CN102142591B - Microwave dielectric resonator, manufacturing method thereof and microwave dielectric duplexer - Google Patents
Microwave dielectric resonator, manufacturing method thereof and microwave dielectric duplexer Download PDFInfo
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- CN102142591B CN102142591B CN201010532141XA CN201010532141A CN102142591B CN 102142591 B CN102142591 B CN 102142591B CN 201010532141X A CN201010532141X A CN 201010532141XA CN 201010532141 A CN201010532141 A CN 201010532141A CN 102142591 B CN102142591 B CN 102142591B
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Abstract
The embodiment of the invention discloses a microwave dielectric resonator, a manufacturing method thereof and a microwave dielectric duplexer. The manufacturing method of the microwave dielectric resonator comprises the steps of: mixing main materials according to a set proportion and carrying out ball milling to obtain first mixed powder, wherein the main materials include Mg(OH)2, CaCO3 and TiO2; mixing trace additives according to a set proportion and carrying out ball milling or sand milling to obtain second mixed powder, wherein the trace additives include ZrO2, NbO and Yi2O5; mixing the first mixed powder and the second mixed powder, carrying out ball milling or sand milling and granulating to obtain third mixed powder; and carrying out die-casting formation and sintering on the third mixed powder to obtain the microwave dielectric resonator. By means of the embodiment of the invention, the advantages of reducing sintering temperature, improving sintering compactness and improving Q-value property and the frequency stability of the microwave dielectric resonator are achieved.
Description
Technical field
The embodiment of the present invention relates to communication technical field, relates in particular to a kind of microwave dielectric resonator and manufacture method thereof and microwave-medium duplexer.
Background technology
Microwave dielectric resonator has quality factor (Quality; Be called for short: Q) be worth the remarkable advantages such as high, that frequency stability is good.Microwave dielectric resonator generally comprises: transverse electric and magnetic field (Transverse Electric and Magnetic Field; Be called for short: TEM) pattern, transverse magnetic field (Transverse Magnetic Field; Be called for short: TM) pattern and transverse electric field (Transverse Electric Field; Be called for short: TE) pattern.Along with the development of communications industry, the microwave dielectric resonator of TEM pattern comprises that at various communicating terminals the aspects such as mobile phone, mobile phone, intercom are used widely.Because communication base station is higher for the Q value requirement of microwave-medium, for example: require the Q value to be greater than 6500, resonance frequency reaches 1908MHZ, but the microwave dielectric resonator of TM pattern can't reach the requirement of communication base station application due to the restriction of material and manufacture craft always.
The technology formation of microwave dielectric resonator mainly comprises microwave ceramic material formula, material and dielectric resonator manufacture craft.Aspect the material of the microwave dielectric resonator of TM pattern, the microwave dielectric material that the dielectric constant of take is " 21 " left and right is example, the microwave dielectric material that mainly comprises Ba-Mg-Ta system, Ba-Mn-Ta system, but the selling at exorbitant prices due to Ta, apply in batches limited, aspect mobile phone terminal, mainly use the microwave dielectric material of Mg-Ca-Ti system.In addition, the indium addition system of microwave dielectric material is ZnO or SiO
2Deng or seldom add trace and help the burning material.The Q value performance of the microwave dielectric material of existing TM pattern is generally between 3000~5000.In the technique manufacture process of microwave dielectric resonator, ball milling adopts common ball milling dispersing mode more, adopts greater particle size as 6.5mm or above single abrading-ball; In sintering process, exist residual carbon phenomenon in various degree as 0.5%~2% carbon residual phenomena.
Because the interpolation indium addition system that has microwave dielectric resonator now mainly comprises ZnO, SiO
2Deng the cooling glass material, cause Q value performance and the frequency stability of microwave dielectric resonator low; If reduce ZnO or SiO in order to improve Q value performance
2Addition, cause the sintering difficulty large, densified sintering product is poor.
Summary of the invention
The invention provides a kind of microwave dielectric resonator and manufacture method thereof and microwave-medium duplexer, low in order to the Q value performance and the frequency stability that solve microwave dielectric resonator of the prior art, the sintering difficulty of manufacture process is large, the poor defect of densified sintering product, the Q value performance and the frequency stability that improve microwave dielectric resonator are low, reduce sintering temperature, improve densified sintering product.
The embodiment of the present invention provides a kind of manufacture method of microwave dielectric resonator, comprising:
Main material, according to preset proportion mixing and ball milling or sand milling, is obtained to the first mixed powder, and described main material comprises Mg (OH)
2, CaCO
3And TiO
2
Minute addition, according to the preset proportion mixing and ball milling, is obtained to the second mixed powder, and described minute addition comprises ZrO
2, NbO and Y
2O
5
By granulation after described the first mixed powder and the second mixed powder mixing and ball milling or sand milling, obtain the 3rd mixed powder;
Described the 3rd mixed powder is obtained to microwave dielectric resonator through die cast and sintering.
The microwave dielectric resonator that the embodiment of the present invention also provides a kind of manufacture method of the arbitrary described microwave dielectric resonator provided according to the embodiment of the present invention to make.
The embodiment of the present invention also provides a kind of microwave-medium duplexer, comprising: any one microwave dielectric resonator that the embodiment of the present invention provides.
Microwave dielectric resonator provided by the invention and manufacture method thereof and microwave-medium duplexer, the main material of manufacturing microwave dielectric resonator comprises Mg (OH)
2, CaCO
3And TiO
2, minute addition comprises ZrO
2, NbO and Y
2O
5, can reduce sintering temperature, improve densified sintering product, suppress the aggregative growth of indivedual crystal grain, control the consistency of compactness and crystal grain, improve Q value performance and the frequency stability of microwave dielectric resonator; Not containing the cooling glass material, further improve Q value performance and the frequency stability of microwave dielectric resonator in minute addition.
The accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, below will the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain according to these accompanying drawings other accompanying drawing.
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 1 provides for the embodiment of the present invention one;
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 2 provides for the embodiment of the present invention two;
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 3 provides for the embodiment of the present invention three;
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 4 provides for the embodiment of the present invention four;
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 5 provides for the embodiment of the present invention five.
Embodiment
For the purpose, technical scheme and the advantage that make the embodiment of the present invention clearer, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making under the creative work prerequisite the every other embodiment obtained, belong to the scope of protection of the invention.
Embodiment mono-
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 1 provides for the embodiment of the present invention one, as shown in Figure 1, the manufacture method of this microwave dielectric resonator comprises the following steps:
The main material that the present embodiment is manufactured microwave dielectric resonator comprises Mg (OH)
2, CaCO
3And TiO
2, minute addition comprises ZrO
2, NbO and Y
2O
5, can reduce sintering temperature, improve densified sintering product, suppress the aggregative growth of indivedual crystal grain, control the consistency of compactness and crystal grain, improve Q value performance and the frequency stability of microwave dielectric resonator; Not containing the cooling glass material, further improve Q value performance and the frequency stability of microwave dielectric resonator in minute addition.
Embodiment bis-
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 2 provides for the embodiment of the present invention two, as shown in Figure 2, on the basis of above-described embodiment, the step 101 of the manufacture method of this microwave dielectric resonator specifically comprises the following steps:
The main material that the present embodiment is manufactured microwave dielectric resonator comprises Mg (OH)
2, CaCO
3And TiO
2, minute addition comprises ZrO
2, NbO and Y
2O
5, sintering is easy and compactness good, can improve Q value performance and the frequency stability of microwave dielectric resonator; Not containing the cooling glass material, further improve Q value performance and the frequency stability of microwave dielectric resonator in minute addition.
Embodiment tri-
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 3 provides for the embodiment of the present invention three, as shown in Figure 3, on the basis of above-described embodiment, the step 102 of the manufacture method of this microwave dielectric resonator specifically comprises the following steps:
Wherein, in minute addition, can also comprise: Al
2O
3And SiO
2, described Al
2O
3Shared ratio is 0~2%, described SiO
2Shared ratio is 0~2%.Al in the embodiment of the present invention
2O
3And SiO
2Can select powder on form.
The main material that the present embodiment is manufactured microwave dielectric resonator comprises Mg (OH)
2, CaCO
3And TiO
2, minute addition comprises ZrO
2, NbO and Y
2O
5Can reduce sintering temperature, improve densified sintering product, the aggregative growth that suppresses indivedual crystal grain, control the consistency of compactness and crystal grain, improve Q value and the frequency stability of microwave dielectric resonator, for example: the microwave dielectric resonator that the dielectric constant that adopts the manufacture method manufacture of embodiment of the present invention microwave dielectric resonator is " 21 ", can reach more than 6500 in specific single chamber test Q value performance, meet the demand of communication base station to meagre dielectric resonator; Not containing the cooling glass material, further improve Q value performance and the frequency stability of microwave dielectric resonator in minute addition; In addition, because minute addition comprises ZrO
2, NbO and Y
2O
5Even add a small amount of cooling glass material SiO
2, also very little on Q value performance and frequency stability impact.
Embodiment tetra-
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 4 provides for the embodiment of the present invention four, as shown in Figure 4, on the basis of above-described embodiment, the step 103 of the manufacture method of this microwave dielectric resonator specifically comprises the following steps:
The main material that the present embodiment is manufactured microwave dielectric resonator comprises Mg (OH)
2, CaCO
3And TiO
2, minute addition comprises ZrO
2, NbO and Y
2O
5, can reduce sintering temperature, improve densified sintering product, suppress the aggregative growth of indivedual crystal grain, control the consistency of compactness and crystal grain, improve Q value performance and the frequency stability of microwave dielectric resonator; Not containing the cooling glass material, further improve Q value performance and the frequency stability of microwave dielectric resonator in minute addition; In addition, because minute addition comprises ZrO
2, NbO and Y
2O
5Even add a small amount of cooling glass material SiO
2, also very little on Q value performance and frequency stability impact; Add organic dispersing agent before adding PVA, can improve powder dispersity, reduce the powder reuniting phenomenon.
Embodiment five
The flow chart of the manufacture method of the microwave dielectric resonator that Fig. 5 provides for the embodiment of the present invention five, as shown in Figure 5, on the basis of above-described embodiment, the step 104 of the manufacture method of this microwave dielectric resonator specifically comprises the following steps:
The pressure of step 501, employing 20MPa~200MPa, by described the 3rd mixed powder die cast, obtain base substrate;
The main material that the present embodiment is manufactured microwave dielectric resonator comprises Mg (OH)
2, CaCO
3And TiO
2, minute addition comprises ZrO
2, NbO and Y
2O
5, can reduce sintering temperature, improve densified sintering product, suppress the aggregative growth of indivedual crystal grain, control the consistency of compactness and crystal grain, improve Q value performance and the frequency stability of microwave dielectric resonator; Not containing the cooling glass material, further improve Q value performance and the frequency stability of microwave dielectric resonator in minute addition; In addition, because minute addition comprises ZrO
2, NbO and Y
2O
5Even add a small amount of cooling glass material SiO
2, also very little on Q value performance and frequency stability impact; Add organic dispersing agent before adding PVA, can improve powder dispersity, reduce the powder reuniting phenomenon; In sintering process, advance gurgling in the process of sintered body and pass into moisture, can promote the organic substance of intensification section to get rid of, the carbon after the minimizing sintering is residual, further improves the Q value performance of microwave dielectric resonator.
In the process of all mixing and ball milling in above-described embodiment, the zirconia ball of an above different-grain diameter or cylinder can be mixed to use, wherein, described zirconia ball or cylinder particle size range are 1.5mm~6.5mm.For example: adopting 2 particle diameters in the mixed once mechanical milling process is that 1.5mm, 1 particle diameter are 4mm, a zirconia ball that particle diameter is 6.5mm; Perhaps in the mixed once mechanical milling process, adopt 6 zirconia balls that particle diameter is 1.5mm, adopt 2 zirconia balls that particle diameter is 4mm in another mixing and ball milling process.In embodiment of the present invention mixing and ball milling process, different-grain diameter ball or cylinder are used in collocation, can improve the dispersion effect of mixing and ball milling, guarantee the normal distribution of powder granularity.In order further to optimize the dispersion effect of mixing and ball milling, guarantee the normal distribution of powder granularity, can also adjust the parameters such as time of mixing and ball milling and abrading-ball rotating speed.
Embodiment six
The microwave dielectric resonator that the embodiment of the present invention six provides can adopt the manufacture method of any one microwave dielectric resonator in the embodiment of the present invention to make.
The main material that the present embodiment is manufactured microwave dielectric resonator comprises Mg (OH)
2, CaCO
3And TiO
2, minute addition comprises ZrO
2, NbO and Y
2O
5, can reduce sintering temperature, improve densified sintering product, suppress the aggregative growth of indivedual crystal grain, control the consistency of compactness and crystal grain, improve Q value performance and the frequency stability of microwave dielectric resonator; Not containing the cooling glass material, further improve Q value performance and the frequency stability of microwave dielectric resonator in minute addition; In addition, because minute addition comprises ZrO
2, NbO and Y
2O
5Even add a small amount of cooling glass material SiO
2, also very little on Q value performance and frequency stability impact.
Embodiment seven
The embodiment of the present invention seven provides a kind of microwave-medium duplexer, comprising: any one microwave dielectric resonator that the embodiment of the present invention provides.Microwave dielectric resonator is the core component of microwave-medium duplexer, and the miniaturization provided in the embodiment of the present invention, the microwave-medium duplexer of low-power consumption can be provided the duplexer of communication base station.
The main material that the microwave dielectric resonator manufacture of the present embodiment microwave-medium duplexer adopts comprises Mg (OH)
2, CaCO
3And TiO
2, minute addition comprises ZrO
2, NbO and Y
2O
5, can reduce sintering temperature, improve densified sintering product, suppress the aggregative growth of indivedual crystal grain, control the consistency of compactness and crystal grain, improve Q value performance and the frequency stability of microwave dielectric resonator; Not containing the cooling glass material, further improve Q value performance and the frequency stability of microwave dielectric resonator in minute addition; In addition, because minute addition comprises ZrO
2, NbO and Y
2O
5Even add a small amount of cooling glass material SiO
2, also very little on Q value performance and frequency stability impact.
Finally it should be noted that: above embodiment only, in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: its technical scheme that still can put down in writing aforementioned each embodiment is modified, or part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (10)
1. the manufacture method of a microwave dielectric resonator, is characterized in that, comprising:
Main material, according to preset proportion mixing and ball milling or sand milling, is obtained to the first mixed powder, and described main material comprises Mg (OH)
2, CaCO
3And TiO
2, the mass ratio of described main material is Mg (OH)
2: 30%~45%, CaCO
3: 2%~10%, TiO
2: 45%~65%;
Minute addition, according to the preset proportion mixing and ball milling, is obtained to the second mixed powder, and described minute addition comprises ZrO
2, NbO and Y
2O
5, the mass ratio of described minute addition is ZrO
2: 0~2%, NbO:0~2%, Y
2O
5: 0~2%;
By granulation after described the first mixed powder and the second mixed powder mixing and ball milling or sand milling, obtain the 3rd mixed powder;
Described the 3rd mixed powder is obtained to microwave dielectric resonator through die cast and sintering.
2. the manufacture method of microwave dielectric resonator according to claim 1, is characterized in that, described by main material according to preset proportion mixing and ball milling or sand milling, obtain the first mixed powder, described main material comprises Mg (OH)
2, CaCO
3And TiO
2, be specially:
Main material is added in ball grinder according to preset proportion, and described main material comprises Mg (OH)
2, CaCO
3And TiO
2, wherein said Mg (OH)
2Shared mass ratio is 30%~45%, described CaCO
3Shared mass ratio is 2%~10%, described TiO
2Shared mass ratio is 45%~65%;
Add water in the ball grinder that has added described main material;
By described main material and water, mixing and ball milling in ball grinder was taken out and is drained after 2~10 hours from ball grinder;
The powder sintering that will take out at 1000~1300 degree 2~6 hours;
Add in ball grinder again the powder after sintering and water to mixing and ball milling 2~10 hours, or, after the powder after sintering is added in sand mill to sand milling 5~20 times, dry and obtain described the first mixed powder.
3. the manufacture method of microwave dielectric resonator according to claim 2, is characterized in that, described by minute addition according to the preset proportion mixing and ball milling, obtain the second mixed powder, described minute addition comprises ZrO
2, NbO and Y
2O
5, be specially:
Minute addition is added in ball grinder according to preset proportion, and described minute addition comprises ZrO
2, NbO and Y
2O
5Wherein said ZrO
2Shared mass ratio is 0~2%; Described Y
2O
5Shared mass ratio is 0~2%; The shared mass ratio of described NbO is 0~2%;
Add water in the ball grinder that has added described minute addition;
By described minute addition and water, mixing and ball milling in ball grinder was taken out and is drained after 2~10 hours from ball grinder;
The powder sintering that will take out at 1000~1200 degree 2~5 hours;
Adding in ball grinder the powder after sintering and water to mixing and ball milling again, after 2~10 hours, dries and obtains the second mixed powder.
4. the manufacture method of microwave dielectric resonator according to claim 3, is characterized in that, described minute addition also comprises: Al
2O
3And SiO
2, described Al
2O
3Shared ratio is 0~2%, described SiO
2Shared ratio is 0~2%.
5. according to the manufacture method of claim 2,3 or 4 described microwave dielectric resonators, it is characterized in that, by granulation after described the first mixed powder and the second mixed powder mixing and ball milling or sand milling, obtain the 3rd mixed powder, be specially:
Described the first mixed powder is added in ball grinder or sand mill;
Add water in the ball grinder that has added described the first mixed powder or sand mill;
By described the first mixed powder and water mixing and ball milling 1~5 hour for the first time in ball grinder, or in sand mill sand milling 5~20 times for the first time;
Add described the second mixed powder in the ball grinder after mixing and ball milling for the first time or sand mill;
Add organic dispersing agent in the ball grinder that has added described the second mixed powder or sand mill, the shared mass ratio of the content of described organic dispersing agent is 0.5%~1%;
By powder, the second mixed powder and organic dispersing agent after mixing and ball milling for the first time mixing and ball milling 1~5 hour for the second time in ball grinder, or at sand mill sand milling 5~20 times for the second time;
Add the poly-vinyl alcohol solution that concentration is 0.5% in the described ball grinder after mixing and ball milling for the second time or sand mill;
By the powder after mixing and ball milling for the second time and described poly-vinyl alcohol solution in ball grinder mixing and ball milling 1~5 hour or in sand mill mist projection granulating after sand milling 5~20 times, obtain the 3rd mixed powder.
6. the manufacture method of microwave dielectric resonator according to claim 5, is characterized in that, described organic dispersing agent is ammonium polymethacrylate.
7. the manufacture method of microwave dielectric resonator according to claim 1, is characterized in that, described described the 3rd mixed powder obtained to microwave dielectric resonator through die cast and sintering, is specially:
Adopt the pressure of 20MPa~200MPa, by described the 3rd mixed powder die cast, obtain base substrate;
Spend and pass under the condition of moisture 1000~1400, the described base substrate of sintering obtains microwave ceramics medium, and wherein, the pass of the temperature and time of described sintering is: at room temperature~1000 degree sintering 5~10 hours; Spend sintering 2~6 hours 1000~1400, the water temperature range that described moisture advances gurgling is: 30~40 degree;
Silver, silver ink firing and test are polished, draped over one's shoulders to described microwave ceramics medium, obtained described microwave dielectric resonator.
8. according to the manufacture method of the arbitrary described microwave dielectric resonator of claim 1-4, it is characterized in that: in described mixing and ball milling process, the zirconia ball of an above different-grain diameter or cylinder are mixed to use, and described zirconia ball or cylinder particle size range are 1.5mm~6.5mm.
9. the microwave dielectric resonator made according to the manufacture method of the arbitrary described microwave dielectric resonator of claim 1-8.
10. a microwave-medium duplexer, is characterized in that, comprising: microwave dielectric resonator claimed in claim 9.
Priority Applications (6)
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CN201010532141XA CN102142591B (en) | 2010-11-01 | 2010-11-01 | Microwave dielectric resonator, manufacturing method thereof and microwave dielectric duplexer |
BRPI1106087A BRPI1106087A2 (en) | 2010-11-01 | 2011-05-12 | microwave dielectric resonator, method for producing the same and microwave dielectric duplexer. |
PCT/CN2011/073991 WO2012058916A1 (en) | 2010-11-01 | 2011-05-12 | Microwave dielectric resonator, preparation method thereof, and microwave dielectric duplexer |
HU1200482A HUP1200482A2 (en) | 2010-11-01 | 2011-05-12 | Microwave dielectric resonator, preparation method thereof, and microwave dielectric duplexer |
CN201180001287.4A CN102318135B (en) | 2010-11-01 | 2011-05-12 | Microwave dielectric resonator, production method thereof, and microwave dielectric duplexer |
MX2011012653A MX2011012653A (en) | 2010-11-01 | 2011-05-12 | Microwave dielectric resonator, preparation method thereof, and microwave dielectric duplexer. |
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CN201010532141XA CN102142591B (en) | 2010-11-01 | 2010-11-01 | Microwave dielectric resonator, manufacturing method thereof and microwave dielectric duplexer |
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BR (1) | BRPI1106087A2 (en) |
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CN105000884A (en) * | 2015-08-18 | 2015-10-28 | 广东国华新材料科技股份有限公司 | Microwave dielectric ceramic material as well as preparation method and application thereof |
CN112898006A (en) * | 2021-03-22 | 2021-06-04 | 江苏启诚磁业有限公司 | Preparation process of permanent magnetic ferrite ball milling mixing material |
CN112939595B (en) * | 2021-04-06 | 2022-11-11 | 厦门松元电子股份有限公司 | Microwave dielectric ceramic material with near-zero temperature coefficient at high temperature and preparation method thereof |
CN115849876B (en) * | 2022-12-28 | 2023-11-24 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Low-temperature sintered medium-low dielectric low-loss microwave dielectric ceramic and preparation method thereof |
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JP2002029837A (en) * | 2000-07-12 | 2002-01-29 | Murata Mfg Co Ltd | Dielectric porcelain composition for high frequency, dielectric resonator, dielectric filter, dielectric duplexer and communication appliance |
US6723673B2 (en) * | 2000-08-31 | 2004-04-20 | Mra Laboratories, Inc. | High dielectric constant very low fired X7R ceramic capacitor, and powder for making |
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BRPI1106087A2 (en) | 2016-05-10 |
CN102318135B (en) | 2014-04-30 |
WO2012058916A1 (en) | 2012-05-10 |
CN102318135A (en) | 2012-01-11 |
MX2011012653A (en) | 2012-07-04 |
HUP1200482A2 (en) | 2013-01-28 |
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