CN100584796C - Y2O3-TiO2 series microwave dielectric ceramic and preparation method thereof - Google Patents
Y2O3-TiO2 series microwave dielectric ceramic and preparation method thereof Download PDFInfo
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- CN100584796C CN100584796C CN200710135176A CN200710135176A CN100584796C CN 100584796 C CN100584796 C CN 100584796C CN 200710135176 A CN200710135176 A CN 200710135176A CN 200710135176 A CN200710135176 A CN 200710135176A CN 100584796 C CN100584796 C CN 100584796C
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- 239000000919 ceramic Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 14
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000004567 concrete Substances 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 4
- 239000013078 crystal Substances 0.000 abstract 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- 238000002791 soaking Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 238000004891 communication Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- ZACYQVZHFIYKMW-UHFFFAOYSA-N iridium titanium Chemical compound [Ti].[Ir] ZACYQVZHFIYKMW-UHFFFAOYSA-N 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 238000009702 powder compression Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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Abstract
The invention relates to Y2O3-TiO2 serial microwave dielectric ceramics and a preparation method thereof. The raw materials of Y2O3, TiO2 and Bi2O3 are weighted in proportions, mixed, milled, dried, pre-sintered, pressed to be molded and sintered to obtain the microwave dielectric ceramics. The main crystal phase is Yi2Ti2O7 pyrochlore structure. The pure Y2O3-TiO2 serial produced through the invention is provided with good dielectric performance and is a middle dielectric constant microwave medium with perfect performances. When Bi2O3 is doped in the pure Y2O3-TiO2 microwave dielectric ceramics, the sintering temperature of the pure Y2O3-TiO2 microwave dielectric ceramics is obviously lowered, the dielectric constant is obviously improved, and low dielectric loss is maintained.
Description
Technical field
The present invention relates to a kind of medium dielectric constant microwave medium microwave-medium ceramics and preparation method, it mainly is applicable to the dielectric resonance device of microwave military radar and communication system; Relate in particular to a kind of Y
2O
3-TiO
2Series microwave dielectric ceramic and preparation method thereof.
Background technology
In the size of dwindling circuit and improve on its performance, this just requires microwave-medium ceramics should have high DIELECTRIC CONSTANT r to the planner of modern mobile communication and Satellite Communication System, low dielectric loss target tightening.The medium dielectric constant microwave medium microwave-medium ceramics is mainly used in the dielectric resonance device of microwave military radar and communication system, and its Essential Performance Requirements is: specific inductivity is 30～80, and dielectric loss is low as far as possible.People drop into more and more high-end medium dielectric constant microwave medium microwave-medium ceramics (specific inductivity 42～80) and pay close attention at present, and existing high-end medium dielectric constant microwave medium microwave-medium ceramics system is few, and the research field of the medium dielectric constant microwave medium microwave-medium ceramics system of specific inductivity about 40～50 also belongs to blank at present.Study more BaO-TiO at present
2(ε
r=9.8) be (Zr, Sn) TiO
4(ε r=40.0) is BiNbO
4(ε r=39.0) be etc. in the dielectric microwave-medium ceramics generally exist dielectric loss bigger, problems such as phase composite complexity.Therefore, the medium dielectric constant microwave medium stupalith of preparation dielectric properties excellence also needs further research.
Summary of the invention
The objective of the invention is for improve existing in dielectric microwave-medium ceramics dielectric loss bigger, problem such as phase composite complexity and proposed a kind of new Y
2O
3-TiO
2It is the medium dielectric constant microwave medium microwave-medium ceramics.Another object of the present invention provides the preparation method of above-mentioned microwave-medium ceramics.
Technical scheme of the present invention is: a kind of Y
2O
3-TiO
2It is as follows that series microwave dielectric ceramic, its raw material each component and each component account for the molar percentage of raw material total amount:
The material component molar percentage
Y
2O
3 25～50％
Bi
2O
3 0～7％。
Above-mentioned microwave-medium ceramics, its principal crystalline phase are Yi
2Ti
2O
7Pyrochlore constitution.
The present invention also provides the preparation method of above-mentioned microwave-medium ceramics, and its concrete steps are as follows:
A, take by weighing each raw material according to the above ratio; Mix the back ball milling, oven dry, pre-burning is regrinded;
B, in the powder that above-mentioned ball milling is crossed, add binding agent, grind granulation about 1～3 hour then, sieve, and with powder compression moulding;
C, forming composition is heated up sintering and insulation, furnace cooling then.
Wherein ball mill is preferably the roller milling machine in the steps A, adopts wet ball grinding 16～24 hours; Regrind about 6 hours; 3～3.5 ℃/min of pre-burning temperature rise rate in the steps A, calcined temperature are 900 ℃～1200 ℃, and the pre-burning time is 2h～8h.
Binding agent described in the step B is for being polyvinyl alcohol (PVA) or Xylo-Mucine (CMC), and its add-on is to account for 7～10% of raw material total mass; Sieve among the step B with 80 mesh sieve, moulding process is dry-pressing formed.Be shaped to circle or other shape thin slices.
3～3.5 ℃/min of temperature rise rate among the step C, sintering temperature is 1260～1460 ℃, soaking time 2h～8h.
The prepared pure Y of the present invention
2O
3-TiO
2The system dielectric properties are (ε better
rBe 32～52, Q is 3427～8519), be the comparatively excellent medium dielectric constant microwave medium microwave-medium of a kind of performance.And by doping Bi
2O
3The pure Y in back
2O
3-TiO
2The sintering temperature of microwave-medium ceramics obviously reduces (1280～1340 ℃), and specific inductivity is significantly improved, and has kept lower dielectric loss (ε
rBe about 62～73, Q is 3597～8000).
Find that through experimental study the principal crystalline phase of this system all is the Y of pyrochlore constitution
2Ti
2O
7, second is mutually less, easily prepares one-component ceramic under suitable stoichiometric ratio and sintering process.Except improving dielectric properties, owing to add Bi
2O
3Reduced pure Y
2O
3-TiO
2Ceramic sintering temperature, this has very big promoter action for reducing in the energy dissipation.
Beneficial effect:
1. the invention provides a kind of new medium dielectric constant microwave medium system microwave-medium ceramics---pure Y of dielectric properties excellence
2O
3-TiO
2Series microwave dielectric ceramic (ε r=32～52) has been filled up the blank in the medium dielectric constant microwave medium microwave-medium ceramics architectural study field of specific inductivity about 40～50.
2 the present invention by doping vario-property after dielectric properties be improved (ε r=62～73), and sintering temperature (1280～1340 ℃) reduces, and saved the energy and improved practicality.
2. compliance with environmental protection requirements of the present invention, nontoxicity, environmentally safe.
3. material crystalline phase of the present invention is formed single, and second is mutually less, easily prepares one-component ceramic.
4. the present invention helps improving the comprehensive utilization ratio of rare earth resources, slows down Y
2O
3The surplus relatively of rare earth oxide.
Description of drawings
Fig. 1 different B i
2O
3The adulterated Y of content
2Ti
2O
7The XRD figure spectrum of pottery.
Embodiment
The invention will be further described below in conjunction with embodiment, but should not limit protection scope of the present invention with this.
The composition of 9 specific embodiments of 1 doping vario-property iridium titanium microwave dielectric ceramic materials of the present invention is as shown in table 1:
Table 1
| Component (mol%) 1 # 2 # 3 # 4 # 5 # 6 # BiO2 0 0 0 3.3 5 6.67 Y 2O 3 40 33.3 28.57 30 28.32 6.67 TiO 260 66.7 71.43., 66.7 66.7 66.7 sintering temperatures (℃) 1,420 1,460 1,480 1,320 1,320 1280 |
Embodiment 1
#:
Form as in the table 11
#Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 16 hours.
3. after the raw material stoving in 1050 ℃, air atmosphere pre-burning 5h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 1 hour in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1420 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 3h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method
rAnd quality factor q.Dielectric properties are as follows: ε
r=32, Qf=3564.
Embodiment 2
#:
Form as in the table 12
#Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 18 hours.
3. after the raw material stoving in 1100 ℃, air atmosphere pre-burning 3h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) again on planetary mills.
5. the ratio adding concentration in 8wt% is the PVA binding agent of 7wt%, grinds granulation in about 1 hour in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 8wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1460 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method
rAnd quality factor q.Dielectric properties are as follows: ε
r=51, Qf=8519.
Embodiment 3
#:
Form as in the table 13
#Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1200 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 3 hours in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1480 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 5h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method
rAnd quality factor q.Dielectric properties are as follows: ε
r=52, Qf=3427.
Execute example 4
#:
Form as in the table 14
#Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 16 hours.
3. after the raw material stoving in 1050 ℃, air atmosphere pre-burning 5h, 3 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 9wt% is the PVA binding agent of 7wt%, grinds granulation in about 3 hours in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 9wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1320 ℃, sintering in the air atmosphere, 3.5 ℃/min of temperature rise rate, soaking time 3h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method
rAnd quality factor q.Dielectric properties are as follows: ε
r=62, Qf=3597.
Embodiment 5
#:
Form as in the table 15
#Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 18 hours.
3. after the raw material stoving in 1100 ℃, air atmosphere pre-burning 3h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 10wt% is the PVA binding agent of 7wt%, grinds granulation in about 3 hours in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 10wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1320 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 2h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method
rAnd quality factor q.Dielectric properties are as follows: ε
r=67, Qf=8000.
Embodiment 6
#:
Form as in the table 16
#Shown in, concrete preparation method comprises the following steps:
1. calculate the weight percent of raw material by the molar percentage (mol%) of the composition of selecting raw material, take by weighing raw material then.
2. the sample that weighs up is placed ball grinder, wet ball grinding 24 hours.
3. after the raw material stoving in 1200 ℃, air atmosphere pre-burning 2h, 3.5 ℃/min of temperature rise rate lowers the temperature with stove then.
4. with the material of pre-burning, wet ball grinding 6 hours (300 rev/mins) on planetary mills.
5. the ratio adding concentration in 7wt% is the PVA binding agent of 7wt%, grinds granulation in about 3 hours in agate mortar, crosses 80 mesh sieves.
6. the powder that will be mixed with 7wt%PVA with powder compressing machine is pressed into thick one by one about 3mm, and the thin discs of diameter 13mm, pressure are about 100MPa.
7. with disk at 1280 ℃, sintering in the air atmosphere, 3 ℃/min of temperature rise rate, soaking time 6h lowers the temperature with stove then.
Test result to this microwave dielectric ceramic materials is as follows:
With the sample surfaces polishing, adopt Agilient 8722ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method
rAnd quality factor q.Dielectric properties are as follows: ε
r=73, Qf=7518.
Claims (3)
1, a kind of Y
2O
3-TiO
2It is as follows that series microwave dielectric ceramic, its raw material each component and each component account for the molar percentage of raw material total amount:
The material component molar percentage
Y
2O
3 28.3～30％
TiO
2 66.7％
Bi
2O
3 3.3～5％。
2, microwave-medium ceramics according to claim 1 is characterized in that its principal crystalline phase is Y
2Ti
2O
7Pyrochlore constitution.
3, a kind of preparation method of microwave-medium ceramics as claimed in claim 1, its concrete steps are as follows:
A, take by weighing each raw material according to the above ratio; Mixed driving roll formula ball mill wet ball grinding 16～24 hours, oven dry with 3～3.5 ℃/min of temperature rise rate, is warming up to 900 ℃～1200 ℃, and pre-burning 2h～8h regrinds;
B, in the powder that above-mentioned ball milling is crossed, add binding agent, grind granulation in 1～3 hour then, cross 80 mesh sieves, and powder is dry-pressing formed; Wherein said binding agent is polyvinyl alcohol or Xylo-Mucine, and its add-on is to account for 7～10% of raw material total mass;
C, forming composition is heated up with 3～3.5 ℃/min of speed, rise to 1260～1460 ℃ of sintering, and insulation 2h～8h, furnace cooling then.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102153342B (en) * | 2010-12-27 | 2013-02-06 | 南京工业大学 | Composite doped modified Y2Ti2O7 microwave medium ceramic material |
| CN102659406B (en) * | 2012-05-23 | 2013-10-30 | 南京工业大学 | Nd2O3-TiO2 system microwave dielectric ceramic and preparation method of Nd2O3-TiO2 microwave dielectric ceramic |
| CN102659408A (en) * | 2012-05-23 | 2012-09-12 | 南京工业大学 | La2O3-TiO2 system microwave medium ceramic and preparation method thereof |
| CN103714880B (en) * | 2013-12-10 | 2016-04-06 | 西安理工大学 | Prevent ceramic material and the spraying method of high-voltage line surface corona and pollution flashover |
| CN104528813B (en) * | 2014-12-04 | 2016-07-27 | 西南科技大学 | A kind of Y2Ti2O7The SHS process of pyrochlore and densifying method |
| CN108220737B (en) * | 2018-01-11 | 2019-12-24 | 中南大学 | Metal ceramic with negative dielectric constant and preparation method thereof |
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Non-Patent Citations (2)
| Title |
|---|
| Pressure-induced order-disorder transitions in pyrochloreRE2Ti2O7 (RE=Y, Gd). F.X. Zhang,B. Manoun, S.K. Saxena.Materials Letters,Vol.第60卷 . 2006 |
| Pressure-induced order-disorder transitions in pyrochloreRE2Ti2O7 (RE=Y, Gd). F.X. Zhang,B. Manoun, S.K. Saxena.Materials Letters,Vol.第60卷 . 2006 * |
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