magnetic conductivity of the dielectric materials is lower (the magnetic conductivity of the dielectric materials is 1) or the dielectric constant is lower (generally below 10), and the integrated components are difficult to further miniaturize, and the microwave dielectric ceramics with higher dielectric constant, the microwave ferrites with high magnetic conductivity and the silver palladium paste are co-fired at high temperature, so that the good high-frequency characteristics of the microwave dielectric ceramics can be utilized, the steep absorption characteristics of the ferrite materials can be utilized to enhance the out-of-band inhibition of the devices, the electrical performance of the microwave devices can be improved, and the electronic devices can be miniaturized.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of a multilayer heterogeneous ceramic high-temperature co-fired L C filter, in the method, through adjusting raw materials and a preparation process, the problem of multilayer heterogeneous ceramic co-fired junction matching can be solved, and the filter can be further miniaturized.
The second purpose of the invention is to provide a multilayer heterogeneous ceramic high-temperature co-fired L C filter, which is prepared by the method of the invention, and the filter has high dielectric constant and magnetic conductivity, and small volume, and can effectively improve the integration level of products.
The third purpose of the invention is to provide a device or a device of a multilayer heterogeneous ceramic high-temperature co-fired L C filter.
The preparation method of the multilayer heterogeneous ceramic high-temperature co-fired L C filter comprises the following steps:
(a) preparing a microwave dielectric ceramic green ceramic tape and a microwave ferrite green ceramic tape which have the same sintering temperature and horizontal shrinkage rate;
(b) punching a hole on the raw porcelain tape, and then filling the hole;
(c) printing a capacitor or an inductor on the green ceramic tape;
(d) carrying out lamination, hot isostatic pressing and hot cutting on the green ceramic tape to obtain a multilayer heterogeneous ceramic high-temperature co-fired L C filter green blank;
(e) sintering and post-treating the multilayer heterogeneous ceramic high-temperature co-fired L C filter raw blank to obtain a finished product;
preferably, the post-treatment comprises chamfering, end coating, silver burning, electroplating and detection.
Optionally, in the present invention, step (a)) In the microwave dielectric ceramic, M is2SiO2System, magnesium calcium titanate system, zinc niobate system, ATiO3-LnAlO3A ceramic of the barium or barium titanium system;
wherein M is Zn and/or Mg, A is Ca, Sr or Ba, L n is rare earth element;
preferably, the dielectric constant of the microwave dielectric ceramic is 5-130;
and/or the microwave ferrite material is one or more complex ferrite materials of Mn-Zn, Ni-Zn or Cu-Zn.
Optionally, in the invention, in the step (a), the sintering temperatures of the obtained microwave dielectric ceramic green tape and the microwave ferrite material green tape are matched by adjusting the raw material formula, adding an auxiliary agent and adjusting the particle size of the raw material;
preferably, the auxiliary agent is one or a mixture of more of zinc borosilicate glass powder, silicon dioxide, boron trioxide, bismuth trioxide, niobium pentoxide and zinc oxide, or calcium oxide.
Optionally, in the present invention, in step (a), the microwave dielectric ceramic green tape and the microwave ferrite green tape are prepared by tape casting, and the horizontal shrinkage rates of the microwave dielectric ceramic green tape and the microwave ferrite green tape are matched by controlling the tape casting process parameters;
preferably, the sizes of the microwave dielectric ceramic green ceramic tape and the microwave ferrite green ceramic tape are 4-8 inches.
Optionally, in the present invention, the slurry used for filling the hole in step (b) is silver palladium metal slurry; preferably, the mass ratio of the silver to the palladium in the slurry is 30: 70-80: 20; preferably, the solids content of the slurry is 88. + -.5%.
Optionally, in the present invention, in step (c), a capacitor is printed on the microwave dielectric ceramic green tape, and an inductor is printed on the microwave ferrite material; preferably, the metal slurry used for printing is silver palladium slurry; more preferably, the solid content of the slurry is 50-60%; further preferably, the mass ratio of silver to palladium in the silver-palladium slurry is 30: 70-80: 20.
Optionally, in the invention, the sintering in the step (d) includes the following steps, firstly, heating from room temperature to 600 ℃, wherein the heating speed is less than or equal to 0.5 ℃/min; then, the temperature is raised from 600 ℃ to 1100-1400 ℃, the temperature raising speed is 0.5-3 ℃/min, and the temperature is kept for 1-5 h at the temperature.
Meanwhile, the invention also provides a multilayer heterogeneous ceramic high-temperature co-fired L C filter prepared by the method.
Optionally, in the present invention, the inductance layer of the multilayer heterogeneous ceramic high-temperature co-fired L C filter is microwave ferrite ceramic, and the capacitance layer is microwave dielectric ceramic;
preferably, the structure of the multilayer heterogeneous ceramic high-temperature co-fired L C filter is a sandwich structure with an upper microwave dielectric ceramic layer and a lower microwave dielectric ceramic layer and a middle microwave ferrite layer.
Likewise, the invention also provides a device or a device comprising the multilayer heterogeneous ceramic high-temperature co-fired L C filter.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention solves the problem of high-temperature co-firing matching of multilayer microwave dielectric ceramics, microwave ferrite materials and silver-palladium slurry, and various defects of heterogeneous ceramics are caused in the co-firing process because the three materials are generally difficult to match in performance parameters such as sintering temperature, shrinkage rate, thermal expansion coefficient and the like. The invention well solves the problems of macroscopic warping layering, micro-cracks, defects and the like, realizes the high-temperature co-firing of the multilayer heterogeneous material, and provides a new material foundation for microwave components and assemblies with multilayer structures.
(2) Compared with the existing homogeneous L TCC or HTCC ceramics, the invention uses the silver-palladium metal with high conductivity and high-temperature sintering resistance as a conductor material, and has the advantages of L TCC and HTCC.
(3) Compared with the L C filter co-fired by multilayer homogeneous ceramics, the microwave dielectric ceramics of the multilayer heterogeneous ceramics L C filter has higher dielectric constant, the magnetic conductivity of the ferrite material is also very high, the product volume can be greatly reduced, and the foundation is laid for further improving the integration level of the existing multilayer co-fired ceramic product.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a simulation structure diagram of a L C filter made of K25 homogeneous microwave dielectric ceramic;
FIG. 3 is a simulation structure diagram of a L C filter prepared by using K25 and a ferrite heterogeneous material;
FIG. 4 is a drawing of a K25 and ferrite multilayer alloplastic ceramic tape laminate after hot isostatic pressing;
FIG. 5 is a graph of the performance of the K25 and ferrite high temperature co-fired L C filter test of the present invention;
FIG. 6 is a diagram of the performance of the K38 and ferrite high temperature co-fired L C filter test.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. 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.
In the invention, the problem of co-sintering matching of multilayer heterogeneous ceramics is solved by adopting measures of adding a low-temperature sintering aid, adjusting the particle size of raw materials, designing a casting material formula and casting parameters, improving a sintering process system and the like; meanwhile, the size of the filter is further miniaturized by embedding a capacitor in the microwave dielectric layer, embedding an inductor in the microwave ferrite material and the like.
Specifically, the preparation method of the filter of the present invention can refer to the following steps:
(a) the simulation design of the multilayer alloplasm ceramic L C filter comprises designing a multilayer alloplasm ceramic high-temperature co-fired filter according to the simulation of L C filter indexes, wherein, in order to reduce the volume and obtain large inductance, an inductance layer part adopts ferrite magnetic materials, and a capacitance part adopts dielectric materials with high dielectric constants;
preferably, the filter has a sandwich structure (sandwich structure) with an upper microwave dielectric ceramic layer and a lower microwave dielectric ceramic layer, and a middle microwave ferrite layer.
(b) Preparing a microwave dielectric ceramic green porcelain tape: the microwave dielectric ceramic material is prepared by adopting a traditional solid phase method, wherein the microwave dielectric ceramic contains M2SiO2System (M is Zn, Mg), magnesium calcium titanate system, zinc niobate system, ATO3-LnAlO3A system (A is Ca, Sr or Ba; L n is L a, Nd, Sm and other rare earths) or barium titanium system, etc.;
then, mixing the prepared microwave dielectric ceramic material with an auxiliary agent, grinding to obtain mixed powder, and controlling the grinding speed and the grinding time to regulate and control the average particle size of the mixed powder; the sintering characteristics of the microwave dielectric ceramic such as sintering temperature, shrinkage rate, expansion coefficient and the like can be regulated and controlled by adjusting the raw material formula of the microwave dielectric ceramic, adding a liquid-phase sintering aid, changing the average particle size of the raw materials by grinding and the like;
the auxiliary agent comprises zinc borosilicate glass powder, silicon dioxide, boron trioxide, bismuth trioxide, niobium pentoxide, zinc oxide, calcium oxide or the like;
then, blending parameters such as a resin formula, solid content, viscosity, rheological property and the like of the ceramic tape casting material with the mixed powder according to a conventional tape casting process to prepare tape casting slurry, then performing tape casting to obtain a green porcelain tape, and controlling the shrinkage rate of the tape casting green porcelain tape in the X, Y direction and the thickness of the green porcelain tape in the Z direction in the sintering process by controlling parameters such as the speed, a temperature zone, the height of a knife edge and the like in the tape casting process;
the green tape may be 4 inches, 6 inches, or 8 inches in size.
(c) Preparing a microwave ferrite green porcelain tape: the microwave ferrite material is prepared by adopting a traditional solid phase method, preferably, the microwave ferrite material comprises one or more composite system ferrite materials of Mn-Zn, Ni-Zn or Cu-Zn, and the like;
then, mixing the microwave ferrite material with an auxiliary agent and then grinding to obtain mixed powder; meanwhile, by adjusting the raw material formula of the ferrite material, adding a liquid-phase sintering aid, changing the average particle size of the raw material and other methods, the sintering temperature of the microwave ferrite (namely the sintering temperature of the microwave ferrite ceramic sintered from the microwave ferrite green tape) can be matched with (the temperature is the same as or equal to) the sintering temperature of the microwave dielectric ceramic (namely the sintering temperature of the microwave dielectric ceramic sintered from the microwave dielectric ceramic green tape), and the shrinkage rate and the expansion coefficient are matched with (the shrinkage rate and the expansion coefficient are the same as or equal to) the microwave dielectric ceramic;
the auxiliary agent comprises zinc borosilicate glass powder, silicon dioxide, diboron trioxide, bismuth trioxide or calcium oxide and the like;
then, according to the conventional casting operation steps, parameters such as a resin formula, solid content, viscosity, rheological property and the like of the ceramic casting material are prepared to prepare casting slurry of the microwave ferrite material; meanwhile, parameters such as speed, temperature zone, knife edge height and the like in the tape casting process are controlled, so that the shrinkage rate of the tape-cast green porcelain in the X, Y direction is matched with (is consistent with or equal to) microwave dielectric ceramics, and the thickness in the Z direction is controlled;
the green tape may be 4 inches, 6 inches, or 8 inches in size.
(d) Punching and filling holes: punching holes on a preset position belt of the raw porcelain by laser or a mechanical mode, and filling silver-palladium metal slurry into the holes through a wire mesh or a steel plate mesh to determine the communication of inner leads and good heat dissipation performance;
the solid content of the silver-palladium slurry is 88 +/-5%, and the mass ratio of silver to palladium in the slurry is 30: 70-80: 20.
(e) Screen printing: regulating and controlling a silk screen printing number process, namely respectively silk-screening preset metal conductor wiring on two kinds of raw porcelain strips, printing a built-in capacitor on the microwave dielectric ceramic raw porcelain strip, and printing a built-in inductor on a microwave ferrite material;
wherein the solid content of the silver palladium slurry is 50-60%.
(f) Lamination and hot isostatic pressing: carrying out accurate alignment lamination on the silk-screen green porcelain tapes according to a pre-designed sequence and layer number, wherein the alignment accuracy requirement is less than +/-10 mu m;
and then, keeping the pressure for 0.3-2 h under the conditions of 100-200 MPa and 40-80 ℃ by using a hot isostatic pressing technology to perform hot isostatic pressing forming, so that the filter blank is densified, the shrinkage rate of the L C filter blank is consistent when the L C filter blank is densified and sintered, and a multilayer L C filter blank is formed.
(g) And (4) hot cutting, namely cutting the multilayer L C filter green body to separate the single L C filter green body.
(h) L C filter high temperature cofiring, namely in a high temperature box type sintering furnace, carrying out binder removal and sintering on the cut L C filter green body;
wherein the temperature rise curve of sintering is that the room temperature is raised to 600 ℃, the sintering belongs to the glue discharging process before 600 ℃, and the temperature rise rate needs to be less than or equal to 0.5 ℃/min; then, the temperature is raised from 600 ℃ to 1100-1400 ℃ (peak temperature T)maxTemperature adjustment can be carried out within the range according to the formula of the raw porcelain strip), the temperature rising speed is 0.5-3 ℃/min, and the heat is preserved for 1-5 h at the peak temperature;
through high-temperature co-sintering, internal stress can be uniformly released, micro defects at a ceramic composite interface are reduced or inhibited, and a matched co-sintered body is obtained.
The method comprises the following steps of end coating, electroplating, leading out an outer electrode, electroplating a tin-lead protective layer, increasing the weldability, detecting, testing the electrical property and judging whether the size and the appearance are qualified, and the preparation method of the multilayer heterogeneous high-temperature co-fired ceramic L C filter comprises the following specific steps:
(i) chamfering: removing burrs and impurity particles on the surface after sintering, so that the surface of the product is smooth and the inner electrode is fully exposed.
(j) End coating and electroplating: end coating is carried out by adopting silver paste, an outer electrode is led out, and the sintering temperature is 600-800 ℃; tin and lead are electroplated as a protective layer to enhance solderability.
(k) And (3) detection, namely performing electrical property test and detection and screening of the appearance size on the prepared multilayer heterogeneous high-temperature co-fired ceramic L C filter.
The multilayer heterogeneous high-temperature co-fired ceramic L C filter prepared by the method not only has higher dielectric constant and magnetic conductivity, but also can effectively realize the miniaturization of the filter, reduce the weight and volume of the filter and improve the integration level.
Furthermore, the filter can be further applied to microwave electronic components or corresponding equipment, such as related electronic equipment in the wireless communication fields of global positioning systems, wireless local area networks in the automobile field, aerospace and the like.
EXAMPLE 1 preparation of multilayer high temperature co-fired L C Filter of microwave dielectric ceramic (K25) having dielectric constant of 25 and Ni-Zn-Fe ferrite
A K25 microwave dielectric ceramic and Ni-Zn-Fe ferrite multilayer high-temperature co-fired L C filter is prepared according to the flow shown in figure 1, and the technical indexes of the K25 microwave dielectric ceramic and Ni-Zn-Fe ferrite multilayer high-temperature co-fired L C filter are as follows, wherein the pass band frequency (GHz) is (3.94-5.5), the insertion loss (dB) is less than or equal to 4.5, the in-band fluctuation (dB) is less than or equal to 1.5, the out-of-band inhibition is more than or equal to 45dB @ f (f is less than or equal to 2.75GHz and f is more than or equal to 6.34GHz), the input and output standing wave is less than or equal to 1.5:
(a) the simulation design of the multilayer heterogeneous ceramic L C filter adopts a sandwich structure with an upper microwave dielectric layer and a lower microwave dielectric layer and a microwave ferrite layer in the middle, wherein the inductance layer part adopts a Ni-Zn-Fe ferrite magnetic material, the magnetic conductivity of the material is 300, the capacitance part adopts a K25 microwave dielectric ceramic material, and the simulation structure of the product is shown in figure 2.
(b) Preparing a microwave dielectric ceramic green porcelain tape: the main formula is Ca prepared by adopting the traditional solid phase methodxMgyLa2z/3TiO3The K25 microwave dielectric ceramic material is characterized in that x + y + z is 1, x is more than or equal to 0.07 and less than or equal to 0.15, x is more than or equal to 00.81 and less than or equal to 0.95, and x is more than or equal to 00.02 and less than or equal to 0.15;
adding 0.1-0.5 wt% of liquid-phase sintering aid silicon dioxide into the microwave dielectric ceramic material, then sanding (35Hz for 20-40 min) the mixed powder to change the average particle size of the raw material, adjusting the average particle size to 0.5-1 mu m, and enabling the sintering temperature to be 1220-1250 ℃.
Then, the rheological properties such as the viscosity of the casting material and the like and casting parameters are regulated and controlled, the shrinkage rate of the green tape in the X, Y direction is controlled, and the thickness of the obtained casting green tape is 72 mu m.
(c) Preparing a microwave ferrite green porcelain tape: preparing Fe-Zn-Ni microwave ferrite material by adopting a traditional solid phase method, and blending an original formula by using Ni/Zn/Fe according to a molar ratio of (0.04-0.39) to (0.09-0.27) to (0.47-0.65);
then adding 0.2-0.7 wt% of sintering aid Bi2O3And then, changing the average grain size of the raw materials by sanding (40Hz, 30 min-60 min), and enabling the average grain size to reach 0.3-0.8 mu m, so that the final sintering temperature of the ferrite material is basically consistent with the sintering temperature of K25 ceramic. Wherein the magnetic conductivity of the Fe-Zn-Ni microwave ferrite material is 300.
And regulating and controlling rheological properties such as viscosity and the like and casting parameters of the casting material to ensure that the shrinkage rate of the microwave ferrite green tape in the X, Y direction is consistent with that of the microwave dielectric ceramic, and the thickness of the casting green tape is 45 mu m.
(d) Punching and filling holes: punching holes on the punched green porcelain tape by laser, and pouring silver-palladium slurry, wherein the solid content of the slurry is 88 +/-5%, and the mass ratio of silver to palladium in the slurry is 60: 40.
(e) Screen printing: and adjusting and controlling a screen printing number process, and screen printing preset metal conductor wires on two raw porcelain tapes, wherein the metal slurry is silver palladium slurry with the solid content of 50-60%, and the mass ratio of silver to palladium of the slurry is 60: 40.
(f) Lamination and hot isostatic pressing: aligning and laminating the silk-screen green ceramic tapes according to a pre-designed sequence and layer number, keeping the pressure for 0.5h under the conditions that the pressure is 100 MPa-200 MPa and the temperature is 40-80 ℃, and carrying out hot isostatic pressing forming to obtain a multilayer heterogeneous material substrate blank body, wherein the uppermost layer is provided with a parting line as shown in figure 4.
(g) And cutting, namely cutting the multilayer substrate blank according to the cutting lines to separate the single L C filter green bodies.
(h) And (3) high-temperature co-firing the L C filter, namely, carrying out glue removal and sintering on the cut L C filter green body in a high-temperature box type sintering furnace, wherein the heat is preserved for 5 hours at 600 ℃ for glue removal, the temperature is raised to 1220-1250 ℃ at the speed of 0.5-3 ℃/min, and the heat is preserved for 3 hours.
(i) Chamfering: removing the burrs and impurity particles on the surface after sintering, and ensuring that the surface of the product is smooth and the inner electrode is fully exposed.
(j) End coating and electroplating: silver paste is adopted for end coating, and the sintering temperature is 600-800 ℃. Tin and lead are electroplated as a protective layer to enhance solderability.
(k) And (3) detecting, namely, carrying out electrical property test and detection and screening of the appearance size on the prepared multilayer heterogeneous high-temperature co-fired ceramic L C filter, wherein the electrical property test result is shown in figure 5, and the technical index requirement is met.
Compared with the homogeneous K25 microwave dielectric ceramic, the simulated structure is shown in FIG. 3, and the size of the product is 3216 (metric, 3.2 × 1.6 mm).
Therefore, if a L C filter with the same technical indexes as those of the L C filter prepared in the embodiment 1 is prepared by taking the homogeneous K25 microwave ceramic as a raw material, the simulation structure of the L C filter can reach 3.2 × 1.6.6 mm, which is far larger than the 1.6 × 0.8.8 mm size of the multi-layer heterogeneous high-temperature co-fired ceramic L C filter prepared by the method disclosed by the invention.
Example 2 preparation of multilayer high temperature co-fired L C Filter of microwave dielectric ceramic (K38) and ferrite with dielectric constant of 38
The filter index in the embodiment 2 is the same as the filter index L C in the embodiment 1, but the dielectric constant is increased and the sintering temperature is reduced due to the replacement of K25 with a barium-titanium series microwave dielectric ceramic layer (K38), and in order to enable the heterogeneous ceramic to be co-fired in a high-temperature matching way, the microwave ferrite material is adjusted to be Ni-Zn-Fe-Cu system, the size of the finally prepared filter can be further reduced to 1005(1 × 0.5mm), and the specific preparation steps refer to the following steps:
(a) the simulation design of the multilayer heterogeneous ceramic L C filter also adopts a sandwich structure of microwave dielectric ceramic sandwiched by microwave ferrites on two surfaces, wherein the inductance layer part adopts a Ni-Zn-Fe-Cu ferrite magnetic material, the magnetic conductivity of the magnetic material is set to be 300, and the capacitance part adopts a K38 microwave dielectric ceramic material.
(b) Preparing a microwave dielectric ceramic green porcelain tape: the main formula is Ba prepared by adopting the traditional solid phase methodxTiyO3The K38 microwave dielectric ceramic material, wherein y/x is 4-4.5;
adding 5-20 wt% of liquid-phase sintering aid ZnO and Nb into the prepared K38 microwave dielectric ceramic material2O51-6 wt%, and the mixed powder is modified by sanding (35Hz, 30-60 min)Changing the average grain size of the raw materials to 0.4-0.9 μm, and ensuring that the sintering temperature is 1140-1180 ℃. And regulating and controlling rheological properties such as viscosity and the like and casting parameters of the casting material, and controlling the shrinkage rate of the green tape in the X, Y direction, wherein the thickness of the cast green tape is 53 mu m.
(c) Preparing a microwave ferrite green porcelain tape: the method comprises the steps of preparing a Ni-Zn-Fe-Cu ferrite material by a traditional solid phase method, blending an original formula by Ni/Zn/Fe/Cu according to a molar ratio of (0.04-0.31), (0.09-0.23), (0.41-0.63) and (0.03-0.10), adding 0.3-0.6 wt% of a sintering aid CaO, changing the average particle size of raw materials by sanding (40Hz, 40 min-60 min), wherein the average particle size reaches 0.3-0.7 mu m, and the final sintering temperature of the ferrite material is basically consistent with the sintering temperature of K38 ceramic. Wherein the magnetic permeability of the Ni-Zn-Fe-Cu ferrite material is 300. And regulating and controlling rheological properties such as viscosity and the like and casting parameters of the casting material to ensure that the shrinkage rate of the microwave ferrite green tape in the X, Y direction is consistent with that of the microwave dielectric ceramic, and the thickness of the casting green tape is 35 mu m.
(d) Punching and filling holes: punching holes on the punched green porcelain tape by laser, and pouring silver-palladium slurry, wherein the solid content of the slurry is 88 +/-5%, and the mass ratio of silver to palladium in the slurry is 70: 30.
(e) Screen printing: and adjusting and controlling a screen printing number process, and screen printing preset metal conductor wires on two raw porcelain tapes, wherein the metal slurry is silver palladium slurry with the solid content of 50-60%, and the mass ratio of silver to palladium of the slurry is 70: 30.
(f) Lamination and hot isostatic pressing: aligning and laminating the silk-screen green ceramic tapes according to a pre-designed sequence and layers, maintaining the pressure for 1h under the conditions that the pressure is 100-200 MPa and the temperature is 40-80 ℃, and carrying out hot isostatic pressing molding.
(g) And cutting, namely cutting the multilayer substrate blank to separate the single L C filter green bodies.
(h) And (3) co-firing the L C filter at a high temperature, namely, carrying out glue removal and sintering on the cut L C filter green body in a high-temperature box type sintering furnace, wherein the temperature is kept at 600 ℃ for 5 hours, the glue removal is carried out, the temperature is increased to 1140-1180 ℃ at the speed of 0.5-3 ℃/min, and the temperature is kept for 4 hours.
(i) Chamfering: removing the burrs and impurity particles on the surface after sintering, and ensuring that the surface of the product is smooth and the inner electrode is fully exposed.
(j) End coating: silver paste is adopted for end coating, and the sintering temperature is 600-800 ℃. Tin and lead are electroplated as a protective layer to enhance solderability.
(k) And (3) detecting, namely, carrying out electrical property test and detection and screening of the appearance size on the prepared multilayer heterogeneous high-temperature co-fired ceramic L C filter, wherein the test result is shown in figure 6, and the technical index requirement is met.
From the experimental results of the embodiment 1 and the embodiment 2, it can be seen that compared with the L C filter made of the homogeneous material, the size of the multi-layer heterogeneous material high-temperature co-fired L C filter can be reduced to 1/2-1/3, and the volume thereof can be reduced to 1/8-1/20, so that the weight and the manufacturing cost of the product are both greatly reduced.
Further comparing the two examples, it can be seen that the dielectric constant of the microwave dielectric ceramic in example 2 becomes larger, therefore, the size of the filter formed by co-firing the K38 microwave dielectric ceramic and the ferrite at high temperature L C can be further reduced under the same index, and the electrical properties of the product are not greatly different.
The foregoing is a further detailed description of the invention in connection with preferred embodiments and is not intended to limit the invention to the precise form disclosed. It will be understood by those skilled in the art that various changes in detail may be effected therein without departing from the scope of the invention as defined by the appended claims.
Claims (3)
1. The preparation method of the multilayer heterogeneous ceramic high-temperature co-fired L C filter is characterized by comprising the following steps:
(a) preparing a microwave dielectric ceramic green porcelain tape and a microwave ferrite green porcelain tape with equivalent sintering temperature and horizontal shrinkage rate, wherein the microwave dielectric ceramic is a barium-titanium system K38 microwave dielectric ceramic, the microwave ferrite is a Ni-Zn-Fe-Cu system,
the main formula is Ba prepared by adopting a solid phase methodxTiyO3The K38 microwave dielectric ceramic material, wherein y/x is 4-4.5; in the preparation of5-20 wt% of liquid-phase sintering aid ZnO and Nb are added into the K38 microwave dielectric ceramic material2O51-6 wt%, sanding the mixed powder to enable the average particle size to reach 0.4-0.9 μm, and enabling the sintering temperature of the mixed powder to be 1140-1180 ℃, wherein the sanding frequency is 35Hz, and the sanding time is 30-60 min;
preparing a Ni-Zn-Fe-Cu ferrite material by a solid phase method, blending an original formula by Ni/Zn/Fe/Cu according to the mol ratio of (0.04-0.31) to (0.09-0.23) to (0.41-0.63) to (0.03-0.10), adding 0.3-0.6 wt% of a sintering aid CaO, changing the average particle size of the raw material by sanding to reach 0.3-0.7 mu m, and enabling the final sintering temperature of the ferrite material to be basically consistent with the sintering temperature of K38 ceramic, wherein the sanding frequency is 40Hz and the time is 40-60 min; wherein the magnetic permeability of the Ni-Zn-Fe-Cu ferrite material is 300;
(b) punching holes on the green porcelain tape, filling the holes,
punching holes on the punched green porcelain tape by laser, and pouring silver-palladium slurry, wherein the solid content of the slurry is 88 +/-5%, and the mass ratio of silver to palladium in the slurry is 70: 30;
(c) a capacitor or an inductor is printed on the green tape,
the printing method comprises the following steps of (1) printing, wherein metal slurry is silver palladium slurry, the solid content of the metal slurry is 50-60%, and the mass ratio of silver to palladium in the slurry is 70: 30;
the inductor adopts a Ni-Zn-Fe-Cu ferrite magnetic material, and the magnetic conductivity is set to be 300; the capacitor is made of K38 microwave dielectric ceramic material;
(d) the green ceramic tape is laminated, hot isostatic pressed and hot cut to obtain a multilayer heterogeneous ceramic high-temperature co-fired L C filter green blank,
wherein, the lamination layer adopts a sandwich structure of microwave dielectric ceramic with microwave ferrite on two surfaces;
keeping the pressure for 1h under the conditions that the pressure is 100-200 MPa and the temperature is 40-80 ℃, and carrying out hot isostatic pressing;
(e) sintering and post-treating the multilayer heterogeneous ceramic high-temperature co-fired L C filter raw blank to obtain a finished product;
the sintering in the step (d) comprises the following steps of firstly heating from room temperature to 600 ℃, wherein the heating speed is less than or equal to 0.5 ℃/min; then, heating from 600 ℃ to 1100-1400 ℃, wherein the heating speed is 0.5-3 ℃/min, and keeping the temperature for 1-5 h;
and the post-treatment comprises chamfering, end coating, silver burning, electroplating and detection.
2. The preparation method according to claim 1, wherein in the step (a), the microwave dielectric ceramic green tape and the microwave ferrite green tape are prepared by a tape casting method, and the horizontal shrinkage rates of the microwave dielectric ceramic green tape and the microwave ferrite green tape are matched by controlling the tape casting process parameters;
the sizes of the microwave dielectric ceramic green ceramic tape and the microwave ferrite green ceramic tape are 4-8 inches.
3. The multilayer heterogeneous ceramic high temperature co-fired L C filter prepared according to the method of claim 1 or 2.
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| CN108759941A (en) * | 2018-05-28 | 2018-11-06 | 深圳研勤达科技有限公司 | A kind of small-bore measurement by capacitance conduit and preparation method thereof |
| CN110211930A (en) * | 2019-05-29 | 2019-09-06 | 中国电子科技集团公司第三十八研究所 | A kind of substrate with heterosphere structure, preparation method and application |
| CN114804858B (en) * | 2021-01-28 | 2023-07-04 | 山东国瓷功能材料股份有限公司 | Low-temperature co-fired ceramic material for filter and preparation method and application thereof |
| CN113061024B (en) * | 2021-04-08 | 2022-08-26 | 山东国瓷功能材料股份有限公司 | Low-temperature co-fired material and prepared green ceramic chip and device for overcurrent protection |
| CN113372103B (en) * | 2021-07-13 | 2023-01-20 | 中国振华集团云科电子有限公司 | Low-dielectric low-high-frequency-loss LTCC ceramic material and preparation method thereof |
| CN113573484B (en) * | 2021-09-23 | 2022-03-25 | 西安宏星电子浆料科技股份有限公司 | Small-batch rapid manufacturing method for LTCC (Low temperature Co-fired ceramic) substrates |
| CN114105625A (en) * | 2021-10-25 | 2022-03-01 | 北京无线电测量研究所 | Preparation method and application of ferrite-ceramic heterogeneous co-fired material |
| CN115626820B (en) * | 2022-11-02 | 2023-10-31 | 西南科技大学 | Preparation method of heterogeneous laminated cofired ferrite ceramic |
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