CN103833359A - Microwave ceramic dielectric resonator and preparation method thereof - Google Patents

Microwave ceramic dielectric resonator and preparation method thereof Download PDF

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CN103833359A
CN103833359A CN201310222593.1A CN201310222593A CN103833359A CN 103833359 A CN103833359 A CN 103833359A CN 201310222593 A CN201310222593 A CN 201310222593A CN 103833359 A CN103833359 A CN 103833359A
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microwave ceramics
medium resonator
ceramics medium
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ceramic dielectric
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薛冰
薛万荣
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NANJING ZHIYUAN MICROWAVE SCIENCE & TECHNOLOGY Co Ltd
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Abstract

The invention discloses a microwave ceramic dielectric resonator and a preparation method thereof, belonging to the field of electronics. The microwave ceramic dielectric resonator is prepared from the following raw materials in percentage by mass: 5-20% of Al2O3, 10-40% of TiO2, 10-30% of SrO, 10-40% of La2O3, 0.01-0.5% of K2O, 0.1-1% of Na2O, 0.01-1% of Fe2O3, 0.01-2% of SiO2, 0.1-1.5% of MgO, 0.01-1.5% of Cr2O3, 0.1-2% of ZrO2, 0.001-1% of IrO2, 0.1-1% of Sm2O3, 0.001-0.5% of MnO, 0.1-0.5% of Nd2O3, 0.1-1% of V2O5, 0.01-0.5% of CuO, 0.1-0.5% of Pr2O3, 0.01-1.5% of CaO and 0.1-0.8% of Fe3O4. The preparation method comprises the following steps: mixing, synthesizing, grinding, spray granulation, forming and firing. The microwave ceramic dielectric resonator contains a certain quantity of rare-earth oxides, and thus, has the advantages of higher dielectric constant, favorable quality factor, excellent frequency stability, obvious price advantage and very high cost performance.

Description

Microwave ceramics medium resonator and preparation method thereof
Technical field
The invention belongs to telecommunications field, relate to a kind of microwave ceramics medium resonator and preparation method thereof, be specifically related to a kind of cableless communication and wireless network microwave ceramics medium resonator and preparation method thereof.
Background technology
Along with the development of wireless communication technique, more and more higher to the performance requriements of base station in wireless communication networks, its median filter is one of important device.Originally the wave filter in base station is metal cavitg wave filter, in order to improve the performance of wave filter, makes full use of channel resource and volume, has researched and developed the dielectric cavity wave filter that adds microwave ceramics medium resonator in metal chamber.Dielectric cavity wave filter can make original metal chamber wave filter volume-diminished, and performance is improved and makes frequency stability better, can under the power condition of tens watts to thousands of watts, use, and wherein the most key is exactly microwave ceramics medium resonator.
Summary of the invention
It is higher that technical problem to be solved by this invention is to provide a kind of specific inductivity, and quality factor are good, the microwave ceramics medium resonator that frequency stability is superior, and the present invention also provides the preparation method of microwave ceramics medium resonator.
The object of this invention is to provide a kind of microwave ceramics medium resonator.
The object of the invention is to be achieved through the following technical solutions:
A kind of microwave ceramics medium resonator, it is made up of the raw material of following massfraction: 5 ~ 20% Al 2o 3, 10 ~ 40% TiO 2, 10～30% SrO, 10～40% La 2o 3, 0.01～0.5%K 2o, 0.1～1%Na 2o, 0.01～1%Fe 2o 3, 0.01～2%SiO 2, 0.1～1.5%MgO, 0.01～1.5%Cr 2o 3, 0.1～2%ZrO 2, 0.001～1%IrO 2, 0.1～1%Sm 2o 3, 0.001～0.5%MnO, 0.1～0.5%Nd 2o 3, 0.1～1%V 2o 5, 0.01～0.5%CuO, 0.1～0.5%Pr 2o 3, 0.01～1.5%CaO, 0.1～0.8%Fe 3o 4.
Preferably, described microwave ceramics medium resonator, it is made up of the raw material of following massfraction: 5 ~ 15% Al 2o 3, 15 ~ 30% TiO 2, 15～30% SrO, 15～30% La 2o 3, 0.01～0.1%K 2o, 0.1～0.6%Na 2o, 0.01～0.8%Fe 2o 3, 0.05～1.5%SiO 2, 0.1～1.0%MgO, 0.01～1.0%Cr 2o 3, 0.2～1.5%ZrO 2, 0.001～0.5%IrO 2, 0.2～0.6%Sm 2o 3, 0.002～0.3%MnO, 0.1～0.2%Nd 2o 3, 0.1～0.8%V 2o 5, 0.01～0.1%CuO, 0.2～0.3%Pr 2o 3, 0.01～1.0%CaO, 0.1～0.4%Fe 3o 4.
Described microwave ceramics medium resonator, DIELECTRIC CONSTANT ε r=35～43, quality factor q 0=10000～25000, temperature coefficient of resonance frequency τ f=-3～3ppm/ DEG C (45 DEG C～+ 105 DEG C).
Another object of the present invention is to provide the preparation method of microwave ceramics medium resonator, comprises the following steps successively:
1) batch mixing, synthetic: take above-mentioned raw materials component and proportionally mix, calcining once at 1050～1150 DEG C;
2) grind: grind and make fineness reach D90≤1.5 μ m;
3) mist projection granulating: add binding agent to be mixed to get slurry, mist projection granulating;
4) moulding: under 1.0MPa～1.5Mpa, compression moulding obtains green compact;
5) burn till: raw embryo sintering 5～15 hours at 1450～1600 DEG C, obtains ceramic dielectric resonator.
Step 3) in, the binding agent preferred mass mark 5%PVA aqueous solution; Wherein the add-on of binding agent is preferably 8%～15% of raw material total mass.
The present invention also provides the application of microwave ceramics medium resonator at preparation cableless communication microwave ceramics medium resonator and wireless network microwave ceramics medium resonator.
The described microwave ceramics medium resonator for cableless communication is often under relatively high power state, and its structure is made up of two portions: columnar microwave ceramics medium resonator and bracket.Described microwave ceramics medium resonator external diameter (A) 10～100mm for cableless communication, internal diameter (C) 3～20 mm, high (B) 5～50 mm.As operating frequency f owhen=880～3500 MHz, Q=10000～25000, τ f=-3～3ppm/ DEG C (45 DEG C～+ 105 DEG C).
The described residing power of microwave-medium ceramics resonator for wireless network is less, and size is less, is tubular structure, external diameter (A) 10～20 mm, internal diameter (C) 3～8 mm, high (B) 20～40 mm.As operating frequency f owhen=1.8～2.9 GHz, Q=10000～25000, τ f=-3～3ppm/ DEG C (45 ° of C-+105 ° C).
Compared to the prior art, beneficial effect of the present invention:
The rare earth oxide that contains some amount in microwave ceramics medium resonator component of the present invention, not only specific inductivity is higher, and quality factor are good, and frequency stability is superior, and in view of China is rare earth resources big country, price advantage is obvious, has very high cost performance.
Brief description of the drawings
Fig. 1 is the structural representation of cableless communication microwave ceramics medium resonator of the present invention.
Fig. 2 is the structural representation of wireless network microwave ceramics medium resonator of the present invention.
Embodiment
Embodiment 1
Take the raw material of following mass percent: 5% Al 2o 3, 30% TiO 2, 30% SrO, 30% La 2o 3, 0.1% K 2o, 0.1% Na 2o, 0.8% Fe 2o 3, 0.05% SiO 2, 1.0% MgO, 0.05% Cr 2o 3, 0.2% ZrO 2, 0.1% IrO 2, 0.6% Sm 2o 3, 0.3% MnO, 0.2% Nd 2o 3, 0.2% V 2o 5, 0.1% CuO, 0.2% Pr 2o 3, 0.9% CaO, 0.1% Fe 3o 4, mix, in electric furnace, at 1100 DEG C, calcine once; Adopt ball mill grinding, make fineness reach D90≤1.5 μ m; 8% the 5%PVA aqueous solution that adds feed composition quality, is mixed to get slurry, processes slurry and make slurry moisture drying and form spheroidal particle in spray tower; Adopt compression moulding under hydraulic automatic forming machine 1.5Mpa to obtain green compact; Raw embryo is placed in high-temperature electric resistance furnace, and sintering 5 hours at 1450 DEG C obtains the microwave ceramics medium resonator of external diameter 100 mm, internal diameter 20 mm, high 50 mm.
As shown in Figure 1, the microwave ceramics medium resonator 1 making and bracket 2 assemblings obtain the microwave ceramics medium resonator for cableless communication.
Adoption Network analyser and high-low temperature test chamber are tested the cableless communication microwave ceramics medium resonator making, test cavity size 120 × 120 × 90mm, DIELECTRIC CONSTANT ε r=42; f owhen=950 ± 30 MHz, Q=24000 ± 1500, τ f=-3～3ppm/ DEG C (45 ° of C-+105 ° C).
Embodiment 2
Take the raw material of following mass percent: 10% Al 2o 3, 25% TiO 2, 25% SrO, 30% La 2o 3, 0.06% K 2o, 0.6%Na 2o, 0.44%Fe 2o 3, 1.5%SiO 2, 1.0%MgO, 1.0%Cr 2o 3, 1.5%ZrO 2, 0.5%IrO 2, 0.6%Sm 2o 3, 0.3%MnO, 0.2%Nd 2o 3, 0.8%V 2o 5, 0.05%CuO, 0.25%Pr 2o 3, 1.0%CaO, 0.2%Fe 3o 4, mix, in electric furnace, at 1150 DEG C, calcine once; Adopt ball mill grinding, make fineness reach D90≤1.5 μ m; 10% the 5%PVA aqueous solution that adds feed composition quality, is mixed to get slurry, processes slurry and make slurry moisture drying and form spheroidal particle in spray tower; Adopt compression moulding under hydraulic automatic forming machine 1.0MPa to obtain green compact; Raw embryo is placed in high-temperature electric resistance furnace, and sintering 10 hours at 1550 DEG C obtains the microwave ceramics medium resonator of external diameter 50mm, internal diameter 15 mm, high 25 mm.
As shown in Figure 1, the microwave ceramics medium resonator 1 making and bracket 2 assemblings obtain the microwave ceramics medium resonator for cableless communication.
Adoption Network analyser and high-low temperature test chamber enter the capable test of cableless communication microwave ceramics medium resonator to making, and test cavity size: 70 × 70 × 50mm, records: DIELECTRIC CONSTANT ε r=38.5; f owhen=1400 ± 50MHz, Q=22000 ± 1000, τ f=-3～3ppm/ DEG C (45 ° of C-+105 ° C).
Embodiment 3
Take the raw material of following mass percent: 15% Al 2o 3, 30% TiO 2, 30% SrO, 15% La 2o 3, 0.1% K 2o, 0.4% Na 2o, 0.6% Fe 2o 3, 1.2% SiO 2, 1.0% MgO, 1.0% Cr 2o 3, 1.5% ZrO 2, 0.5% IrO 2, 0.6% Sm 2o 3, 0.3% MnO, 0.2% Nd 2o 3, 0.8% V 2o 5, 0.1% CuO, 0.3% Pr 2o 3, 1.0% CaO, 0.4% Fe 3o 4, mix, in electric furnace, at 1100 DEG C, calcine once; Adopt ball mill grinding, make fineness reach D90≤1.5 μ m; 15% the 5%PVA aqueous solution that adds feed composition quality, is mixed to get slurry, processes slurry and make slurry moisture drying and form spheroidal particle in spray tower; Adopt compression moulding under hydraulic automatic forming machine 1.5Mpa to obtain green compact; Raw embryo is placed in high-temperature electric resistance furnace, and sintering 5 hours at 1600 DEG C obtains the microwave ceramics medium resonator of external diameter 10mm, internal diameter 3 mm, high 5 mm.
As shown in Figure 1, the microwave ceramics medium resonator 1 making and bracket 2 assemblings obtain the microwave ceramics medium resonator for cableless communication.
Adoption Network analyser and high-low temperature test chamber are tested the cableless communication microwave ceramics medium resonator making, test cavity size: 20 × 20 × 15mm, DIELECTRIC CONSTANT ε r=41.5; f owhen=3500 ± 50MHz, Q=12000 ± 1500, τ f=-3～3ppm/ DEG C (45 ° of C-+105 ° C).
Embodiment 4
Take the raw material of following mass percent: 12% Al 2o 3, 28% TiO 2, 30% SrO, 25% La 2o 3, 0.1% K 2o, 0.1% Na 2o, 0.8% Fe 2o 3, 0.05% SiO 2, 1.0% MgO, 0.05% Cr 2o 3, 0.2% ZrO 2, 0.1% IrO 2, 0.6% Sm 2o 3, 0.3% MnO, 0.2% Nd 2o 3, 0.2% V 2o 5, 0.1% CuO, 0.2% Pr 2o 3, 0.9% CaO, 0.1% Fe 3o 4, mix, in electric furnace, at 1100 DEG C, calcine once; Adopt ball mill grinding, make fineness reach D90≤1.5 μ m; 8% the 5%PVA aqueous solution that adds feed composition quality, is mixed to get slurry, processes slurry and make slurry moisture drying and form spheroidal particle in spray tower; Adopt compression moulding under hydraulic automatic forming machine 1.5MPa to obtain green compact; Raw embryo is placed in high-temperature electric resistance furnace, and sintering 5 hours at 1450 DEG C obtains the wireless network microwave ceramics medium resonator of the tubular structure of external diameter 20 mm as shown in Figure 2, internal diameter 8 mm, high 32 mm.
Adoption Network analyser and high-low temperature test chamber are tested the wireless network microwave ceramics medium resonator making, test cavity size:
Figure DEST_PATH_GDA0000351174451
, DIELECTRIC CONSTANT ε r=38; f owhen=1.9 ± 0.05GHz, Q=14000 ± 1000, τ f=-3～3ppm/ DEG C (45 ° of C-+105 ° C).
Embodiment 5
Take the raw material of following mass percent: 15% Al 2o 3, 30% TiO 2, 15% SrO, 30% La 2o 3, 0.06% K 2o, 0.6%Na 2o, 0.44%Fe 2o 3, 1.5%SiO 2, 1.0%MgO, 1.0%Cr 2o 3, 1.5%ZrO 2, 0.5%IrO 2, 0.6%Sm 2o 3, 0.3%MnO, 0.2%Nd 2o 3, 0.8%V 2o 5, 0.05%CuO, 0.25%Pr 2o 3, 1.0%CaO, 0.2%Fe 3o 4, mix, in electric furnace, at 1150 DEG C, calcine once; Adopt ball mill grinding, make fineness reach D90≤1.5 μ m; 10% the 5%PVA aqueous solution that adds feed composition quality, is mixed to get slurry, processes slurry and make slurry moisture drying and form spheroidal particle in spray tower; Adopt compression moulding under hydraulic automatic forming machine 1.0MPa to obtain green compact; Raw embryo is placed in high-temperature electric resistance furnace, and sintering 10 hours at 1550 DEG C obtains the wireless network microwave ceramics medium resonator of the tubular structure of external diameter 10mm as shown in Figure 2, internal diameter 3mm, high 20mm.
Adoption Network analyser and high-low temperature test chamber are tested the wireless network microwave ceramics medium resonator making, test cavity size:
Figure DEST_PATH_GDA0000351174452
, DIELECTRIC CONSTANT ε r=42.5; f owhen=2.5 ± 0.05GHz, Q=11000 ± 1000, τ f=-3～3ppm/ DEG C (45 ° of C-+105 ° C).
Embodiment 6
Take the raw material of following mass percent: 15% Al 2o 3, 15% TiO 2, 30% SrO, 30% La 2o 3, 0.1% K 2o, 0.4% Na 2o, 0.6% Fe 2o 3, 1.2% SiO 2, 1.0% MgO, 1.0% Cr 2o 3, 1.5% ZrO 2, 0.5% IrO 2, 0.6% Sm 2o 3, 0.3% MnO, 0.2% Nd 2o 3, 0.8% V 2o 5, 0.1% CuO, 0.3% Pr 2o 3, 1.0% CaO, 0.4% Fe 3o 4, mix, in electric furnace, at 1100 DEG C, calcine once; Adopt ball mill grinding, make fineness reach D90≤1.5 μ m; 15% the 5%PVA aqueous solution that adds feed composition quality, is mixed to get slurry, processes slurry and make slurry moisture drying and form spheroidal particle in spray tower; Adopt compression moulding under hydraulic automatic forming machine 1.5Mpa to obtain green compact; Raw embryo is placed in high-temperature electric resistance furnace, and sintering 5 hours at 1600 DEG C obtains the wireless network microwave ceramics medium resonator of the tubular structure of external diameter 15mm as shown in Figure 2, internal diameter 5mm, high 28mm.
Adoption Network analyser and high-low temperature test chamber are tested the wireless network microwave ceramics medium resonator making, test cavity size: , DIELECTRIC CONSTANT ε r=41.5; f owhen=2.8 ± 0.05GHz, Q=12000 ± 1000, τ f=-3～3ppm/ DEG C (45 ° of C-+105 ° C).

Claims (4)

1. a microwave ceramics medium resonator, is characterized in that it is made up of the raw material of following massfraction: 5 ~ 20% Al 2o 3, 10 ~ 40% TiO 2, 10～30% SrO, 10～40% La 2o 3, 0.01～0.5%K 2o, 0.1～1%Na 2o, 0.01～1%Fe 2o 3, 0.01～2%SiO 2, 0.1～1.5%MgO, 0.01～1.5%Cr 2o 3, 0.1～2%ZrO 2, 0.001～1%IrO 2, 0.1～1%Sm 2o 3, 0.001～0.5%MnO, 0.1～0.5%Nd 2o 3, 0.1～1%V 2o 5, 0.01～0.5%CuO, 0.1～0.5%Pr 2o 3, 0.01～1.5%CaO, 0.1～0.8%Fe 3o 4.
2. microwave ceramics medium resonator according to claim 1, is characterized in that it is made up of the raw material of following massfraction: 5 ~ 15% Al 2o 3, 15 ~ 30% TiO 2, 15～30% SrO, 15～30% La 2o 3, 0.01～0.1%K 2o, 0.1～0.6%Na 2o, 0.01～0.8%Fe 2o 3, 0.05～1.5%SiO 2, 0.1～1.0%MgO, 0.01～1.0%Cr 2o 3, 0.2～1.5%ZrO 2, 0.001～0.5%IrO 2, 0.2～0.6%Sm 2o 3, 0.002～0.3%MnO, 0.1～0.2%Nd 2o 3, 0.1～0.8%V 2o 5, 0.01～0.1%CuO, 0.2～0.3%Pr 2o 3, 0.01～1.0%CaO, 0.1～0.4%Fe 3o 4.
3. the preparation method of the microwave ceramics medium resonator described in claim 1 or 2, is characterized in that comprising the following steps successively:
1) batch mixing, synthetic: take above-mentioned raw materials component and proportionally mix, calcining once at 1050～1150 DEG C;
2) grind: grind and make fineness reach D90≤1.5 μ m;
3) mist projection granulating: add binding agent to be mixed to get slurry, mist projection granulating;
4) moulding: under 1.0MPa～1.5Mpa, compression moulding obtains green compact;
5) burn till: raw embryo sintering 5～15 hours at 1450～1600 DEG C, obtains ceramic dielectric resonator.
4. the preparation method of microwave ceramics medium resonator according to claim 3, is characterized in that step 3) in, described binding agent is the massfraction 5%PVA aqueous solution; Wherein the add-on of binding agent is 8%～15% of raw material total mass.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104446477A (en) * 2014-12-08 2015-03-25 苏州艾福电子通讯有限公司 Microwave dielectric ceramic powder, preparation method thereof, microwave dielectric ceramic and microwave component
CN105198423A (en) * 2015-08-18 2015-12-30 电子科技大学 Sr-La-Al-based microwave dielectric ceramic material and preparation method thereof
CN105837203A (en) * 2016-03-21 2016-08-10 南京智元微波科技有限公司 Microwave ceramic material, dielectric resonator prepared from material and preparation method of dielectric resonator
CN106431388A (en) * 2016-09-22 2017-02-22 深圳方泰新材料技术有限公司 Microwave ceramic dielectric resonator and preparation method and application thereof
CN113248250A (en) * 2021-06-15 2021-08-13 南京瑞基通讯技术有限公司 Microwave ceramic dielectric resonator or microwave dielectric substrate and preparation method thereof

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CN102584214A (en) * 2012-02-14 2012-07-18 郴州功田电子陶瓷技术有限公司 Environment-friendly microwave dielectric ceramic material for small precise antenna
CN102584218A (en) * 2012-02-14 2012-07-18 郴州功田电子陶瓷技术有限公司 Environment-friendly microwave dielectric ceramic for L wave band

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102491734A (en) * 2011-12-08 2012-06-13 福州大学 Medium high-Q microwave dielectric ceramics and preparation method thereof
CN102584214A (en) * 2012-02-14 2012-07-18 郴州功田电子陶瓷技术有限公司 Environment-friendly microwave dielectric ceramic material for small precise antenna
CN102584218A (en) * 2012-02-14 2012-07-18 郴州功田电子陶瓷技术有限公司 Environment-friendly microwave dielectric ceramic for L wave band

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104446477A (en) * 2014-12-08 2015-03-25 苏州艾福电子通讯有限公司 Microwave dielectric ceramic powder, preparation method thereof, microwave dielectric ceramic and microwave component
CN104446477B (en) * 2014-12-08 2016-04-27 苏州艾福电子通讯股份有限公司 Microwave dielectric ceramic powder and method, microwave-medium ceramics, microwave device
CN105198423A (en) * 2015-08-18 2015-12-30 电子科技大学 Sr-La-Al-based microwave dielectric ceramic material and preparation method thereof
CN105837203A (en) * 2016-03-21 2016-08-10 南京智元微波科技有限公司 Microwave ceramic material, dielectric resonator prepared from material and preparation method of dielectric resonator
CN106431388A (en) * 2016-09-22 2017-02-22 深圳方泰新材料技术有限公司 Microwave ceramic dielectric resonator and preparation method and application thereof
CN113248250A (en) * 2021-06-15 2021-08-13 南京瑞基通讯技术有限公司 Microwave ceramic dielectric resonator or microwave dielectric substrate and preparation method thereof

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