CN102531581A - Microwave dielectric ceramic with intermediate dielectric constant and high Q value and preparation method thereof - Google Patents
Microwave dielectric ceramic with intermediate dielectric constant and high Q value and preparation method thereof Download PDFInfo
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- CN102531581A CN102531581A CN2011104571501A CN201110457150A CN102531581A CN 102531581 A CN102531581 A CN 102531581A CN 2011104571501 A CN2011104571501 A CN 2011104571501A CN 201110457150 A CN201110457150 A CN 201110457150A CN 102531581 A CN102531581 A CN 102531581A
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Abstract
The invention belongs to the technical field of material science and more particularly relates to a microwave dielectric ceramic with an intermediate dielectric constant and a high Q value and a preparation method thereof. The expression formula of the microwave dielectric ceramic with the intermediate dielectric constant and the high Q value is as follows: xCaasr1-aTiO3-(1-x)SmbY(1-b)AlO3+y wt% of BO, wherein BO is one or mixture of more of MnO2, WO3, CeO2, Nb2O5, TiO2, Fe2O3 and Ta2O3; x is more than or equal to 0.6 and is less than or equal to 0.8, a is more than or equal to 0.01 and is less than or equal to 0.2, b is more than or equal to 0.4 and less than or equal to 1, and y is more than or equal to 0 and is less than or equal to 3. The microwave dielectric ceramic provided by the invention has the characteristics of intermediate dielectric constant, high Q value, adjustable temperature coefficient of resonance frequency and the like; the dielectric constant is 42-50 and the Qf value is 30000-40000 GHz; the serialization of the temperature coefficient of the resonance frequency can be realized and Tf is more than or equal to -10 and is less than or equal to +10 ppm, so that the microwave dielectric ceramic provided by the invention can be used for manufacturing microwave frequency devices with high powder and high stability, including a filter, a duplexer, a combiner and the like. Therefore, the microwave dielectric ceramic with the intermediate dielectric constant and the high Q value and the preparation method thereof, provided by the invention, have a great application value in industry.
Description
Technical field
The invention belongs to materials science field, relate in particular to the high Q value of a kind of medium dielectric constant microwave medium microwave-medium ceramics and preparation method thereof.
Background technology
Microwave-medium ceramics is one type and is applied to microwave frequency band (300MHz~300GHz), in Circuits System, bring into play the pottery of a series of circuit functions such as media isolated, Medium Wave Guide and dielectric resonance.The resonator, wave filter, antenna, the duplexer equifrequent device that make with microwave-medium ceramics can be widely used in various fields such as radio communication, satellite-signal reception, various radar system, global satellite-signal navigationsystem; The tremendous development of communication base station, digital TV receiving system etc. in recent years particularly, centering dielectric constant and high Q value microwave-medium ceramics demand is increasing, and also have higher requirement simultaneously: specific inductivity should be bigger, to reduce the size of devices size; The Qf value should be high more good more, to reduce the dielectric loss of microwave device; Temperature coefficient of resonance frequency is answered seriation, to satisfy the variant prodn demand, reaches the stability of product with the temperature variation performance.
At present, the high Q value of reported medium dielectric constant microwave medium microwave dielectric material system and dielectric properties are following: (1) BaTi
4O
9, ε
r≈ 38, Qf=30000~40000GHz,
τ f ≈+14ppm/ ℃; (2) Ba
2Ti
9O
20, ε
r≈ 39, Qf=32000~40000GHz,
τ f ≈ 4ppm/ ℃; (3) (Zr, Sn) TiO
4, ε
r≈ 37~39, Qf=32000~40000GHz,
τ f ≈-4~+ 12ppm/ ℃.Above-mentioned materials ε
rAll below 40, in order to prepare ε
rGreater than 40, high Q value microwave dielectric ceramic materials, the present invention selects big specific inductivity (Ca, Sr) TiO for use
3Material and high Q value (Sm, Y) AlO
3Material carries out compound, successfully prepares ε
rThe high Q value of=42~50 medium dielectric constant microwave medium microwave dielectric material.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a purpose that provides provides and a kind of specific inductivity is 42~50, high Q value, the high Q value of medium dielectric constant microwave medium microwave-medium ceramics that temperature coefficient of resonance frequency is adjustable.Another object of the present invention provides a kind of preparation method of the above-mentioned high Q value of medium dielectric constant microwave medium microwave-medium ceramics.
In order to realize first above-mentioned purpose, the technical scheme that the present invention adopted is following:
The high Q value of a kind of medium dielectric constant microwave medium microwave-medium ceramics, the composition of raw materials expression formula of this microwave-medium ceramics is: xCa
aSr
1-aTiO
3+ (1-x) Sm
bY
(1-b)AlO
3+ ywt%BO; Wherein,
0.6≤x≤0.8;
0.01≤a≤0.3;
0.4≤b≤1;
0≤y≤3, y is for accounting for xCaTi
aO
3+ (1-x) Sm
bY
(1-b)AlO
3Mass percent;
Said BO is MnO
2, WO
3, CeO
2, Nb
2O
5, TiO
2, Fe
2O
3, Ta
2O
3In one or more mix.
As preferably, 0.68≤x in the composition of raw materials of above-mentioned microwave-medium ceramics≤0.75; 0.01≤a≤0.2; 0.6≤b≤0.9; 0≤y≤1.
Remake to preferably 0.01≤a in the composition of raw materials of above-mentioned microwave-medium ceramics≤0.05; 0.6≤b≤0.8; 0≤y≤0.7.
In order to realize second above-mentioned purpose, the technical scheme that the present invention adopted is following:
The high Q value of above-mentioned medium dielectric constant microwave medium microwave-medium ceramics preparation method, this method be successively as follows:
1) with starting material CaCO
3, SrCO
3, TiO
2, Sm
2O
3, Y
2O
3And Al
2O
3Heat-treated 2 hours at 400 ℃~1000 ℃;
2) with CaCO
3, SrCO
3, TiO
2Press Ca
aSr
1-aTiO
3The chemical formula batching, the wet ball-milling method was mixed 18~30 hours, and the oven dry back is at 1100~1200 ℃, and pre-burning is 2.5~3.5 hours in the air atmosphere, synthetic Ca
aSr
1-aTiO
3
3) with Sm
2O
3, Y
2O
3And Al
2O
3Press Sm
bY
(1-b)AlO
3The chemical formula batching, the wet ball-milling method was mixed 18~30 hours, and the oven dry back is at 1150~1300 ℃, and pre-burning is 2.5~3.5 hours in the air atmosphere, synthetic Sm
bY
(1-b)AlO
3
4) with synthetic Ca
aSr
1-aTiO
3, Sm
bY
(1-b)AlO
3Press described prescription second batch with starting material BO, mixed 18~30 hours, obtain porcelain after the oven dry with the wet ball-milling method; Add the granulation of 5wt% poly (vinyl alcohol) binder to this porcelain, at 4~6MPa pressure pressed disk, at 1400~1500 ℃, sintering is 3~8 hours in the air atmosphere, obtains the high Q value of described medium dielectric constant microwave medium microwave dielectric ceramic materials.
The present invention who adopts above-mentioned prescription and technology to form is through SrCO
3Part replaces CaCO
3, guaranteeing effectively to have improved specific inductivity under the bigger situation of Qf value; Pass through Y
2O
3Part replaces Sm
2O
3, can effectively improve the Q value; The introducing that oxide compound BO is an amount of can effectively improve the Q value and be lowered into the burning temperature; The present invention can obtain ε
r=42~50, the Qf value is 30000~40000 GHz, temperature coefficient of resonance frequency is adjustable (10≤Tf≤+ 10ppm) microwave dielectric ceramic materials.Through starting material are heat-treated, can effectively improve powder purity in the technology of the present invention, reach the purpose that improves the Qf value with active; This material technology process is easy to control, and favorable reproducibility is applicable to scale operation.
Description of drawings
Fig. 1 is the SEM figure of embodiment 4 obtained porcelain body sections.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
At first with starting material CaCO
3, SrCO
3, TiO
2, Sm
2O
3, Y
2O
3And Al
2O
3Heat-treated 2 hours at 400 ℃~1000 ℃.
Secondly with CaCO
3, SrCO
3, TiO
2Press Ca
aSr
1-aTiO
3The chemical formula batching, the wet ball-milling method was mixed 18~30 hours, and the oven dry back is at 1100~1200 ℃, and pre-burning is 3 hours in the air atmosphere, synthetic Ca
aSr
1-aTiO
3With Sm
2O
3, Y
2O
3And Al
2O
3Press Sm
bY
(1-b)AlO
3The chemical formula batching, the wet ball-milling method was mixed 18~30 hours, and the oven dry back is at 1150~1300 ℃, and pre-burning is 3 hours in the air atmosphere, synthetic Sm
bY
(1-b)AlO
3
Then with synthetic Ca
aSr
1-aTiO
3, Sm
bY
(1-b)AlO
3Press the described prescription second batch of claim 1 with starting material BO, mixed 18~30 hours, obtain porcelain after the oven dry with the wet ball-milling method.Add the granulation of 5wt% Z 150PH (PVA) tackiness agent to this porcelain; Press down at 5MPa pressure and to process diameter 20mm, the disk of thickness 11~13mm is at 1400~1500 ℃; Sintering is 3~8 hours in the air atmosphere, obtains the high Q value of medium dielectric constant microwave medium microwave dielectric ceramic materials.
Table 1 shows and constitutes prescription composition of the present invention, and table 2 shows corresponding processing condition and dielectric properties.
Table 1 prescription is formed
Table 2 processing condition and dielectric properties
Numbering | Thermal treatment temp (℃) | One-tenth burning temperature (℃) | ε r | Qf | Tf |
1 | 400 | 1500 | 42.5 | 42000 | -1.7 |
2 | 400 | 1500 | 42.6 | 41200 | -2.1 |
3 | 400 | 1500 | 43.1 | 40200 | 0.1 |
4 | 600 | 1480 | 44.5 | 40000 | 1.1 |
5 | 600 | 1480 | 45.2 | 39600 | 2.5 |
6 | 600 | 1480 | 45.8 | 39000 | 3.0 |
7 | 800 | 1450 | 47.5 | 34600 | 4.1 |
8 | 800 | 1480 | 46.8 | 38200 | 3.5 |
9 | 800 | 1450 | 47.0 | 35800 | 3.8 |
10 | 800 | 1450 | 47.1 | 34800 | 3.6 |
11 | 1000 | 1450 | 47.3 | 33000 | 3.5 |
12 | 1000 | 1450 | 47.7 | 33900 | 3.8 |
(result is as shown in Figure 1 for scanning electron microscope, the SEM) microscopic appearance of observation embodiment 4 porcelain body sections with sem.As can be seen from the figure, the porcelain body section is fine and close, and the existence of a small amount of small pore is only arranged, and meets the fine and close characteristic of high Q material porcelain body.
The foregoing description has been illustrated technical conceive of the present invention and characteristics, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change and modify, and all should be encompassed within protection scope of the present invention.
Claims (4)
1. the high Q value of a medium dielectric constant microwave medium microwave-medium ceramics is characterized in that the composition of raw materials expression formula of this microwave-medium ceramics is: xCa
aSr
1-aTiO
3+ (1-x) Sm
bY
(1-b)AlO
3+ ywt%BO; Wherein,
0.6≤x≤0.8;
0.01≤a≤0.3;
0.4≤b≤1;
0≤y≤3, y is for accounting for xCaTi
aO
3+ (1-x) Sm
bY
(1-b)AlO
3Mass percent;
Said BO is MnO
2, WO
3, CeO
2, Nb
2O
5, TiO
2, Fe
2O
3, Ta
2O
3In one or more mix.
2. the high Q value of a kind of medium dielectric constant microwave medium according to claim 1 microwave-medium ceramics is characterized in that 0.68≤x≤0.75 in the composition of raw materials of this microwave-medium ceramics; 0.01≤a≤0.2; 0.6≤b≤0.9; 0≤y≤1.
3. the high Q value of a kind of medium dielectric constant microwave medium according to claim 2 microwave-medium ceramics is characterized in that 0.01≤a≤0.05 in the composition of raw materials of this microwave-medium ceramics; 0.6≤b≤0.8; 0≤y≤0.7.
4. preparation method who prepares like claim 1 or the high Q value of 2 or 3 described medium dielectric constant microwave medium microwave-medium ceramics is characterized in that this method is successively as follows:
1) with starting material CaCO
3, SrCO
3, TiO
2, Sm
2O
3, Y
2O
3And Al
2O
3Heat-treated 2 hours at 400 ℃~1000 ℃;
2) with CaCO
3, SrCO
3, TiO
2Press Ca
aSr
1-aTiO
3The chemical formula batching, the wet ball-milling method was mixed 18~30 hours, and the oven dry back is at 1100~1200 ℃, and pre-burning is 2.5~3.5 hours in the air atmosphere, synthetic Ca
aSr
1-aTiO
3
3) with Sm
2O
3, Y
2O
3And Al
2O
3Press Sm
bY
(1-b)AlO
3The chemical formula batching, the wet ball-milling method was mixed 18~30 hours, and the oven dry back is at 1150~1300 ℃, and pre-burning is 2.5~3.5 hours in the air atmosphere, synthetic Sm
bY
(1-b)AlO
3
4) with synthetic Ca
aSr
1-aTiO
3, Sm
bY
(1-b)AlO
3Press described prescription second batch with starting material BO, mixed 18~30 hours, obtain porcelain after the oven dry with the wet ball-milling method; Add the granulation of 5wt% poly (vinyl alcohol) binder to this porcelain, at 4~6MPa pressure pressed disk, at 1400~1500 ℃, sintering is 3~8 hours in the air atmosphere, obtains the high Q value of described medium dielectric constant microwave medium microwave dielectric ceramic materials.
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CN104211397A (en) * | 2014-09-16 | 2014-12-17 | 桂林理工大学 | Temperature stable type microwave dielectric ceramic Nb2VY3O12 with ultralow dielectric constant |
CN104211391A (en) * | 2014-09-27 | 2014-12-17 | 桂林理工大学 | Low-temperature sintering temperature-stable medium dielectric constant microwave dielectric ceramic Bi3La5Ti7O26 and preparation method thereof |
CN104311029A (en) * | 2014-09-27 | 2015-01-28 | 桂林理工大学 | Temperature-stable type microwave dielectric ceramic Bi<2>La<4>Ti<5>O19 having middle dielectric constant |
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C56 | Change in the name or address of the patentee | ||
CP03 | Change of name, title or address |
Address after: 314003 Jiaxing City, Zhejiang Province Economic Development Zone Yong Wui street is the original Road No. 66 Patentee after: Jiaxing Jiali Electronic Co., Ltd. Address before: 314003 Jiaxing Economic Development Zone, Tong Tong Street is the original road, No. 66, No. Patentee before: Jiaxing Jiali Electronic Co., Ltd. |