CN106995312A - Heterogeneous multi-layer ceramic high temperature burns the preparation method of LC wave filters altogether - Google Patents
Heterogeneous multi-layer ceramic high temperature burns the preparation method of LC wave filters altogether Download PDFInfo
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- CN106995312A CN106995312A CN201710305323.5A CN201710305323A CN106995312A CN 106995312 A CN106995312 A CN 106995312A CN 201710305323 A CN201710305323 A CN 201710305323A CN 106995312 A CN106995312 A CN 106995312A
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- microwave
- high temperature
- green band
- wave filters
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 52
- 238000005245 sintering Methods 0.000 claims description 45
- 239000002002 slurry Substances 0.000 claims description 33
- 229910052763 palladium Inorganic materials 0.000 claims description 26
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 15
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- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 4
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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 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
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- RPEUFVJJAJYJSS-UHFFFAOYSA-N zinc;oxido(dioxo)niobium Chemical compound [Zn+2].[O-][Nb](=O)=O.[O-][Nb](=O)=O RPEUFVJJAJYJSS-UHFFFAOYSA-N 0.000 claims description 3
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- 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 claims description 2
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- 238000010521 absorption reaction Methods 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- B28B1/00—Producing shaped prefabricated articles from the material
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Abstract
The invention provides the preparation method that heterogeneous multi-layer ceramic high temperature burns LC wave filters altogether.The inventive method is by designing the formula for raw stock of microwave ferrite material and microwave-medium ceramics and being cast material formula, and to curtain coating, the adjustment of co-firing technology, so as to effectively solve prior art LC wave filters using the microwave dielectric material of homogeneity for the heat dispersion caused by raw material and high frequency electricity degradation, the technical problem such as the product number of plies is excessive, volume is excessive, and realize that multi-layer sheet type LC filter product develops to subminaturization, lightweight, high frequency, high-quality direction, it is significant and market application foreground is good.
Description
Technical field
Field is manufactured the present invention relates to wave filter, LC wave filters are burnt altogether in particular to heterogeneous multi-layer ceramic high temperature
Preparation method.
Background technology
With the development of science and technology the field such as space flight and aviation is gradually stepped up to wireless communication technique requirement, and then for microwave
Integrated level, electrical property, volume, weight, the reliability of electronic component, and amplitude-phase consistency etc. it is also proposed higher requirement.
Multilayer co-firing ceramics (including low temperature and high temperature multilayer co-firing ceramics) turn into multi-chip with excellent electricity, machinery, thermodynamic property
The preferred material of component (MCM, Multi-Chip Module), MCM can be realized in the form of 3D (three-dimensional) multilayer circuit structure
Various small-power radio frequencies and microwave function module or even system it is highly integrated, with excellent high frequency characteristics, be widely used in boat
The fields such as empty space flight, radio communication.
At present, domestic existing many bar LTCC (LTCC, Low Temperature Co-fired
Ceramic) line of production technology, the material of use is mainly derived from 951 series of Dupont companies of the U.S., and (ceramic dielectric is normal
Number 7.8) and Ferro companies A6 serial (ceramic dielectric constant 5.9), the series material includes green band, series resistance
Slurry, serial gold paste, serial silver paste, packaging slurry etc., co-fired temperature is 850 DEG C, and green band is ceramic for the low dielectric microwave of homogeneity.
HTCC (HTCC, High Temperature Co-fired Ceramic) by sintering temperature due to not limited, ceramics
Substrate can using pure microwave ceramics phase without glass phase, dielectric constant than LTCC with glass ceramics big, loss angle tangent
The advantages of small, perfect heat-dissipating, high mechanical strength, compared to LTCC, the electrical properties of HTCC microwave products is more excellent, volume is smaller, but
The ceramic substrate material that current HTCC is used remains as single type, mainly there is aluminum oxide, aluminium nitride, silicon nitride etc..
The outer LC wave filters developed of Current Domestic also focus on LTCC wave filters, and material therefor is microwave-medium of the same race
Material or microwave ferrite material with gold and silver slurry by firing altogether, and its shortcoming is relatively low (the dielectric material magnetic conductivity of magnetic conductivity
1) or dielectric constant is relatively low (typically below 10) for, it is difficult to further be minimized to integrated component.And by higher dielectric
The microwave-medium ceramics of constant and the microwave ferrite of high magnetic permeability carry out high temperature co-firing with silver-colored palladium slurry, just can both utilize microwave
The good high frequency characteristics of dielectric ceramic, can strengthen the outer suppression of band of device using the precipitous absorption characteristic of Ferrite Material again
System, can not only improve the electrical property of microwave device, while it is also possible that electronic component is minimized.But, due to two
The sintering characteristics such as firing temperature, the shrinkage factor that kind heterogeneous functional layer and silver-colored palladium are starched are different, thus will altogether be burnt after its lamination, can produce
The common burning mismatch problems of material, and cause common Beijing enamel body the warpage of macroscopic level, cracking or microcosmic micro- occur between layers
The defects such as crackle, hole, have a strong impact on the Performance And Reliability of device.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide the preparation method that a kind of heterogeneous multi-layer ceramic high temperature burns LC wave filters altogether, institute
State in method, by the adjustment to raw material and preparation technology, can solve the problem that the ceramic co-fired knot matching problem of heterogeneous multi-layer, and cause
Wave filter further realizes miniaturization.
The second object of the present invention is that provide a kind of heterogeneous multi-layer ceramic high temperature burns LC wave filters altogether, and it is by present invention side
Method is prepared, and wave filter dielectric constant and magnetic conductivity of the present invention are high, while small volume, can effectively improve the integrated of product
Degree.
The third object of the present invention is to provide device or device that a kind of heterogeneous multi-layer ceramic high temperature burns LC wave filters altogether.
Heterogeneous multi-layer ceramic high temperature burns the preparation method of LC wave filters altogether, and the preparation method comprises the following steps:
(a) sintering temperature the microwave-medium ceramics green band and microwave ferrite green suitable with horizontal shrinkage factor are prepared
Band;
(b) punched on green band, then filling perforation;
(c) print capacitor or inductance on green band;
(d) green band is obtained into heterogeneous multi-layer ceramic high temperature through lamination, high temperature insostatic pressing (HIP) and thermal cutting and burns the life of LC wave filters altogether
Blank;
(e) by heterogeneous multi-layer ceramic high temperature burn altogether LC wave filter green billets it is sintered and post processing, obtain finished product;
It is preferred that, the post processing includes chamfering, end painting, silver ink firing, plating and detection.
Optionally, in the present invention, in step (a), microwave-medium ceramics are M2SiO2System, magnesium titanate calcium system, zinc niobate
System, ATiO3-LnAlO3System or barium titanium system ceramics;
Wherein, M is Zn and/or Mg, A are Ca, Sr or Ba;Ln is rare earth element;
It is preferred that, the dielectric constant of microwave-medium ceramics is 5~130;
And/or, microwave ferrite material is Mn-Zn, Ni-Zn or Cu-Zn one or more of compound system ferrite materials
Material.
Optionally, in the present invention, by adjusting composition of raw materials, addition auxiliary agent and regulation raw material particle size in step (a) so that
The microwave-medium ceramics green band of gained and the sintering temperature of microwave ferrite material green band match;
It is preferred that, the auxiliary agent is zinc borosilicate glass powder, silica, diboron trioxide, bismuth oxide, five oxidations two
One or more of mixtures in niobium, zinc oxide, or calcium oxide.
Optionally, in the present invention, in step (a), microwave-medium ceramics green band and microwave iron oxygen are prepared with the tape casting
Body green band, and by controlling the technological parameter of curtain coating so that microwave-medium ceramics green band and microwave ferrite green band
Horizontal shrinkage factor match;
It is preferred that, the size of microwave-medium ceramics green band and microwave ferrite green band is 4~8 inches.
Optionally, in the present invention, filling perforation slurry therewith is silver-colored palladium metal slurry in step (b);It is preferred that, in slurry silver and
The mass ratio of palladium is 30:70~80:20;It is preferred that, the solid content of slurry is 88 ± 5%.
Optionally, in the present invention, in step (c), the print capacitor on microwave-medium ceramics green band, microwave ferrite material
Printed inductance on material;It is preferred that, printing metal paste used is silver-colored palladium slurry;It is furthermore preferred that slurry solid content 50%~60%;
It is further preferred that silver-colored palladium quality is than scope 30 in silver-colored palladium slurry:70~80:20.
Optionally, in the present invention, sintering comprises the following steps described in step (d), first by room temperature to 600 DEG C,
Programming rate≤0.5 DEG C/min;Then, 1100~1400 DEG C are warming up to by 600 DEG C, programming rate is 0.5~3 DEG C/min, and
1~5h is incubated at such a temperature.
Meanwhile, LC filtering is burnt altogether present invention also offers the heterogeneous multi-layer ceramic high temperature as made from the method for the invention
Device.
Optionally, in the present invention, the inductor layer that the heterogeneous multi-layer ceramic high temperature burns LC wave filters altogether is microwave ferrite
Ceramics, capacitor layers are microwave-medium ceramics;
It is preferred that, it is microwave-medium ceramics that the heterogeneous multi-layer ceramic high temperature burns the structure of LC wave filters for two layers up and down altogether
Layer, centre is the sandwich structure of microwave ferrite layer.
Likewise, present invention provides the device or device for burning LC wave filters altogether comprising heterogeneous multi-layer ceramic high temperature of the present invention
Part.
Compared with prior art, beneficial effects of the present invention are:
(1) present invention solves multiplayer microwave media ceramic, microwave ferrite material and matched with the high temperature co-firing of silver-colored palladium slurry
Problem, because these three materials typically are difficult to match in the performance parameters such as sintering temperature, shrinkage factor and thermal coefficient of expansion, because
And generally cause heterogeneous ceramics to occur various defects during common burning.The present invention solves macroscopical warpage layering well, micro-
The problems such as seeing crackle and defect, realizes the high temperature co-firing of heterogeneous multi-layer material, is the microwave device and component of sandwich construction
There is provided new material foundation.
(2) it is of the invention with existing homogeneity LTCC or HTCC ceramic phases ratio, the silver for having used high conductivity, high temperature resistant to sinter
Palladium metal has LTCC and HTCC advantage concurrently as conductor material.
(3) compared with the ceramic co-fired LC wave filters of multilayer homogeneity, the microwave of heterogeneous multi-layer ceramics LC wave filters of the present invention
Media ceramic has higher dielectric constant, and the magnetic conductivity of Ferrite Material is also very high, and small product size can significantly reduce, and be existing
The further raising of some multilayer co-firing ceramic product integrated levels lays the foundation.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described.
Fig. 1 is process chart of the invention;
Fig. 2 is to prepare LC wave filter simulation architecture figures using K25 homogeneities microwave-medium ceramics;
Fig. 3 is using K25 and ferrite dissimilar materials preparation LC wave filter simulation architecture figures;
Fig. 4 is K25 of the present invention and ferrite multilayered heterogeneous green with the pictorial diagram after lamination and high temperature insostatic pressing (HIP);
Fig. 5 is K25 of the present invention and ferrite high temperature co-firing LC filters to test performance maps;
Fig. 6 is K38 of the present invention and ferrite high temperature co-firing LC filters to test performance maps.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, be
The conventional products that can be obtained by commercially available purchase.
In the present invention, by using addition low-temperature sintering auxiliary agent, adjustment raw material particle size, design curtain coating material formula and curtain coating
The measures such as parameter, improvement sintering process system, solve the ceramic co-fired knot matching problem of heterogeneous multi-layer;Meanwhile, by microwave
Dielectric layer built-in capacity, it is interior in microwave ferrite material to bury the modes such as inductance so that filter size is further minimized.
Specifically, the preparation method of wave filter of the present invention may be referred to it is as follows:
(a) design of Simulation of heterogeneous multi-layer ceramics LC wave filters:Made pottery according to LC Filter specification design of Simulation heterogeneous multi-layer
Porcelain high temperature co-firing wave filter, meanwhile, in order to reduce volume and obtain big inductance value, inductance layer segment uses ferrimagnetism material
Material, capacitive part uses the dielectric material of high-k;
It is preferred that, the structure of wave filter is microwave-medium ceramics layer two layers for above and below, and centre is the three of microwave ferrite layer
Mingzhi's structure (interlayer structure).
(b) prepared by microwave-medium ceramics green band:Microwave dielectric ceramic materials are prepared using conventional solid-state method, wherein, it is micro-
Ripple media ceramic includes M2SiO2It is (M is Zn, Mg), magnesium titanate calcium system, zinc niobate system, ATiO3-LnAlO3System (A is Ca,
Sr or Ba;Ln is La, Nd, the rare earth such as Sm) or barium titanium system etc.;
Then, ground after obtained microwave dielectric ceramic materials are mixed with auxiliary agent, obtain mixed powder, and pass through control
Grinding rate processed and milling time are to regulate and control the average grain diameter of mixed powder;And matched somebody with somebody by the raw material for adjusting microwave-medium ceramics
Side, addition liquid phase sintering, and the methods such as raw material average grain diameter are changed using grinding, microwave-medium ceramics can burnt
Regulated and controled on the sintering characteristics such as junction temperature, shrinkage factor and the coefficient of expansion;
The auxiliary agent includes zinc borosilicate glass powder, silica, diboron trioxide, bismuth oxide, niobium pentaoxide, oxygen
Change zinc, or calcium oxide etc.;
Then, the casting molding processes by mixed powder again routinely, allotment ceramics are cast the resin formula of material, contained admittedly
The parameters such as amount, viscosity, rheological behavior, prepare casting slurry, and then flow casting molding obtains green band, by controlling in casting technique
The parameter such as speed, warm area, edge height, green band X, contraction of Y-direction in sintering process of flow casting molding can be controlled
Rate and Z-direction green tape thickness;
The size of green band can be 4 inches, 6 inches or 8 inches.
(c) prepared by microwave ferrite green band:Microwave ferrite material is prepared using conventional solid-state method, it is preferred that microwave
Ferrite Material includes Mn-Zn, Ni-Zn or Cu-Zn one or more of compound system Ferrite Materials etc.;
Then, ground after microwave ferrite material is mixed with auxiliary agent, obtain mixed powder;Meanwhile, by adjusting iron oxygen
The methods such as formula for raw stock, addition liquid phase sintering, the change raw material average grain diameter of body material, can cause microwave ferrite
Sintering temperature (sintering temperature for sintering microwave ferrite ceramics into by microwave ferrite green band) and microwave-medium ceramics
Sintering temperature (sintering temperature for sintering microwave-medium ceramics into by microwave-medium ceramics green band) match that (temperature is identical
Or quite), shrinkage factor matches and (reached consistent or suitable) with the coefficient of expansion and microwave-medium ceramics;
The auxiliary agent includes zinc borosilicate glass powder, silica, diboron trioxide, bismuth oxide or calcium oxide etc.;
Then, operating procedure is cast according to conventional, the resin formula of allotment ceramics curtain coating material, solid content, viscosity, rheology are special
The parameters such as property, prepare the casting slurry of microwave ferrite material;Meanwhile, speed, warm area, edge height in control casting technique
Etc. parameter, green band X, Y-direction shrinkage factor and the microwave-medium ceramics of its flow casting molding are made to match and (reach consistent or suitable),
Z-direction thickness is controlled simultaneously;
The size of green band can be 4 inches, 6 inches or 8 inches.
(d) punching and filling perforation:Punched by laser or mechanical system on the predeterminated position band of green, and by silk screen or
Expanded metal lath pours into silver-colored palladium metal slurry in hole, determines inside conductor connection and good heat dispersion;
Wherein, the solid content of silver-colored palladium slurry used is that the mass ratio of silver and palladium in 88 ± 5%, slurry is 30:70~80:
20。
(e) silk-screen printing:Regulate and control silk screen printing technique, the metallic conductor cabling preset is distinguished into silk-screen to two kinds of greens
Take, and print on microwave-medium ceramics green band built-in inductance is printed on built-in capacitance, microwave ferrite material;
Wherein, the solid content of silver-colored palladium slurry used is 50%~60%.
(f) lamination and high temperature insostatic pressing (HIP):The good green band of silk-screen is carried out according to pre-designed order and the number of plies accurate
Lamination is aligned, the required precision of contraposition is less than ± 10 μm;
Then, using hot isostatic pressing technique under conditions of 100~200MPa and 40~80 DEG C, 0.3~2h of pressurize is carried out
Hip moulding, makes its densification, it is ensured that LC wave filter green compact are closely knit consistent with shrinkage factor when sintering, and form multilayer LC filtering
Device green.
(g) thermal cutting:Multi-layer LC filter green is cut, single LC wave filters green is separated.
(h) LC wave filters high temperature co-firing:Carried out in high-temperature box type sintering furnace, and to the LC wave filters green of well cutting
Dumping and sintering;
Wherein, the heating curve of sintering be room temperature to 600 DEG C, dumping process was belonged to before 600 DEG C, heating rate is needed
≤0.5℃/min;Then, 1100~1400 DEG C of (peak temperature T are warming up to by 600 DEG Cmax, can be according to green band formula as above
In the range of enter trip temperature adjustment), programming rate be 0.5~3 DEG C/min, and under peak temperature be incubated 1~5h;
Connect by high temperature co-firing, it can be ensured that uniformly discharge internal stress, reduce or suppression Ceramic Composite interface is microcosmic
The generation of defect, obtains the common burning body of matching.
End is applied, plating --- external electrode is drawn, electrotinning lead protection layer increases solderability;Detection --- electric performance test
And whether size appearance is qualified.The heterogeneous multi-layer HTCC LC wave filters that the present invention is provided prepare specific steps such as
Under:
(i) chamfering:Remove surface spikes, impurity particle after sintering so that product surface is smooth, interior electrode is fully exposed.
(j) end applies, electroplated:End painting is carried out using silver paste, external electrode is drawn, sintering temperature is at 600~800 DEG C;Electrotinning
Lead strengthens solderability as protective layer.
(k) detect:The heterogeneous multi-layer HTCC LC wave filters prepared are subjected to electric performance test and outward appearance chi
Very little detection and screening.
Not only there is higher dielectric constant as the heterogeneous multi-layer HTCC LC wave filters obtained by the above method
And magnetic conductivity, while also can effectively realize the miniaturization of wave filter, the weight and volume of wave filter is reduced, and improve integrated
Degree.
Further, the wave filter can also be further applied in microwave electron component or corresponding equipment, example
In such as global positioning system, automotive field WLAN, the associated electronic device of Aero-Space wireless communication field.
Embodiment 1:Dielectric constant is that 25 microwave-medium ceramics (K25) burn LC altogether with the ferritic multi-layer high-temperatures of Ni-Zn-Fe
It is prepared by wave filter
K25 microwave-medium ceramics and the ferrite multilayered high temperature co-firing LC filtering of Ni-Zn-Fe are prepared according to flow shown in Fig. 1
Device, technical requirement is as follows:Band connection frequency (GHz):(3.94-5.5);Insertion Loss (dB):≤4.5;Passband fluctuation (dB):≤
1.5;Out-of-band rejection:≥45dB@(f≤2.75GHz&f≥6.34GHz);Input and output standing wave:≤1.5.Wave filter is finally made
Size is 1608 (metric system, 1.6 × 0.8mm), and specific preparation process is as follows:
(a) design of Simulation of heterogeneous multi-layer ceramics LC wave filters:Use up and down two layers be microwave-medium layer, it is middle for microwave
The sandwich structure of ferrite layer.Wherein, inductance layer segment uses Ni-Zn-Fe ferrite magnetic materials, and its magnetic conductivity is 300,
Capacitive part uses K25 microwave dielectric ceramic materials, and product simulation structure is as shown in Figure 2.
(b) prepared by microwave-medium ceramics green band:Conventional solid-state method is used to prepare main formula for CaxMgyLa2z/3TiO3's
K25 microwave dielectric ceramic materials, wherein, x+y+z=1,0.07≤x≤0.15,00.81≤x≤0.95,00.02≤x≤
0.15;
Addition 0.1~0.5wt% liquid phase sintering silica is added in microwave dielectric ceramic materials, then mixed powder
Material is sanded (35Hz, 20min~40min) and changes raw material average grain diameter, and adjustment average grain diameter reaches 0.5~1 μm, makes it
Sintering temperature is at 1220~1250 DEG C.
Then, the rheological behavior such as viscosity of regulation and control curtain coating material and curtain coating parameter, the contraction of control green band in the x, y direction
Rate, gained curtain coating green tape thickness is 72 μm.
(c) prepared by microwave ferrite green band:Fe-Zn-Ni microwave ferrite materials are prepared using conventional solid-state method, passed through
Ni/Zn/Fe example (0.04~0.39) in molar ratio:(0.09~0.27):(0.47~0.65) original formulation allotment is carried out;
Then 0.2~0.7wt% sintering aid Bi is added2O3, then changed by the way that (40Hz, 30min~60min) is sanded
Become raw material average grain diameter, and cause average grain diameter to reach 0.3~0.8 μm, the final sintering temperature of Ferrite Material is made pottery with K25
Porcelain sintering temperature is basically identical.Wherein, Fe-Zn-Ni microwave ferrite materials magnetic conductivity is 300.
Regulate and control the rheological behaviors such as the viscosity of curtain coating material and curtain coating parameter, make microwave ferrite green with contraction in X, Y-direction
Rate is consistent with microwave-medium ceramics, and curtain coating green tape thickness is 45 μm.
(d) punching and filling perforation:Punched by laser on made green band, and pour into silver-colored palladium slurry, slurry solid content
For 88 ± 5%, the mass ratio of silver and palladium in slurry is 60:40.
(e) silk-screen printing:Regulate and control silk screen printing technique, the metallic conductor cabling preset is screen-printed to two kinds of greens
Take, wherein metal paste is starched for the silver-colored palladium of solid content 50~60%, slurry is 60 in the mass ratio of silver and palladium:40.
(f) lamination and high temperature insostatic pressing (HIP):The good green band of silk-screen is aligned according to pre-designed order and the number of plies
Lamination, is that 100MPa~200MPa, temperature are that under conditions of 40~80 DEG C, pressurize 0.5h carries out hip moulding in pressure,
Obtained heterogeneous multi-layer material substrate base substrate is as shown in figure 4, uppermost one layer with cutting line.
(g) cut:By cutting wire cutting multilager base plate base substrate, single LC wave filters green is set to be separated.
(h) LC wave filters high temperature co-firing:In high-temperature box type sintering furnace, the LC wave filter green to well cutting is arranged
Glue and sintering, wherein, it is incubated 5h at 600 DEG C and carries out dumping, 1220~1250 DEG C, guarantor is warming up to 0.5~3 DEG C/min speed
Warm 3h.
(i) chamfering:Surface spikes, impurity particle after sintering are removed, is that product surface is smooth, interior electrode is fully exposed.
(j) end applies, electroplated:End painting is carried out using silver paste, sintering temperature is at 600~800 DEG C.Plating tin-lead is used as protection
Layer, strengthens solderability.
(k) detect:The heterogeneous multi-layer HTCC LC wave filters prepared are subjected to electric performance test and outward appearance chi
Very little detection and screening, electric performance test result is as shown in figure 5, reach technical requirement.
Contrast is using the K25 microwave-medium ceramics of homogeneity, and its simulation architecture is as shown in figure 3, product size is 3216 (public
System, 3.2 × 1.6mm).
As can be seen here, if using homogeneity K25 microwave ceramics as the LC filters in the same manner as in Example 1 of material prepared technology index
Ripple device, the simulation architecture of the wave filter will reach 3.2 × 1.6mm, different much larger than according to the multilayer prepared by the inventive method
1.6 × 0.8mm of matter HTCC LC wave filters size.
Embodiment 2:Dielectric constant is that 38 microwave-medium ceramics (K38) burn LC wave filter systems altogether with ferritic multi-layer high-temperature
It is standby
The median filter index of embodiment 2 is identical with LC Filter specifications in embodiment 1.But due to having changed K25 into barium titaniums
The microwave-medium ceramics layer (K38) of system, dielectric constant increase and sintering temperature reduction, in order that obtaining heterogeneous ceramic high temperature matching altogether
Burn, microwave ferrite material is adjusted to Ni-Zn-Fe-Cu systems.Finally obtained filter size can be further reduced to
1005 (1 × 0.5mm), specific preparation process is with reference to as follows:
(a) design of Simulation of heterogeneous multi-layer ceramics LC wave filters:It is same to press from both sides microwave iron oxygen using two sides microwave-medium ceramics
The sandwich structure of body.Wherein, inductance layer segment uses Ni-Zn-Fe-Cu ferrite magnetic materials, and its magnetic conductivity is set to
300, capacitive part uses K38 microwave dielectric ceramic materials.
(b) prepared by microwave-medium ceramics green band:Conventional solid-state method is used to prepare main formula for BaxTiyO3K38 microwaves
Medium ceramic material, wherein, y/x=4~4.5;
Addition liquid phase sintering ZnO 5~20wt% and Nb are added in obtained K38 microwave dielectric ceramic materials2O51
~6wt%, (35Hz, 30min~60min) is sanded to mixed powder and changes raw material average grain diameter, average grain diameter reaches
0.4~0.9 μm, make its sintering temperature at 1140~1180 DEG C.The rheological behaviors such as the viscosity of regulation and control curtain coating material and curtain coating parameter, control
The shrinkage factor of green band processed in the x, y direction, curtain coating green tape thickness is 53 μm.
(c) prepared by microwave ferrite green band:Ni-Zn-Fe-Cu Ferrite Materials are prepared using conventional solid-state method, passed through
Ni/Zn/Fe/Cu example (0.04~0.31) in molar ratio:(0.09~0.23):(0.41~0.63):(0.03~0.10) carry out
Original formulation is allocated, and then adds 0.3~0.6wt% sintering aid CaO, is changed by the way that (40Hz, 40min~60min) is sanded
Become raw material average grain diameter, average grain diameter reaches 0.3~0.7 μm, makes the final sintering temperature of Ferrite Material and K38 ceramic post sinterings
Temperature is basically identical.Wherein, the magnetic conductivity of Ni-Zn-Fe-Cu Ferrite Materials is 300.The rheologies such as the viscosity of regulation and control curtain coating material are special
Property and curtain coating parameter, make microwave ferrite green band X, shrinkage factor is consistent with microwave-medium ceramics in Y-direction, curtain coating green tape thickness
Spend for 35 μm.
(d) punching and filling perforation:Punched by laser on made green band, and pour into silver-colored palladium slurry, slurry solid content
For 88 ± 5%, the mass ratio of silver and palladium in slurry is 70:30.
(e) silk-screen printing:Regulate and control silk screen printing technique, the metallic conductor cabling preset is screen-printed to two kinds of greens
Take, wherein metal paste is starched for the silver-colored palladium of solid content 50~60%, slurry is 70 in the mass ratio of silver and palladium:30.
(f) lamination and high temperature insostatic pressing (HIP):The good green band of silk-screen is aligned according to pre-designed order and the number of plies
Lamination, is that 100MPa~200MPa, temperature are that under conditions of 40~80 DEG C, pressurize 1h carries out hip moulding in pressure.
(g) cut:Multilager base plate base substrate is cut, single LC wave filters green is separated.
(h) LC wave filters high temperature co-firing:In high-temperature box type sintering furnace, the LC wave filter green to well cutting is arranged
Glue and sintering.Wherein, it is incubated 5h at 600 DEG C and carries out dumping, 1140~1180 DEG C, guarantor is warming up to 0.5~3 DEG C/min speed
Warm 4h.
(i) chamfering:Surface spikes, impurity particle after sintering are removed, is that product surface is smooth, interior electrode is fully exposed.
(j) end is applied:End painting is carried out using silver paste, sintering temperature is at 600~800 DEG C.Tin-lead is electroplated as protective layer, enhancing
Solderability.
(k) detect:The heterogeneous multi-layer HTCC LC wave filters prepared are subjected to electric performance test and outward appearance chi
Very little detection and screening, test result is as shown in fig. 6, reach technical requirement.
It can be seen from the experimental result of embodiment 1 and embodiment 2 compared to the LC wave filters of homogeneous material for, this
The size that invention heterogeneous multi-layer material at high temperature burns LC wave filters altogether can be contracted to 1/2~1/3, volume-diminished to 1/8 to 1/20,
Therefore the weight and manufacturing cost of product are all greatly lowered.
Further compare two embodiments to understand, the dielectric constant of microwave dielectric ceramic becomes big in embodiment 2, therefore,
It can further be reduced with the size of K38 microwave-medium ceramics and ferrite high temperature co-firing LC wave filters under identical index, and produced
Product electrical property is more or less the same.
Above content is to combine optimum implementation to say the further description done to the present invention, it is impossible to assert the present invention
Specific implementation be only limited to these explanations.It should be appreciated by those skilled in the art limited not departing from by appended claims
In the case of fixed, various modifications can be carried out in detail, protection scope of the present invention should be all considered as belonging to.
Claims (10)
1. heterogeneous multi-layer ceramic high temperature burns the preparation method of LC wave filters altogether, it is characterised in that the preparation method includes as follows
Step:
(a) sintering temperature the microwave-medium ceramics green band and microwave ferrite green band suitable with horizontal shrinkage factor are prepared;
(b) punched on green band, then filling perforation;
(c) print capacitor or inductance on green band;
(d) green band is obtained into heterogeneous multi-layer ceramic high temperature through lamination, high temperature insostatic pressing (HIP) and thermal cutting and burns LC wave filter green billets altogether;
(e) by heterogeneous multi-layer ceramic high temperature burn altogether LC wave filter green billets it is sintered and post processing, obtain finished product;
It is preferred that, the post processing includes chamfering, end painting, silver ink firing, plating and detection.
2. preparation method according to claim 1, it is characterised in that in step (a), microwave-medium ceramics are M2SiO2System,
Magnesium titanate calcium system, zinc niobate system, ATiO3-LnAlO3System or barium titanium system ceramics;
Wherein, M is Zn and/or Mg, A are Ca, Sr or Ba;Ln is rare earth element;
It is preferred that, the dielectric constant of microwave-medium ceramics is 5~130;
And/or, microwave ferrite material is Mn-Zn, Ni-Zn or Cu-Zn one or more of compound system Ferrite Materials.
3. preparation method according to claim 1, it is characterised in that helped in step (a) by adjusting composition of raw materials, addition
Agent and regulation raw material particle size so that the microwave-medium ceramics green band of gained and the sintering temperature of microwave ferrite material green band
Degree matches;
It is preferred that, the auxiliary agent be zinc borosilicate glass powder, silica, diboron trioxide, bismuth oxide, niobium pentaoxide,
One or more of mixtures in zinc oxide, or calcium oxide.
4. preparation method according to claim 3, it is characterised in that in step (a), microwave-medium pottery is prepared with the tape casting
Porcelain green band and microwave ferrite green band, and by controlling the technological parameter of curtain coating so that microwave-medium ceramics green band
And the horizontal shrinkage factor of microwave ferrite green band matches;
It is preferred that, the size of microwave-medium ceramics green band and microwave ferrite green band is 4~8 inches.
5. preparation method according to claim 1, it is characterised in that filling perforation slurry therewith is silver-colored palladium metal in step (b)
Slurry;
It is preferred that, the mass ratio of silver and palladium is 30 in slurry:70~80:20;
It is preferred that, the solid content of slurry is 88 ± 5%.
6. preparation method according to claim 1, it is characterised in that in step (c), on microwave-medium ceramics green band
Printed inductance on print capacitor, microwave ferrite material;
It is preferred that, printing metal paste used is silver-colored palladium slurry;
It is furthermore preferred that slurry solid content 50%~60%;
It is further preferred that silver-colored palladium quality is than scope 30 in silver-colored palladium slurry:70~80:20.
7. preparation method according to claim 1, it is characterised in that sintering comprises the following steps described in step (d), first
First by room temperature to 600 DEG C, programming rate≤0.5 DEG C/min;Then, 1100~1400 DEG C, heating speed are warming up to by 600 DEG C
Spend for 0.5~3 DEG C/min, and be incubated 1~5h at such a temperature.
8. heterogeneous multi-layer ceramic high temperature burns LC wave filters altogether made from the method according to any one of claim 1-7.
9. heterogeneous multi-layer ceramic high temperature according to claim 8 burns LC wave filters altogether, it is characterised in that the heterogeneous multi-layer
It is microwave ferrite ceramics that ceramic high temperature burns the inductor layer of LC wave filters altogether, and capacitor layers are microwave-medium ceramics;
It is preferred that, it is microwave-medium ceramics layer that the heterogeneous multi-layer ceramic high temperature burns the structure of LC wave filters for two layers up and down altogether,
Centre is the sandwich structure of microwave ferrite layer.
10. burn the device or device of LC wave filters altogether comprising heterogeneous multi-layer ceramic high temperature described in claim 8 or 9.
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CN113372103A (en) * | 2021-07-13 | 2021-09-10 | 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 |
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