CN103145416B - Environment-friendly ultralow-temperature sintered microwave dielectric ceramic material and preparation method thereof - Google Patents
Environment-friendly ultralow-temperature sintered microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- CN103145416B CN103145416B CN201310084857.1A CN201310084857A CN103145416B CN 103145416 B CN103145416 B CN 103145416B CN 201310084857 A CN201310084857 A CN 201310084857A CN 103145416 B CN103145416 B CN 103145416B
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims description 43
- 238000000498 ball milling Methods 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 18
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 10
- 229910052573 porcelain Inorganic materials 0.000 description 6
- 238000003556 assay Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000009774 resonance method Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- MOVRNJGDXREIBM-UHFFFAOYSA-N aid-1 Chemical compound O=C1NC(=O)C(C)=CN1C1OC(COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)CO)C(O)C1 MOVRNJGDXREIBM-UHFFFAOYSA-N 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
Abstract
The invention discloses an environment-friendly ultralow-temperature sintered microwave dielectric ceramic material system and a preparation method thereof. The structure expression formula of the system is K2MoxO(3x+1)(x is equal to 2-4). The system can be sintered at very low temperature (460-550 DEG C), has excellent microwave dielectric performance (the dielectric constant ranges from 5 to 8, the quality factor Qf ranges from 30,000GHz to 50,000GHz, the frequency temperature coefficient ranges from minus 60ppm/DEG C to minus 93ppm/DEG C). The powder is prepared by adopting a solid phase synthesis method, and the presintering temperature ranges from 400 DEG C to 450 DEG C. The material system can be sintered jointly with Ag or Al, can be used for preparing low-temperature co-fired ceramic (LTCC) substrates, and is applied to a microwave resonator, a filter, a planar antenna and the like. The environment-friendly ultralow-temperature sintered microwave dielectric ceramic material system and the preparation method thereof meet the environment-friendly requirement, and are non-toxic and free from environment pollution.
Description
Technical field
The invention belongs to electronic ceramic and preparation field thereof, particularly be can be in 470-550 ° of C temperature range the environment-friendly type ultralow temperature-sintered microwave dielectric ceramic material system and preparation method thereof of densified sintering product.
Background technology
Along with the development of modern communications technology, the miniaturization of electronic product, portability, the aspect such as multi-functional, highly reliable and low-cost have been proposed to more and more higher requirement.LTCC is mainly used in the technical elements of high integration, high-performance electronic encapsulation, aspect flexibility, wiring density and the reliability of design, has huge potential.
Microwave-medium ceramics is as the key foundation material of LTCC technology, requirement has low sintering temperature (being less than 900 ° of C), suitable dielectric constant, high quality factor, be bordering on zero temperature coefficient of resonance frequency and good thermal stability, and ceramic material formula should be conducive to technological process, is easy to industrialization.Most traditional electronic ceramics can not meet the requirement of LTCC technology to material, and its reason is that ceramic sintering temperature is too high.Exploitation low-temp sintered material has caused people's interest.
Microwave-medium ceramics is realized low sintering main path to be had: appropriate sintering aid 1. adulterates---low melting point oxide or low-melting glass; 2. adopt wet chemistry method to prepare the powder that surface activity is high; 3. adopt nano-powder; 4. adopt hot pressed sintering.At above these, reduce in the method for sintering temperature, consider that 4. 3. 2. the complexity of production cost, technique be all unfavorable for suitability for industrialized production.1., cost is low for method, and technique is simple, be current conventional low-temperature sintering method, but often additive can worsen ceramic performance.Therefore, finding the microwave-medium ceramics system that novel intrinsic sintering temperature is low is one of direction of future development, particularly the material system of ultra-high dielectric coefficient (being greater than 100) and ultralow dielectric (3-5).
The ultralow-temperature sintering microwave medium ceramic systems being publicly reported at present mainly contains Te base Bi
2o
3– TeO
2, TiO
2– TeO
2, CaO – TeO
2, BaO-TiO
2-TeO
2with Mo base Bi
2o
3-MoO
3, Li
2o-Bi
2o
3-MoO
3, in these systems, minimum sintering temperature reaches 520 ° of C, Te
2(Mo
0.95w
0.05) O
7520 ° of C sintering DIELECTRIC CONSTANT ε
r=13.9, Qf=25820GHz, τ
f=-12.8ppm/ ° C.Li
2mo
4o
13at 520 ° of C sintering ε
r=8.8, Qf=7700GHz, τ
f=-66ppm/ ° C.Consider the costliness of the raw material of Te, and have severe toxicity, be not suitable for a large amount of production.In these sintered at ultra low temperature system ceramic materials, component at least contains the oxide that a kind of fusing point is lower.So the present invention has studied K
2o-MoO
3system, found that this system material has good microwave dielectric property, ε
r=5～8, Qf=30000～50000GHz, τ
f=-60～-93ppm/ ° C, can burn altogether with Ag or Al electrode, and chemical composition and preparation technology are simple, particularly has ultralow sintering temperature (470-550 ° of C), is minimum in the current existing microwave-medium ceramics system of reporting.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned current technology, do not adding on the basis of any sintering aid, ultralow temperature-sintered microwave dielectric ceramic material system and preparation method thereof is provided, and meet the requirement of ltcc substrate material technology.
First object of the present invention is to provide three kinds of ultralow temperature-sintered microwave dielectric ceramic materials, after sintering, its microwave property is relative dielectric constant 5～8, microwave dielectric loss 30000～50000GHz, frequency-temperature coefficient-60～-93ppm/ ° C, topmost feature is at low-down temperature (470～550 ° of C), to carry out sintering, and can burn altogether with Ag or Al electrode, chemical composition and preparation technology are simple simultaneously.
For achieving the above object, the invention provides a kind of environment-friendly type ultralow temperature-sintered microwave dielectric ceramic material system, this ceramic material structure expression is: K
2mo
xo
3x+1, wherein, x=2～4, this system is carried out sintering and is made between 440 ° of C to 550 ° of C of ultralow sintering range.
Second object of the present invention is to provide the preparation method of above-mentioned ultralow temperature-sintered microwave dielectric ceramic material, and technique is simple.
For achieving the above object, the technical solution used in the present invention is:
A preparation method for environment-friendly type ultralow temperature-sintered microwave dielectric ceramic material system, is characterized in that: according to general formula K
2mo
xo
3x+1, wherein, x=2～4, take raw material, after adopting a ball milling that raw material is mixed, carry out presintering at the temperature of 400-450 ° of C, then, carry out secondary ball milling, and finally by compressing tablet sintering and get final product, wherein, the sintering temperature of compressing tablet sintering is 440-550 ° of C.
One time ball milling carries out in ball grinder, and in ball grinder, adds and have zirconium ball and absolute ethyl alcohol, wherein, according to mass ratio, zirconium ball: raw material: absolute ethyl alcohol is 2:1:1.
The parameter of a ball milling is: speed 150r/min, time 4h.
After the powder drying obtaining after a ball milling, put into again crucible and carry out presintering.
The compressing tablet process of compressing tablet sintering is: in the powder after secondary ball milling, adding percentage by weight is that 5% PVA carries out granulation, after granulation, gets 60-120 object powder, under the pressure of 300MPa, is pressed.
After compressing, at 390-440 ° of C insulation 4-5 hour, to get rid of PVA.
The present invention adopts the synthetic method of the most simple and effective solid phase reaction to prepare ceramic material system of the present invention.First, according to formula Design, carry out weighing.Then, adopt a ball milling that raw material is mixed, the synthetic phase needing of pre-burning at suitable temperature, and increase the activity of reacting, adopt secondary ball milling that synthetic powder is levigate.Finally by compressing tablet sintering, obtain needed ceramics sample.Through simple and effective like this preparation method, the dielectric constant of the ceramics sample obtaining changes between 5～8, quality factor q f is distributed in 30, between 000～50,000GHz, temperature coefficient of resonance frequency is between-60～-93ppm/ ° C, sintering temperature is between 470～550 ° of C, can burn altogether with Ag or Al electrode, make it to be applicable to the needs of LTCC technology, expand its range of application.
Accompanying drawing explanation
Fig. 1 is that the XRD of the ceramic systems prepared by the inventive method schemes.
Embodiment
Technical scheme of the present invention is achieved in that the structure representation general formula of ultralow-temperature sintering microwave medium pottery is K
2mo
xo
3x+1, wherein, x=2～4.
Ultralow-temperature sintering microwave medium pottery step of preparation process of the present invention is as follows:
1) by chemical raw material K
2cO
3(purity is 99%) and MoO
3(purity is 99.5%) is by formula general formula K
2mo
xo
3x+1preparation, wherein x=2～4;
2) raw material weighing up is put into ball grinder, according to zirconium ball: the mass ratio of raw material: absolute ethyl alcohol=2:1:1 adds goal and absolute ethyl alcohol, after good seal, be placed on planetary ball mill the rotating speed ball milling 4h with 150r/min;
3) powder after a ball milling takes out and dries (100 ° of C of bake out temperature), then puts into crucible respectively at 400-450 ° of C pre-burning 4h;
4) powder after pre-burning, manually levigate after, put into ball grinder, according to step 2) in same ratio, after good seal, be placed on planetary ball mill the rotating speed ball milling 5h with 150r/min;
5) powder after ball milling is taken out and dries (100 ° of C of bake out temperature), add the PVA of 5wt% to carry out granulation, get 60 orders to the powder between 120 orders, under the pressure of 300MPa, be pressed, at 390-440 ° of C insulation 4-5h, PVA is got rid of.Then at 440-550 ° of C insulation 2h, carry out sintering, obtain needed microwave dielectric ceramic materials.
Ultralow-temperature sintering microwave medium ceramic substrate material of the present invention has following characteristics: relatively low dielectric constant (5～8), lower dielectric loss (30,000～50,000GHz), temperature coefficient of resonance frequency low (TCF=-60～-93ppm/ ° C), ultralow sintering temperature (470～550 ° of C), can burn altogether with Ag or Al electrode, and chemical composition and preparation technology are simple.The present invention meets environmental requirement, nontoxic, environmentally safe.
The present invention is according to the correlation theory of crystal chemistry and Dielectric Physics, and selecting low melting point oxide is initial raw material, with K
2o-MoO
3low fever's compound in Binary Phase Diagram is basis, adopts above process for solid phase synthesis, obtains the well behaved microwave dielectric ceramic materials of sintered microwave at ultralow temperature.
Embodiment 1:
By the raw material K of purity assay
2cO
3and MoO
3in 1:2 ratio, be mixed with main powder, then by the abundant mixing and ball milling of main powder 4 hours, after drying 400 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, after levigate oven dry, add 5wt%PVA granulation, through 60 orders and 120 eye mesh screen bilayers, sieve, under the pressure of 300MPa compressing (sheet or column) on demand, at 390 ° of C insulation 5h, PVA is got rid of, then under 480 ° of C air, sintering 2h becomes porcelain, can obtain ultralow temperature-sintered microwave dielectric ceramic material.
The present invention uses network analyzer (8720ES Agilent) and incubator (DELTA9023, DeltaDesign) to adopt and closes microwave dielectric property and the temperature spectrum that chamber the resonance method has been tested sample.The computing formula of TCF is as follows:
F
85and f
25respectively TE when 85 ° of C and 25 ° of C
01 δresonance frequency under pattern.
The performance of this group ceramic material reaches following index:
K
2mo
2o
7in 480 ° of C air, sinter porcelain into, the dielectric property ε under microwave
r～6 (11.8GHz), quality factor q～3700, Qf～41,740GHz, the temperature coefficient of resonance frequency TCF under microwave～-84ppm/ ° C (25-85 ° of C).
Embodiment 2:
By the raw material K of purity assay
2cO
3and MoO
3in 1:3 ratio, be mixed with main powder, then by the abundant mixing and ball milling of main powder 4 hours, after drying 450 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, after levigate oven dry, add 5wt%PVA granulation, through 60 orders and 120 eye mesh screen bilayers, sieve, under the pressure of 300MPa compressing (sheet or column) on demand, at 440 ° of C insulation 5h, PVA is got rid of, then under 520 ° of C air, sintering 2h becomes porcelain, can obtain ultralow temperature-sintered microwave dielectric ceramic material.
The present invention uses network analyzer (8720ES Agilent) and incubator (DELTA9023, DeltaDesign) to adopt and closes microwave dielectric property and the temperature spectrum that chamber the resonance method has been tested sample.The computing formula of TCF is as follows:
F
85and f
25respectively TE when 85 ° of C and 25 ° of C
01 δresonance frequency under pattern.
The performance of this group ceramic material reaches following index:
K
2mo
3o
10in 520 ° of C air, sinter porcelain into, the dielectric property ε under microwave
r～5.6 (12.2GHz), quality factor q～3188, Qf～35,828GHz, the temperature coefficient of resonance frequency TCF under microwave～-92ppm/ ° C (25-85 ° of C).
Embodiment 3:
By the raw material K of purity assay
2cO
3and MoO
3in 1:4 ratio, be mixed with main powder, then by the abundant mixing and ball milling of main powder 4 hours, after drying 450 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, after levigate oven dry, add 5wt%PVA granulation, through 60 orders and 120 eye mesh screen bilayers, sieve, under the pressure of 300MPa compressing (sheet or column) on demand, at 440 ° of C insulation 5h, PVA is got rid of, then under 550 ° of C air, sintering 2h becomes porcelain, can obtain ultralow temperature-sintered microwave dielectric ceramic material.
The present invention uses network analyzer (8720ES Agilent) and incubator (DELTA9023, DeltaDesign) to adopt and closes microwave dielectric property and the temperature spectrum that chamber the resonance method has been tested sample.The computing formula of TCF is as follows:
F
85and f
25respectively TE when 85 ° of C and 25 ° of C
01 δresonance frequency under pattern.
The performance of this group ceramic material reaches following index:
K
2mo
4o
13in 550 ° of C air, sinter porcelain into, the dielectric property ε under microwave
r～5.3 (11.1GHz), quality factor q～4300, Qf～49,981GHz, the temperature coefficient of resonance frequency TCF under microwave～-66ppm/ ° C (25-85 ° of C).
Embodiment 4:
By the raw material K of purity assay
2cO
3and MoO
3in 1:1 ratio, be mixed with main powder, then by the abundant mixing and ball milling of main powder 4 hours, after drying 500 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, after levigate oven dry, add 5wt%PVA granulation, through 60 orders and 120 eye mesh screen bilayers, sieve, under the pressure of 300MPa compressing (sheet or column) on demand, sticky 450 ° of C insulation 5h rows, then sintering 2h under 600 ° of C air, can obtain ultralow temperature-sintered microwave dielectric ceramic material.
The present invention uses network analyzer (8720ES Agilent) and incubator (DELTA9023, DeltaDesign) to adopt and closes microwave dielectric property and the temperature spectrum that chamber the resonance method has been tested sample.The computing formula of TCF is as follows:
F
85and f
25respectively TE when 85 ° of C and 25 ° of C
01 δresonance frequency under pattern.
The performance of this group ceramic material reaches following index:
K
2moO
4sintering in 600 ° of C air, the dielectric property ε under microwave
r～5.7 (11.05GHz), quality factor q～100, Qf～1000GHz, the temperature coefficient of resonance frequency TCF under microwave～-64ppm/ ° C (25-85 ° of C).
Refer to shown in Fig. 1, by comparing embodiment 1,2,3,4, the K that visible the present invention proposes
2mo
xo
3x+1(x=2～4) system has good microwave dielectric property (ε
r=5～8, Qf=30,000～50,000GHz, TCF=-60～-93ppm/ ° C).Advantage of the present invention is, this environmental protection new system not only can be at ultralow temperature sintering, and there is good microwave dielectric property.
It is pointed out that, according to technical scheme of the present invention, above-described embodiment can also be enumerated many, the results show a large amount of according to applicant, the scope proposing at claims of the present invention, all can reach object of the present invention.
Claims (8)
1. an environment-friendly type ultralow temperature-sintered microwave dielectric ceramic material system, is characterized in that, this ceramic material structure expression is: K
2mo
xo
3x+1wherein, x=2～4, this system is carried out between 440 ℃ to 550 ℃ of ultralow sintering ranges that sintering makes and can be burnt altogether with Ag or Al electrode, after sintering, its microwave property is relative dielectric constant 5～8, microwave dielectric loss 30000～50000GHz, frequency-temperature coefficient-60～-93ppm/ ℃.
2. a preparation method for environment-friendly type ultralow temperature-sintered microwave dielectric ceramic material system, is characterized in that: according to general formula K
2mo
xo
3x+1, wherein, x=2～4, take raw material, after adopting a ball milling that raw material is mixed, carry out presintering at the temperature of 400-450 ℃, then, carry out secondary ball milling, and finally by compressing tablet sintering and get final product, wherein, the sintering temperature of compressing tablet sintering is 440-550 ℃.
3. method as claimed in claim 2, is characterized in that: one time ball milling carries out in ball grinder, and in ball grinder, adds zirconium ball and absolute ethyl alcohol, wherein, according to mass ratio, zirconium ball: raw material: absolute ethyl alcohol is 2:1:1.
4. method as claimed in claim 3, is characterized in that: the parameter of a ball milling is: speed 150r/min, time 4h.
5. method as claimed in claim 2, is characterized in that: after the powder drying obtaining after a ball milling, put into crucible again and carry out presintering.
6. method as claimed in claim 2, it is characterized in that: the compressing tablet process of compressing tablet sintering is: in the powder after secondary ball milling, adding percentage by weight is that 5% PVA carries out granulation, after granulation, get 60-120 object powder, under the pressure of 300MPa, be pressed.
7. method as claimed in claim 6, is characterized in that: after compressing, at 390-440 ℃ of insulation 4-5 hour, to get rid of PVA.
8. a preparation method for environment-friendly type ultralow temperature-sintered microwave dielectric ceramic material system, is characterized in that: comprise the following steps:
1) by raw material K
2cO
3and MoO
3by formula general formula K
2mo
xo
3x+1preparation, wherein x=2～4;
2) raw material weighing up is put into ball grinder, according to zirconium ball: the mass ratio of raw material: absolute ethyl alcohol=2:1:1 adds zirconium ball and absolute ethyl alcohol, after good seal, be placed on planetary ball mill the rotating speed ball milling 4h with 150r/min;
3) powder after a ball milling takes out and dries, and then puts into crucible at 400-450 ℃ of pre-burning 4h;
4) powder after pre-burning, manually levigate after, put into ball grinder, according to step 2) identical method carries out secondary ball milling;
5) powder after secondary ball milling is taken out and dried, add the PVA of percentage by weight 5% to carry out granulation, get 60 orders to the powder between 120 orders, be pressed, at 390-440 ℃ of insulation 4-5h, PVA is got rid of, finally at 440-550 ℃ of insulation 2h, carry out sintering, obtain needed microwave dielectric ceramic materials.
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| CN110436894B (en) * | 2019-06-27 | 2022-10-21 | 深圳顺络电子股份有限公司 | Low-dielectric-constant LTCC material and preparation method thereof |
| CN111187062B (en) * | 2020-01-13 | 2022-03-01 | 杭州电子科技大学 | CaSnSiO5-K2MoO4Base composite ceramic microwave material and preparation method thereof |
| CN113004026B (en) * | 2021-04-22 | 2023-01-13 | 无锡市高宇晟新材料科技有限公司 | LTCC microwave dielectric ceramic material and manufacturing method thereof |
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