CN103936409B - A kind of microwave dielectric ceramic materials and preparation method thereof - Google Patents
A kind of microwave dielectric ceramic materials and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 37
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 17
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 17
- 229910002367 SrTiO Inorganic materials 0.000 claims description 16
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 9
- 239000011572 manganese Substances 0.000 claims description 8
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 2
- 238000011056 performance test Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000011812 mixed powder Substances 0.000 abstract 1
- 239000006104 solid solution Substances 0.000 abstract 1
- 238000005498 polishing Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
Abstract
The present invention discloses a kind of microwave dielectric ceramic materials and preparation method thereof, this material main component (Ca
0.6sr
0.4)
xtiO
3(Li
0.5sm
0.5)
1-xtiO
3combination solid solution.Preparation method is: first synthesize (the Ca that Li compensates
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder, gained mixed powder is incubated 2-4 hour at 1050-1100 DEG C of temperature and carries out pre-burning, gained pre-burning powder is carried out secondary ball milling and sieves; Add a small amount of MnO again
2, ball milling sieves, and is then pressed into columned base substrate, gained base substrate is incubated 2-4 hour at 1180-1300 DEG C of temperature and sinters porcelain into, must mix Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3microwave dielectric ceramic materials.Performance test shows, this material has superperformance: dielectric constant height ε r > 115, quality factor q
f> 2000GHz, resonance temperature coefficient Jue Dui Zhi ∣ τ
f∣ < 45ppm/ DEG C.Preparation technology is relatively simple, stable.
Description
Technical field
The present invention relates to information functional material technical field, particularly a kind of microwave dielectric ceramic materials and preparation method thereof.
Background technology
Microwave-medium ceramics (MWDC) to refer in microwave frequency band circuit as dielectric layer and completes the pottery of one or more functions, its microwave frequency range is from 300MHz ~ 3000GHz, wavelength is from 1mm to 0.1mm, be the critical material of the microwave devices such as the widely used resonator of modern communications, filter, medium wave circuit, have a wide range of applications in radar, automobile telephone, cordless telephone, gps antenna etc.It has high dielectric constant, and lossy microwave is low, and frequency-temperature coefficient is little waits excellent microwave dielectric property, becomes a focus direction of recent domestic microwave dielectric material research field.
The beginning of the seventies, first the Bryan etc. of the U.S. was developed into the BaTi that dielectric constant is 38
4o
9material, the Ba that temperature stability that then the Bell laboratory development of the U.S. is successful is good
2ti
9o
20, achieve the practical of dielectric resonator, opened the curtain of microwave-medium ceramics development history.
Along with microwave technology constantly pushes the high frequency direction of millimeter wave and submillimeter wave and mobile communication and portable terminal to towards miniaturization, lightweight, integrated, high reliability and low cost future development, find high ε
r, high q-factor and low τ
fnew material become a very active focus in the research of current microwave-medium ceramics.As a kind of high-dielectric constant microwave-medium ceramics material that Chinese invention patent CN102898135A announces and preparation method thereof, with the Ca of high dielectric
0.8sr
0.2tiO
3with the Li with large negative temperature coefficient of resonance frequency
0.5sm
0.5tiO
3the microwave dielectric ceramic materials of high-k is prepared in combination, and this material has higher dielectric constant, but quality factor is less, and temperature coefficient of resonance frequency absolute value is higher.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of high-k, low resonant frequency temperature coefficient, loss are lower, the simple microwave dielectric ceramic materials of technique and preparation method thereof.
The technical scheme solved the problem is: a kind of microwave dielectric ceramic materials, and this microwave-medium ceramics is with CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by expression formula Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3molar ratio is prepared burden, wherein 0.5≤x≤0.7.
The preparation method of above-mentioned microwave dielectric ceramic materials comprises the steps:
(1) synthesize Li and compensate (Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder: with CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by CaTiO
3: SrTiO
3: Sm
2o
3: Li
2cO
3: TiO
2=0.6x:0.4x:(0.5-0.5x): (0.5-0.5x+ δ-δ x): 1 molar ratio mixing, ball milling sieves, and dries, within 2-4 hour, carries out pre-burning, gained powder is carried out secondary ball milling and sieves 1050 ~ 1100 DEG C of insulations, acquisition Li compensation (Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder, wherein, 0.5≤x≤0.7,0 δ≤0.05;
(2) a small amount of manganese dioxide MnO is mixed
2: the Li that step (1) obtains is compensated (Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder is according to (Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3: MnO
2=100:y molar ratio mixing and ball milling, dries mix Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder, wherein 0.04≤y≤0.16;
(3) compressing: what step (2) was obtained mixes Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder adds polyethylene (PVA) and mixes, and dries, is then pressed into cylindric base substrate;
(4) microwave-medium ceramics blank sintering: cylindric for gained base substrate is incubated 2-4 hour at 1180-1300 DEG C of temperature and sinters porcelain into, namely obtains mixing Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3microwave dielectric ceramic materials.
Prepared by the present invention mixes Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3microwave dielectric ceramic materials, performance test shows to obtain good microwave dielectric property: dielectric constant height ε
r> 115, quality factor q
f> 2000GHz, resonance temperature coefficient Jue Dui Zhi ∣ τ
f∣ < 45ppm/ DEG C.Preparation process adopts traditional ceramic preparation technique, and preparation technology is relatively simple, stable, thus has wittrgreat utility and promotion prospect.
Embodiment
Below by embodiment, the invention will be further described, but the present invention is not limited to these embodiments.
Embodiment 1
With CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by expression formula (Ca
0.6sr
0.4)
0.5(Li
0.5sm
0.5)
0.5tiO
3the mixing of molar ratio batching, ball milling sieves, and dries, within 4 hours, carries out pre-burning, gained powder is carried out secondary ball milling and sieves 1050 DEG C of insulations, obtains (Ca
0.6sr
0.4)
0.5(Li
0.5sm
0.5)
0.5tiO
3powder.
At (Ca
0.6sr
0.4)
0.5(Li
0.5sm
0.5)
0.5tiO
3the mass concentration adding some in powder is 7% polyvinyl alcohol (PVA), mix, dry, then cylindric base substrate is pressed into, cylindric for gained base substrate is incubated 4 hours at 1180 DEG C of temperature and sinters porcelain into, the twin polishing of gained microwave-medium ceramics is kept two-sided parallel, then for the test of microwave dielectric property etc.
Performance test shows, the microwave dielectric ceramic materials dielectric property of this embodiment gained are as follows: DIELECTRIC CONSTANT ε
r=115, quality factor q
f=2320GHz, temperature coefficient of resonance frequency τ
f=-44ppm/ DEG C.
Embodiment 2
With CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by expression formula (Ca
0.6sr
0.4)
0.6(Li
0.5sm
0.5)
0.4tiO
3the mixing of molar ratio batching, ball milling sieves, and dries, within 3 hours, carries out pre-burning, gained powder is carried out secondary ball milling and sieves 1100 DEG C of insulations, obtains (Ca
0.6sr
0.4)
0.6(Li
0.5sm
0.5)
0.4tiO
3powder.
At Ca
0.6sr
0.4)
0.6(Li
0.5sm
0.5)
0.4tiO
3the mass concentration adding some in powder is 7% polyvinyl alcohol (PVA), mix, dry, then cylindric base substrate is pressed into, cylindric for gained base substrate is incubated 3 hours at 1250 DEG C of temperature and sinters porcelain into, the twin polishing of gained microwave-medium ceramics is kept two-sided parallel, then for the test of microwave dielectric property etc.
Performance test shows, the microwave dielectric ceramic materials dielectric property of this embodiment gained are as follows: DIELECTRIC CONSTANT ε
r=128, quality factor q
f=2278GHz, temperature coefficient of resonance frequency τ
f=-22ppm/ DEG C.
Embodiment 3
Get variable x=0.7, δ in preparation process (1)=0.05, with CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by CaTiO
3: SrTiO
3: Sm
2o
3: Li
2cO
3: TiO
2=0.42:0.28:0.15:(0.15+0.015): 1 molar ratio mixing, is that medium carries out ball milling with absolute ethyl alcohol, within 4 hours, carries out pre-burning, obtain (the Ca of x=0.7, δ=0.05 after oven dry 1050 DEG C of insulations
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3powder.
To (Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3the polyvinyl alcohol (PVA) of 7% is added in powder, mix, dry, then cylindric base substrate is pressed into, cylindric for gained base substrate is incubated 3 hours at 1260 DEG C of temperature and sinters porcelain into, the twin polishing of gained microwave-medium ceramics is kept two-sided parallel, then for the test of microwave dielectric property etc.
Performance test shows, the microwave dielectric ceramic materials dielectric property of this embodiment gained are as follows: dielectric constant=130, quality factor q
f=2143GHz, temperature coefficient of resonance frequency τ
f=-19ppm/ DEG C.
Embodiment 4
With CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by expression formula (Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3the mixing of molar ratio batching, ball milling sieves, and dries, within 4 hours, carries out pre-burning, gained powder is carried out secondary ball milling and sieves 1100 DEG C of insulations, obtains (Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3powder.
At (Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3the mass concentration adding some in powder is 7% polyvinyl alcohol (PVA), mix, dry, then cylindric base substrate is pressed into, cylindric for gained base substrate is incubated 2 hours at 1300 DEG C of temperature and sinters porcelain into, the twin polishing of gained microwave-medium ceramics is kept two-sided parallel, then for the test of microwave dielectric property etc.
Performance test shows, the microwave dielectric ceramic materials dielectric property of this embodiment gained are as follows: DIELECTRIC CONSTANT ε
r=134, quality factor q
f=2043GHz, temperature coefficient of resonance frequency τ
f=-8ppm/ DEG C.
Embodiment 5
Get variable x=0.7, δ in preparation process (1)=0.04, with CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by CaTiO
3: SrTiO
3: Sm
2o
3: Li
2cO
3: TiO
2=0.42:0.28:0.15:(0.15+0.012): 1 molar ratio mixing, is that medium carries out ball milling with absolute ethyl alcohol, within 2 hours, carries out pre-burning, obtain (the Ca of x=0.7, δ=0.04 after oven dry 1070 DEG C of insulations
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3powder.
To (the Ca of x=0.7, δ=0.04
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3a small amount of MnO is mixed in powder
2, get the variable y=0.04 of preparation process (2), then according to Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3: MnO
2=100:0.04 molar ratio mixing and ball milling, dry x=0.7, δ=0.04 mix MnO
2ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3powder
MnO is mixed to x=0.7, δ=0.04
2(Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3the polyvinyl alcohol (PVA) of 7% is added in powder, mix, dry, then cylindric base substrate is pressed into, cylindric for gained base substrate is incubated 2 hours at 1200 DEG C of temperature and sinters porcelain into, the twin polishing of gained microwave-medium ceramics is kept two-sided parallel, then for the test of microwave dielectric property etc.
Performance test shows, the microwave dielectric ceramic materials dielectric property of this embodiment gained are as follows: DIELECTRIC CONSTANT ε
r=125, quality factor q
f=2443GHz, temperature coefficient of resonance frequency τ
f=-20ppm/ DEG C.
Embodiment 6
Get variable x=0.7, δ in preparation process (1)=0.03, with CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by CaTiO
3: SrTiO
3: Sm
2o
3: Li
2cO
3: TiO
2=0.42:0.28:0.15:(0.15+0.009): 1 molar ratio mixing, is that medium carries out ball milling with absolute ethyl alcohol, within 2 hours, carries out pre-burning, obtain (the Ca of x=0.7, δ=0.03 after oven dry 1070 DEG C of insulations
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3powder.
To (the Ca of x=0.7, δ=0.03
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3a small amount of MnO is mixed in powder
2, get the variable y=0.08 of preparation process (2), then according to (Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3: MnO
2=100:0.08 molar ratio mixing and ball milling, dry x=0.7, δ=0.03 mix MnO
2(Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3powder
MnO is mixed to x=0.7, δ=0.03
2(Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3the polyvinyl alcohol (PVA) of 7% is added in powder, mix, dry, then cylindric base substrate is pressed into, cylindric for gained base substrate is incubated 4 hours at 1230 DEG C of temperature and sinters porcelain into, the twin polishing of gained microwave-medium ceramics is kept two-sided parallel, then for the test of microwave dielectric property etc.
Performance test shows, the microwave dielectric ceramic materials dielectric property of this embodiment gained are as follows: DIELECTRIC CONSTANT ε
r=138, quality factor q
f=2745GHz, temperature coefficient of resonance frequency τ
f=-4ppm/ DEG C.
Embodiment 7
Get variable x=0.7, δ in preparation process (1)=0.05, with CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by CaTiO
3: SrTiO
3: Sm
2o
3: Li
2cO
3: TiO
2=0.42:0.28:0.15:(0.15+0.015): 1 molar ratio mixing, is that medium carries out ball milling with absolute ethyl alcohol, within 4 hours, carries out pre-burning, obtain the Ca of x=0.7, δ=0.05 after oven dry 1050 DEG C of insulations
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3powder.
To (the Ca of x=0.7, δ=0.05
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3a small amount of MnO is mixed in powder
2, get the variable y=0.16 of preparation process (2), then according to Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3: MnO
2=100:0.08 molar ratio mixing and ball milling, dry x=0.7, δ=0.05 mix MnO
2(Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.
3tiO
3powder
MnO is mixed to x=0.7, δ=0.05
2(Ca
0.6sr
0.4)
0.7(Li
0.5sm
0.5)
0.3tiO
3the polyvinyl alcohol (PVA) of 7% is added in powder, mix, dry, then cylindric base substrate is pressed into, cylindric for gained base substrate is incubated 3 hours at 1290 DEG C of temperature and sinters porcelain into, the twin polishing of gained microwave-medium ceramics is kept two-sided parallel, then for the test of microwave dielectric property etc.
Performance test shows, the microwave dielectric ceramic materials dielectric property of this embodiment gained are as follows: DIELECTRIC CONSTANT ε
r=140, quality factor q
f=2323GHz, temperature coefficient of resonance frequency τ
f=5ppm/ DEG C.
Claims (2)
1. a preparation method for microwave dielectric ceramic materials, is characterized in that, comprises the steps:
(1) synthesize Li and compensate (Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder: with CaTiO
3, SrTiO
3, Sm
2o
3, Li
2cO
3and TiO
2for raw material, by CaTiO
3: SrTiO
3: Sm
2o
3: Li
2cO
3: TiO
2=0.6x:0.4x:(0.5-0.5x): (0.5-0.5x+ δ-δ x): 1 molar ratio mixing, ball milling sieves, and dries, within 2-4 hour, carries out pre-burning, gained powder is carried out secondary ball milling and sieves 1050 ~ 1100 DEG C of insulations, acquisition Li compensation (Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder, wherein, 0.5≤x≤0.7,0 ≦ δ≤0.05;
(2) a small amount of manganese dioxide MnO is mixed
2: the Li that step (1) obtains is compensated (Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder is according to (Ca
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3: MnO
2=100:y molar ratio mixing and ball milling, dries mix Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder, wherein 0.04≤y≤0.16;
(3) compressing: what step (2) was obtained mixes Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3powder adds polyvinyl alcohol (PVA) and mixes, and dries, is then pressed into cylindric base substrate;
(4) microwave-medium ceramics blank sintering: cylindric for gained base substrate is incubated 2-4 hour at 1180-1300 DEG C of temperature and sinters porcelain into, namely obtains mixing Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3microwave dielectric ceramic materials.
2. prepare by preparation method according to claim 1 and mix Mn and the (Ca compensated through Li
0.6sr
0.4)
x(Li
0.5sm
0.5)
1-xtiO
3microwave dielectric ceramic materials.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724462A (en) * | 2005-07-04 | 2006-01-25 | 浙江大学 | Low temp sintering (Ca Mg) TiO3 series microwave medium ceramic and its preparation tech |
| CN103274684A (en) * | 2013-06-14 | 2013-09-04 | 桂林电子科技大学 | High-permittivity microwave dielectric ceramics capable of being sintered at medium-low temperature and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724462A (en) * | 2005-07-04 | 2006-01-25 | 浙江大学 | Low temp sintering (Ca Mg) TiO3 series microwave medium ceramic and its preparation tech |
| CN103274684A (en) * | 2013-06-14 | 2013-09-04 | 桂林电子科技大学 | High-permittivity microwave dielectric ceramics capable of being sintered at medium-low temperature and preparation method thereof |
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