CN106927792A - The LTCC ceramic materials and preparation method of the nearly zero-temperature coefficient of low dielectric constant and low loss - Google Patents
The LTCC ceramic materials and preparation method of the nearly zero-temperature coefficient of low dielectric constant and low loss Download PDFInfo
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Abstract
The present invention provides the LTCC ceramic materials and preparation method of a kind of nearly zero-temperature coefficient of low dielectric constant and low loss, and the LTCC ceramic materials are in BaSO4BaO B are used on the basis of ceramic powder2O3‑SiO2‑Al2O3The glass of system helps burning reduction sintering temperature and uses TiO2Regulation temperature coefficient of resonance frequency, is capable of achieving 900 DEG C of low-temperature sinterings, and LTCC ceramic materials of the invention dielectric constant under 60GHz is 5.5 9, and low-dielectric loss is<2×10‑3, near-zero resonance frequency temperature coefficient τ f~± 10ppm/ DEG C.In addition, preparation method raw materials for production of the invention are cheap, low production cost, preparation process is simple.LTCC ceramic materials of the invention can use LTCC system（LTCC）, multilayer dielectricity resonator, microwave antenna, the manufacture of the microwave device such as wave filter, industrially have great application value.
Description
Technical field
The invention belongs to electron ceramic material and its manufacture field, and in particular to a kind of inexpensive low dielectric constant and low loss
LTCC ceramic materials of nearly zero-temperature coefficient and preparation method thereof.
Background technology
LTCC (Low Temperature Co-fired Ceramic, LTCC) technology be Hughes Electronics in
A kind of new material technology that nineteen eighty-two develops, it is that low-temperature sintered ceramics powder curtain coating is made into thickness even compact
Green band, after the techniques such as laser boring, slip casting, circuit silk-screen printing are made the circuitous pattern of needs, Multi-stacking compaction 900
Sinter a kind of integrated technology of three-dimensional passive device below DEG C into.At present, LTCC technology is widely used in making microwave communication, partly leads
The fields such as body, photoelectron make electronic component, and it has high integration, high performance remarkable advantage.In recent years, in the world without
By being the whole machine of universal electric, communication equipment or civilian consumer electronic product all rapidly to miniaturization, lightweight, integrated
Change, multifunction and high reliability method develop, and have promoted LTCC technology in SMD wave filter, resonator, coupler, LED
It is widely applied in the electronic components such as display module, bluetooth module, inductance, electric capacity, to high-performance LTCC materials demands
It is increasing.It is domestic to fail to obtain all the time in this field but the high-performance LTCC materials of current commercialization are mainly monopolized by foreign countries
Key breakthrough, causes LTCC integrated devices and component high cost that China researches and develops, is unfavorable for applying and promotes.Therefore, develop
The high-performance LTCC materials for possessing independent intellectual property right are extremely urgent.
Current LTCC materials mainly divide three classes：1. devitrified glass system, the material of this kind of system has less than 900 DEG C and is easy to
The characteristics of sintering, but majority haves the shortcomings that dielectric loss is bigger than normal.2. glass+ceramics compound system, this material is to make ceramics
Material reaches low sintering purpose by adding glass powder, while can keep the good microwave dielectric property of ceramic material again
Energy.3. pure ceramic systems, this kind of material system is difficult to low-temperature sintering in many cases, simultaneously for can less than 900 DEG C burn
There are some big shortcomings of dielectric loss in some ceramic materials of knot, so application scenario relative narrower again.BaSO4Ceramic material
It is originally abundant, with low cost, it is a kind of good microwave dielectric material, the common inserts as frequency PCB.But BaSO4Pottery
Porcelain sintering temperature is (~1300 DEG C) high, it is impossible to directly burnt altogether with the low-melting-point metal such as Ag, Cu；While BaSO4The resonance of ceramics is frequently
Rate temperature coefficient is~-50ppm/ DEG C, can not meet practical application request.It is conventional to have addition eutectic in order to reduce sintering temperature
Point oxide, but cooling extent is limited, it is impossible to sintered at reaching 900 DEG C；Another kind of method is to add low-melting glass, but glass
The presence of phase substantially increases the dielectric loss of material, strongly limit BaSO4The development of ceramics and microwave multilayer device.
In sum, low cost, low-k, low-loss, the LTCC ceramic materials of nearly zero-temperature coefficient and its preparation
Method becomes our research emphasis.
The content of the invention
The shortcoming of prior art, near it is an object of the invention to provide a kind of low dielectric constant and low loss in view of the above
The LTCC ceramic materials and preparation method of zero-temperature coefficient, to realize a kind of nearly zero-temperature coefficient system of inexpensive low dielectric constant and low loss
Several LTCC ceramic materials and preparation method.
In order to achieve the above objects and other related objects, the present invention provides a kind of nearly zero-temperature coefficient system of low dielectric constant and low loss
Several LTCC ceramic materials, glass that it is used and glass ceramic material obtained in Ceramic Composite, the LTCC ceramic materials with
Mass parts meter, including following components：X parts of BaSO4, y parts of BaO-B2O3-SiO2-Al2O3Base glass material and z parts
TiO2, wherein, x+y+z=100.
As a kind of preferred scheme of the LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention,
The LTCC ceramic materials are in terms of mass parts, including following components：60~75 parts of BaSO4, 20~40 parts of BaO-B2O3-
SiO2-Al2O3Base glass material and 5~10 parts of TiO2。
As a kind of preferred scheme of the LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention,
The BaO-B2O3-SiO2-Al2O3Base glass material is counted in mass ratio, including following components：The BaO of 25-35%, 20-40%'s
B2O3, the SiO of 40-60%2, the Al of 1-10%2O3, the MgO of 0-2%, and no more than 2% Na2O+K2O+Li2O。
The present invention is using above-mentioned glass system because this glass (BBSAM) system has relatively low glass transition temperature
(less than 800 DEG C), by adjusting the content of different component in glass, can obtain the glass material with different softening temperatures,
Change content, ratio of the glass powder in low-temperature co-burning ceramic material, the purpose of control material sintering temperature can be reached；Together
When this BBSAM system glass there is relatively low dielectric constant, meet the requirement of low dielectric low-temperature co-burning ceramic material.
BBSAM glass employed in the present invention, B2O3、SiO2、Al2O3It is the formation body of glass network structure, SiO2Contain
, not above 60%, when higher than 60%, glass smelting temperature is too high for amount, is unfavorable for production, and glass is unfavorable for during less than 30%
Formation；Al2O3When content is less than 5%, it is unfavorable for that glass is formed, during higher than 25%, the viscosity of glass is too big, glass melting temperature mistake
It is high；B2O3Help to reduce fusion cast glass temperature, glass viscosity is excessive when content is less than 20%, and during higher than 40%, glass chemistry is steady
Qualitative variation；BaO is favorably improved the chemical stability of glass and reduces the effect of glass smelting temperature, glass during less than 20%
Glass melting temperature is higher, glass dielectric constant increase during higher than 40%；MgO helps to adjust the effect of chemical durability of glass, contains
Amount is too high, is unfavorable for that glass is formed；Na2O、K2O、Li2O has regulation glass smelting temperature action, and total content is too high, glass chemistry
Bad stability, while the dielectric loss of glass drastically becomes big, electrical property is deteriorated.
BBSAM glass employed in the present invention, its technique is, by glass ingredient proportionally dispensing, in V-type batch mixer
Middle dry mixed, gained uniformed powder is founded 2 hours in platinum crucible at 1400 DEG C, is then poured into water glass metal
Quenching, gained cullet in tumbling ball mill wet-milling into slurry, then glass powder granularity D50 dries glass in 2.5um or so
Glass slurry obtains glass powder.
As a kind of preferred scheme of the LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention,
TiO in the LTCC ceramic materials2Its temperature coefficient of resonance frequency is adjusted in the range of 0 ± 10ppm/ DEG C.
LTCC ceramic materials provided by the present invention, wherein the ceramic powder used is：Barium sulfate (BaSO4) and titanium dioxide
Titanium (TiO2).Barium sulfate (BaSO4) have the advantages that dielectric constant is low, dielectric loss is small, by adjusting barium sulfate (BaSO4) and
The different proportion of BBSAM glass, can reach regulation sintering temperature to less than 900 DEG C；Titanium dioxide (TiO2) have it is positive humorous
Vibration frequency temperature coefficient (~+400ppm/ DEG C), by controlling the addition of titanium dioxide, can adjust LTCC ceramic materials
Temperature coefficient of resonance frequency is in the range of 0 ± 10ppm/ DEG C.
As a kind of preferred scheme of the LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention,
Under room temperature and test frequency 60GHz, dielectric constant is 5.5~9 to the LTCC ceramic materials, and dielectric loss is<2×10-3。
The present invention also provides a kind of preparation method of the LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss,
Comprise the following steps：
Step 1), with barium sulfate, titanium dioxide powder and glass dust as initial feed, the proportioning following components in terms of mass parts：
60~75 parts of BaSO4, 20~40 parts of BaO-B2O3-SiO2-Al2O3Base glass material and 5~10 parts of TiO2；
Step 2), with alcohol as solvent, through sand mill ball milling 1-2 hours, slurry Task-size Controlling in D50~2.5um, then
Dried；
Step 3), addition binding agent is granulated, compressing, is finally sintered, and is made LTCC ceramic materials.
As one kind of the preparation method of the LTCC ceramics materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention
Preferred scheme, the BaO-B2O3-SiO2-Al2O3Base glass material is counted in mass ratio, including following components：The BaO of 25-35%,
The B of 20-40%2O3, the SiO of 40-60%2, the Al of 1-10%2O3, the MgO of 0-2%, and no more than 2% Na2O+K2O+
Li2O, is weighed in above ratio, and crucible is loaded after mixing, and 1~3 hour into glass metal, quenching are founded at 1200~1500 DEG C
After dry and levigate obtain the glass dust.
As one kind of the preparation method of the LTCC ceramics materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention
Preferred scheme, it is barium sulfate powder that the barium sulfate is selected.
As one kind of the preparation method of the LTCC ceramics materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention
Preferred scheme, step 3) in, the binding agent is the PVB solution that concentration is 2~5wt%, and its additive capacity is by quality ratio 4
~8wt%.
As one kind of the preparation method of the LTCC ceramics materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention
Preferred scheme, step 3) in, the temperature of sintering is 850~900 DEG C, and sintering atmosphere is air atmosphere, and sintering time is 20~30
Minute.
As described above, the LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention and preparation side
Method, has the advantages that：The present invention provides one kind with BaSO4It is the novel low-cost low dielectric constant and low loss of principal crystalline phase
LTCC microwave ceramic materials and preparation method.The LTCC ceramic materials are in BaSO4BaO-B is used on the basis of ceramic powder2O3-
SiO2-Al2O3The glass of system helps burning reduction sintering temperature and uses TiO2Regulation temperature coefficient of resonance frequency, is capable of achieving 900 DEG C
Low-temperature sintering, LTCC ceramic materials of the invention dielectric constant under 60GHz is 5.5-9, and low-dielectric loss is<2×10-3, closely
Zero resonance frequency temperature coefficient τ f~± 10ppm/ DEG C.In addition, preparation method raw materials for production of the invention are cheap, production cost
Low, preparation process is simple.LTCC ceramic materials of the invention can use LTCC system (LTCC), multilayer dielectricity resonance
The manufacture of the microwave devices such as device, microwave antenna, wave filter, industrially there is great application value.
Brief description of the drawings
The preparation method of the LTCC ceramics materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention is shown as such as Fig. 1
Steps flow chart schematic diagram.
Fig. 2 is shown as the microwave dielectric property of LTCC microwave ceramic materials of the invention with the change of BBSAM glass incorporations
Change graph of relation.
Fig. 3 is shown as the temperature coefficient of resonance frequency and dielectric constant of LTCC microwave ceramic materials of the invention with TiO2Mix
Enter the variation relation curve map of amount.
Fig. 4 present invention gained LTCC microwave ceramic materials are schemed with Ag electrode material matching co-firings interface SEM.
Component label instructions
S11~S13 steps 1~step 3)
Specific embodiment
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages of the invention and effect easily.The present invention can also be by specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Refer to Fig. 1~Fig. 4.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, package count when only display is with relevant component in the present invention rather than according to actual implementation in illustrating then
Mesh, shape and size are drawn, and the kenel of each component, quantity and ratio can be a kind of random change during its actual implementation, and its
Assembly layout kenel is likely to increasingly complex.
Embodiment 1
The present embodiment provides a kind of LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss, its glass for using
Glass and glass ceramic material obtained in Ceramic Composite, the LTCC ceramic materials are in terms of mass parts, including following components：X parts
BaSO4, y parts of BaO-B2O3-SiO2-Al2O3Base glass material and z parts of TiO2, wherein, x+y+z=100.
As an example, the LTCC ceramic materials are in terms of mass parts, including following components：60~75 parts of BaSO4, 20~
40 parts of BaO-B2O3-SiO2-Al2O3Base glass material and 5~10 parts of TiO2。
As an example, the BaO-B2O3-SiO2-Al2O3Base glass material is counted in mass ratio, including following components：25-
The B of 35% BaO, 20-40%2O3, the SiO of 40-60%2, the Al of 1-10%2O3, the MgO of 0-2%, and no more than 2%
Na2O+K2O+Li2O.The present invention is using above-mentioned glass system because this glass (BBSAM) system has relatively low Glass Transition
Temperature (less than 800 DEG C), by adjusting the content of different component in glass, can obtain the glass material with different softening temperatures
Material, changes content, ratio of the glass powder in low-temperature co-burning ceramic material, can reach the mesh of control material sintering temperature
, as shown in Figure 2.The glass of this BBSAM system has relatively low dielectric constant simultaneously, meets low dielectric LTCC material
The requirement of material.BBSAM glass employed in the present invention, B2O3、SiO2、Al2O3It is the formation body of glass network structure, SiO2Contain
, not above 60%, when higher than 60%, glass smelting temperature is too high for amount, is unfavorable for production, and glass is unfavorable for during less than 30%
Formation；Al2O3When content is less than 5%, it is unfavorable for that glass is formed, during higher than 25%, the viscosity of glass is too big, glass melting temperature mistake
It is high；B2O3Help to reduce fusion cast glass temperature, glass viscosity is excessive when content is less than 20%, and during higher than 40%, glass chemistry is steady
Qualitative variation；BaO is favorably improved the chemical stability of glass and reduces the effect of glass smelting temperature, glass during less than 20%
Glass melting temperature is higher, glass dielectric constant increase during higher than 40%；MgO helps to adjust the effect of chemical durability of glass, contains
Amount is too high, is unfavorable for that glass is formed；Na2O、K2O、Li2O has regulation glass smelting temperature action, and total content is too high, glass chemistry
Bad stability, while the dielectric loss of glass drastically becomes big, electrical property is deteriorated.BBSAM glass employed in the present invention, its
Technique is, by glass ingredient proportionally dispensing, the dry mixed in V-type batch mixer, gained uniformed powder, in platinum crucible
Found 2 hours at 1400 DEG C, glass metal be then poured into water quenching, gained cullet in tumbling ball mill wet-milling into slurry
Then material, glass powder granularity D50 dries glass paste and obtains glass powder in 2.5um or so.
As an example, TiO in the LTCC ceramic materials2Its temperature coefficient of resonance frequency is adjusted in 0 ± 10ppm/ DEG C of model
In enclosing.LTCC ceramic materials provided by the present invention, wherein the ceramic powder used is：Barium sulfate (BaSO4) and titanium dioxide
(TiO2).Barium sulfate (BaSO4) have the advantages that dielectric constant is low, dielectric loss is small, by adjusting barium sulfate (BaSO4) and
The different proportion of BBSAM glass, can reach regulation sintering temperature to less than 900 DEG C；Titanium dioxide (TiO2) have it is positive humorous
Vibration frequency temperature coefficient (~+400ppm/ DEG C), by controlling the addition of titanium dioxide, can adjust LTCC ceramic materials
Temperature coefficient of resonance frequency in the range of 0 ± 10ppm/ DEG C, as shown in Figure 3.
As an example, the LTCC ceramic materials are under room temperature and test frequency 60GHz, dielectric constant is 6~8, is situated between
Electrical loss is<2×10-3。
As shown in figure 1, the present embodiment also provides a kind of LTCC ceramics materials of the nearly zero-temperature coefficient of low dielectric constant and low loss
The preparation method of material, comprises the following steps：
Step 1 is carried out first) S11, with barium sulfate, titanium dioxide powder and glass dust as initial feed, is matched somebody with somebody in terms of mass parts
Compare following components：60~75 parts of BaSO4, 20~40 parts of BaO-B2O3-SiO2-Al2O3Base glass material and 5~10 parts
TiO2；
Then step 2 is carried out) S12, with alcohol as solvent, through sand mill ball milling 1-2 hours, slurry Task-size Controlling was in D50
~2.5um, is then dried；
Finally carry out step 3) S13, addition binding agent is granulated, compressing, is finally sintered, and is made LTCC potteries
Ceramic material.
As an example, the BaO-B2O3-SiO2-Al2O3Base glass material is counted in mass ratio, including following components：25-
The B of 35% BaO, 20-40%2O3, the SiO of 40-60%2, the Al of 1-10%2O3, the MgO of 0-2%, and no more than 2%
Na2O+K2O+Li2O, is weighed in above ratio, and crucible is loaded after mixing, is founded at 1200~1500 DEG C 1~3 hour into glass
Liquid, dries after quenching and levigate obtains the glass dust.It is barium sulfate powder that the barium sulfate is selected.
As an example, the binding agent is the PVB solution that concentration is 2~5wt%, its additive capacity is by quality ratio 4
~8wt%.
As an example, the temperature of sintering is 850~900 DEG C, sintering atmosphere is air atmosphere, and sintering time is 20~30 points
Clock.
In a specific implementation process, BaO-B2O3-SiO2-Al2O3Base glass material powder (BBSAM-1) is according to such as
Lower component is founded：BaO 25%, B2O320%, SiO247%, Al2O35.5%, MgO 0.5%, Na2O 0.5%, K2O
0.5%, Li2O 1%；1400 DEG C of glass melting temperature, melting time 2hr, glass is also poured into water quenching, and wet-milling to granularity D50 exists
2.5um or so.
Low-temperature co-burning ceramic material composition and ratio is：70~80 parts of (90% barium sulfate (BaSO4)+10% titanium dioxide
(TiO2), 20~30 parts of BaO-B2O3-SiO2-Al2O3Base glass material powder, compound wet-milling to granularity D50 is left in 2.5um
It is right.
Gained low-temperature co-burning ceramic material is sintered at 880 DEG C, is incubated 30 minutes, and measuring material property under 60GHz is：It is situated between
Electric constant is 7.1-7.8, dielectric loss≤2.0 × 10-3, temperature coefficient of resonance frequency τ f~+7.5ppm/ DEG C.
LTCC ceramic materials powder of the invention can be incubated 20~30 minutes at 850~900 DEG C, with Ag slurry etc. electrode material
Material matching co-firing simultaneously obtains good sintering quality, as shown in Figure 4.
Embodiment 2
The present embodiment provides the LTCC ceramic materials and preparation method of a kind of nearly zero-temperature coefficient of low dielectric constant and low loss,
Its basic scheme such as embodiment 1, wherein：
In the present embodiment, BaO-B2O3-SiO2-Al2O3Base glass material powder (BBSAM-2) is molten according to following component
System：BaO 25%, B2O323%, SiO244%, Al2O35.5%, MgO 0.5%, Na2O 0.5%, K2O 0.5%, Li2O
1%；1400 DEG C of glass melting temperature, melting time 2hr, glass is also poured into water quenching, and wet-milling to granularity D50 is in 2.5um or so.
Low-temperature co-burning ceramic material is constituted in parts by mass, is matched and is：(100-a) (30% glass dust (BBSAM-2)+
70% barium sulfate (BaSO4))+a titanium dioxide (TiO2), wherein, the scope of a is 5~10.Compound wet-milling exists to granularity D50
2.5um or so.
Gained low-temperature co-burning ceramic material is sintered at 880 DEG C, is incubated 30 minutes, and measuring material property under 60GHz is：It is situated between
Electric constant is 7.5~8.5, dielectric loss≤2.0 × 10-3, temperature coefficient of resonance frequency τ f：- 9~+9.5ppm/ DEG C.
Embodiment 3
The present embodiment provides the LTCC ceramic materials and preparation method of a kind of nearly zero-temperature coefficient of low dielectric constant and low loss,
Its basic scheme such as embodiment 1, wherein：
In the present embodiment, BaO-B2O3-SiO2-Al2O3Base glass material powder is molten according to following component (BBSAM-3)
System：BaO 20%, B2O325%, SiO247%, Al2O35%, MgO 1%, Na2O 0.5%, K2O 0.5%, Li2O 1%；It is molten
1400 DEG C of temperature processed, melting time 2hr, glass is also poured into water quenching, and wet-milling to granularity D50 is in 2.5um or so.
Low-temperature co-burning ceramic material is constituted in parts by mass, is matched and is：70 parts of barium sulfate (BaSO4), 6 parts of titanium dioxide
Titanium, 24 parts of BBSAM-3 glass.Compound wet-milling is to granularity D50 in 2.5um or so.
Gained low-temperature co-burning ceramic material is sintered at 900 DEG C, is incubated 30 minutes, and measuring material property under 60GHz is：It is situated between
Electric constant is 5.9, and dielectric loss is 1.85 × 10-3, temperature coefficient of resonance frequency τ f~+3.5ppm/ DEG C
Embodiment 4
The present embodiment provides the LTCC ceramic materials and preparation method of a kind of nearly zero-temperature coefficient of low dielectric constant and low loss,
Its basic scheme such as embodiment 1, wherein：
In the present embodiment, BaO-B2O3-SiO2-Al2O3Base glass material powder (BBSAM-4) is molten according to following component
System：BaO 25%, B2O325%, SiO242%, Al2O34%, MgO 2%, Na2O 0.5%, K2O 0.5%, Li2O 1%；It is molten
1400 DEG C of temperature processed, melting time 2hr, glass is also poured into water quenching, and wet-milling to granularity D50 is in 2.5um or so.
Low-temperature co-burning ceramic material is constituted in parts by mass, is matched and is：65 parts of barium sulfate (BaSO4), 7 parts of titanium dioxide
Titanium, 28 parts of BBSAM-1 glass.Compound wet-milling is to granularity D50 in 2.5um or so.
Gained low-temperature co-burning ceramic material is sintered at 880 DEG C, is incubated 30 minutes, and measuring material property under 60GHz is：It is situated between
Electric constant is 8.12, and dielectric loss is 1.75 × 10-3, temperature coefficient of resonance frequency τ f~+9.0ppm/ DEG C
Embodiment 5
The present embodiment provides the LTCC ceramic materials and preparation method of a kind of nearly zero-temperature coefficient of low dielectric constant and low loss,
Its basic scheme such as embodiment 1, wherein：
In the present embodiment, BaO-B2O3-SiO2-Al2O3Base glass material powder (BBSAM-5) is molten according to following component
System：BaO 25%, B2O328%, SiO240%, Al2O33%, MgO 2%, Na2O 0.5%, K2O 0.5%, Li2O 1%；It is molten
1400 DEG C of temperature processed, melting time 2hr, glass is also poured into water quenching, and wet-milling to granularity D50 is in 2.5um or so.
Low-temperature co-burning ceramic material is constituted in parts by mass, is matched and is：70 parts of barium sulfate (BaSO4), 5 parts of titanium dioxide
Titanium, 25 parts of BBSAM-5 glass.Compound wet-milling is to granularity D50 in 2.5um or so.
Gained low-temperature co-burning ceramic material is sintered at 870 DEG C, is incubated 30 minutes, and measuring material property under 60GHz is：It is situated between
Electric constant is 7.65, and dielectric loss is 1.75 × 10-3, temperature coefficient of resonance frequency τ f~-5.5ppm/ DEG C.
Embodiment 6
The present embodiment provides the LTCC ceramic materials and preparation method of a kind of nearly zero-temperature coefficient of low dielectric constant and low loss,
Its basic scheme such as embodiment 1, wherein：
In the present embodiment, BaO-B2O3-SiO2-Al2O3Base glass material powder (BBSAM-6) is molten according to following component
System：BaO 20%, B2O335%, SiO240%, Al2O32%, MgO 1%, Na2O 0.5%, K2O 0.5%, Li2O 1%；It is molten
1400 DEG C of temperature processed, melting time 2hr, glass is also poured into water quenching, and wet-milling to granularity D50 is in 2.5um or so.
Low-temperature co-burning ceramic material is constituted in parts by mass, is matched and is：68 parts of barium sulfate (BaSO4), 5 parts of titanium dioxide
Titanium, 27 parts of BBSAM-6 glass.Compound wet-milling is to granularity D50 in 2.5um or so.
Gained low-temperature co-burning ceramic material is sintered at 850 DEG C, is incubated 30 minutes, and measuring material property under 60GHz is：It is situated between
Electric constant is 7.25, and dielectric loss is 1.95 × 10-3, temperature coefficient of resonance frequency τ f~-8.5ppm/ DEG C.
As described above, the LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss of the invention and preparation side
Method, has the advantages that：The present invention provides one kind with BaSO4It is the novel low-cost low dielectric constant and low loss of principal crystalline phase
LTCC microwave ceramic materials and preparation method.The LTCC ceramic materials are in BaSO4BaO-B is used on the basis of ceramic powder2O3-
SiO2-Al2O3The glass of system helps burning reduction sintering temperature and uses TiO2Regulation temperature coefficient of resonance frequency, is capable of achieving 900 DEG C
Low-temperature sintering, LTCC ceramic materials of the invention dielectric constant under 60GHz is 5.5-9, and low-dielectric loss is<2×10-3, closely
Zero resonance frequency temperature coefficient τ f~± 10ppm/ DEG C.In addition, preparation method raw materials for production of the invention are cheap, production cost
Low, preparation process is simple.LTCC ceramic materials of the invention can use LTCC system (LTCC), multilayer dielectricity resonance
The manufacture of the microwave devices such as device, microwave antenna, wave filter, industrially there is great application value.So, the present invention is effectively
Overcome various shortcoming of the prior art and have high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (10)
1. a kind of LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss, it is characterised in that the LTCC ceramics
Material is in terms of mass parts, including following components：X parts of BaSO4, y parts of BaO-B2O3-SiO2-Al2O3Base glass material and z
The TiO of part2, wherein, x+y+z=100.
2. LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss according to claim 1, its feature exists
In the LTCC ceramic materials are in terms of mass parts, including following components：60~75 parts of BaSO4, 20~40 parts of BaO-B2O3-
SiO2-Al2O3Base glass material and 5~10 parts of TiO2。
3. LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss according to claim 1, its feature exists
In the BaO-B2O3-SiO2-Al2O3Base glass material is counted in mass ratio, including following components：The BaO of 25-35%, 20-
40% B2O3, the SiO of 40-60%2, the Al of 1-10%2O3, the MgO of 0-2%, and no more than 2% Na2O+K2O+Li2O。
4. LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss according to claim 1, its feature exists
In TiO in the LTCC ceramic materials2Its temperature coefficient of resonance frequency is adjusted in the range of 0 ± 10ppm/ DEG C.
5. LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss according to claim 1, its feature exists
In：Under room temperature and test frequency 60GHz, dielectric constant is 5.5~9 to the LTCC ceramic materials, and dielectric loss is<2×
10-3。
6. a kind of preparation method of the LTCC ceramic materials of the nearly zero-temperature coefficient of low dielectric constant and low loss, it is characterised in that bag
Include following steps：
Step 1), with barium sulfate, titanium dioxide powder and glass dust as initial feed, the proportioning following components in terms of mass parts：60~
75 parts of BaSO4, 20~40 parts of BaO-B2O3-SiO2-Al2O3Base glass material and 5~10 parts of TiO2；
Step 2), with alcohol as solvent, through sand mill ball milling 1-2 hours, then slurry Task-size Controlling was carried out in D50~2.5um
Drying；
Step 3), addition binding agent is granulated, compressing, is finally sintered, and is made LTCC ceramic materials.
7. the nearly zero-temperature coefficient of low dielectric constant and low loss according to claim 6 LTCC ceramics material preparation method,
It is characterized in that：The BaO-B2O3-SiO2-Al2O3Base glass material is counted in mass ratio, including following components：25-35%'s
The B of BaO, 20-40%2O3, the SiO of 40-60%2, the Al of 1-10%2O3, the MgO of 0-2%, and no more than 2% Na2O+
K2O+Li2O, is weighed in above ratio, and crucible is loaded after mixing, and 1~3 hour is founded at 1200~1500 DEG C into glass metal, is quenched
Drying is levigate after cold obtains the glass dust.
8. the nearly zero-temperature coefficient of low dielectric constant and low loss according to claim 6 LTCC ceramics material preparation method,
It is characterized in that：It is barium sulfate powder that the barium sulfate is selected.
9. the nearly zero-temperature coefficient of low dielectric constant and low loss according to claim 6 LTCC ceramics material preparation method,
It is characterized in that：Step 3) in, the binding agent is the PVB solution that concentration is 2~5wt%, and its additive capacity is by quality ratio
It is 4~8wt%.
10. the nearly zero-temperature coefficient of low dielectric constant and low loss according to claim 6 LTCC ceramics material preparation method,
It is characterized in that：Step 3) in, the temperature of sintering is 850~900 DEG C, and sintering atmosphere is air atmosphere, sintering time is 20~
30 minutes.
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