CN102515721B - Low-dielectric-constant microwave medium ceramic and preparation method thereof - Google Patents
Low-dielectric-constant microwave medium ceramic and preparation method thereof Download PDFInfo
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- CN102515721B CN102515721B CN201110416939.2A CN201110416939A CN102515721B CN 102515721 B CN102515721 B CN 102515721B CN 201110416939 A CN201110416939 A CN 201110416939A CN 102515721 B CN102515721 B CN 102515721B
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Abstract
The invention discloses a low-dielectric-constant microwave medium ceramic and a preparation method thereof, which belong to the technical field of microwave medium materials and manufacturing thereof. A ceramic material consists of Al2O3, a percent by weight of BaLa2(Zr0.1Ti0.9)4O12, b percent by weight of BaWO4 and c percent by weight of [xBaO+yWO3], wherein a is more than 0 but less than or equal to 20, (b+c) is more than or equal to 0 but less than or equal to 15, and <y/x> is more than or equal to 1 but less than or equal to 2; and a percent by weight, b percent by weight and c percent by weight refer to the percent by weight in Al2O3. The method comprises the following steps of: synthesizing additives, i.e., BaLa2(Zr0.1Ti0.9)4O12 and BaWO4 respectively by using a corresponding oxide and carbonate in a certain molar ratio; mixing the BaLa2(Zr0.1Ti0.9)4O12 and BaWO4 with raw materials including Al2O3, BaCO3 and WO3 according to the ceramic material composition in the scheme in a wet grinding way; drying, and adding polyvinyl alcohol (PVA) for press molding; and sintering in a box type furnace or a tunnel furnace for 1-4 hours to obtain the low-dielectric-constant microwave medium ceramic. The dielectric constant of the microwave medium ceramic is between 9 and 12, and the microwave medium ceramic has the characteristics of capability of meeting a quality factor required by an application and proximity to a zero frequency temperature coefficient; and the low-dielectric-constant microwave medium ceramic can be widely applied to manufacturing of microwave devices such as a broadband medium antenna, and can meet the technical requirements of mobile communication, satellite communication and the Beidou satellite positioning system of China.
Description
Technical field
The invention belongs to microwave dielectric material manufacturing technology field, the low dielectric constant microwave dielectric ceramic material of particularly using for microwave devices such as polyrod antenna such as Navsats in communication system.
Background technology
Microwave dielectric ceramic materials has been widely used in the communication system such as mobile phone, WLAN (wireless local area network) (WLAN), direct broadcasting satellite (DBS) and global positioning system (GPS).Microwave-medium ceramics conventionally should have higher specific inductivity, low high-frequency loss and approach zero temperature coefficient of resonance frequency.In recent years, the Wideband microwave-medium ceramics antenna that adopts microwave dielectric ceramic materials to make is promoted rapidly, becomes the main product of wide-band microwave antenna.Because wide-band microwave media ceramic antenna is mainly used in high-frequency band (>=2GHz), therefore conventionally use the low dielectric constant microwave dielectric material that high frequency performance is good, generally its specific inductivity is below 15.Wherein, specific inductivity is mainly selected aluminum oxide (α-Al at the material of 10 left and right
2o
3), although this material has advantages of good high frequency performance and frequency characteristic factor (Q × f) high, its temperature coefficient of resonance frequency (τ
f) poor, | τ
f| > 30ppm/ ℃, cause antenna to produce and frequently float in severe cold or extremely hot in the situation that, sensitivity declines, and affects the performance of mobile terminal.In addition aluminum oxide (α-Al,
2o
3) sintering temperature of pottery is generally between 1600-1800 ℃, as the critical material of microwave-medium antenna, so high firing temperature is difficult to meet the mass production requirement of factory.Therefore, the frequency temperature stabilization of aluminum oxide and the research of low temperature sintering have caused people's attention.Cheng-Fu Yang etc. are at Material s Letters, and 2003 (57): " Sintering and microwave dielectric characteristics of MCAS glass-added 0.84Al in 2945-2949.
,o
3-0.16TiO
2ceramics " a kind of Al is disclosed in a literary composition
2o
3-TiO
2sosoloid also passes through to add MgO-CaO-SiO
2-Al
2o
3(MCAS) glass, sintering temperature is down to the technical scheme of 1250 ℃, but the specific inductivity of resulting materials has been reduced to 7～8.5, and its frequency characteristic factor (degradation (< 10000GHz) especially of Q × f).YingDai etc. are at Materials Science and Engineer ing A, and 2008 (475): " Effects of MCAS glass additives on dielectric properties of Al in 76-80.
2o
3-TiO
2ceramics " adjust Al in a literary composition
2o
3-TiO
2the preparation method of the component of sosoloid and MCAS glass, is down to 1350 ℃ by sintering temperature, but the specific inductivity of resulting materials has been increased to 11.6～12.3.
Therefore, how keep specific inductivity substantially constant (10 left and right) and frequency characteristic factor (the high advantage of Q × f) simultaneously, improve frequency stability of temperature (realize | τ
f| < 10ppm/ ℃) and reduce material sintering temperature be aluminum oxide as low dielectric constant microwave dielectric ceramic material high volume applications in the key of the microwave devices such as polyrod antenna such as wide-band microwave media ceramic antenna and Navsat.
Summary of the invention
The invention provides a kind of specific inductivity and be the higher and temperature coefficient of resonance frequency of 10 left and right, frequency characteristic factor and approach zero microwave-medium ceramics, and corresponding preparation technology is provided, this production technique and equipment, without particular requirement, are convenient to batch production and application.
Object of the present invention is mainly to overcome Al
2o
3the shortcoming that media ceramic temperature stability is bad, its technical scheme is with Al
2o
3for principal constituent, adopt non-glass phase sintering technology, use BaLa
2(Zr
0.1ti
0.9)
4o
12as positive frequency tc compensation material, use BaWO
4and/or BaO and WO
3as the doping of specific inductivity conditioning agent, to improve the temperature stability of the microwave dielectric property of material system, particularly material.
A kind of dielectric constant microwave ceramic medium, is characterized in that porcelain consists of: Al
2o
3+ awt%BaLa
2(Zr
0.1ti
0.9)
4o
12+ bwt%BaWO
4+ cwt%[xBaO+yWO
3], wherein: 0 < a≤20,0 < b+c≤15,1≤y/x≤2; Awt%, bwt%, cwt% is for accounting for Al
2o
3weight fraction.
The prioritization scheme of above-mentioned composition is: a kind of dielectric constant microwave ceramic medium, is characterized in that porcelain consists of: Al
2o
3+ awt%BaLa
2(Zr
0.1ti
0.9)
4o
12+ bwt%BaWO
4+ cwt%[xBaO+yWO
3], wherein: 0 < a≤12,0 < b+c≤10,1≤y/x≤1.2; Awt%, bwt%, cwt% is for accounting for Al
2o
3weight fraction.
The prioritization scheme of above-mentioned composition is: Al
2o
3+ awt%BaLa
2(Zr
0.1ti
0.9)
4o
12+ bwt%BaWO
4+ cwt%[xBaO+yWO
3], wherein: 0 < a≤10,0 < b+c≤8,0.8≤y/x≤1; Awt%, bwt%, cwt% is for accounting for Al
2o
3weight fraction.
A preparation method for dielectric constant microwave ceramic medium, comprises the following steps:
1. by barium carbonate (BaCO
3), lanthanum sesquioxide (La
2o
3), zirconium dioxide (ZrO
2) and titanium dioxide (TiO
2) 1: 1: 0.4 in molar ratio: 3.6 batchings, be placed in urethane ball milling bucket, add zirconia ball and deionized water ball milling mixings 24h, after oven dry at box-type furnace or continuous tunnel furnace in 1130 ℃ of precalcining 4h, synthesize BaLa
2(Zr
0.1ti
0.9)
4o
12.2it is one of additive in such scheme.
2. by barium carbonate (BaCO
3) and tungstic oxide (WO
3) 1: 1 in molar ratio batching, be placed in urethane ball milling bucket, add zirconia ball and deionized water ball milling mixings 24h, after oven dry at box-type furnace or continuous tunnel furnace in 750 ℃ of precalcining 4h, synthesize BaWO
4, i.e. one of additive in such scheme.
3. by synthetic BaLa
2(Zr
0.1ti
0.9)
4o
12and BaWO
4additive and Al
2o
3, BaCO
3and WO
3raw material carries out ball milling by the porcelain composition described in such scheme and mixes 24～48h, 100 ℃ of oven dry, add the granulation of 5wt% polyvinyl alcohol (PVA) tackiness agent, be pressed in 100～150MPa the circle sheet that diameter 10mm, thickness are 5mm, at box-type furnace or continuous tunnel furnace in 1500～1600 ℃ of sintering, insulation 1～4h, can obtain material of the present invention.
Microwave-medium ceramics of the present invention, its specific inductivity is 9～12, has the feature that can meet the required quality factor of application and approach zero frequency temperature coefficient simultaneously.Microwave-medium ceramics provided by the present invention belongs to the microwave dielectric ceramic materials of low-k, can be used as the key core material of the microwave devices such as Wide-band dielectric antenna, be mainly used in the modern communications industries such as the big-dipper satellite station-keeping system of mobile communication, satellite communications, China, there is important industrial application value.
Embodiment
Table 1 has provided the several specific exampless and the microwave dielectric property thereof that form each component content of the present invention, and the dielectric properties of stupalith are to record under 11～16GHz in frequency.Certainly the scope that these embodiment are not meant to limit the present invention.
Composition, sintering temperature and the dielectric properties of table 1 dielectric constant microwave ceramic medium
Claims (4)
1. a dielectric constant microwave ceramic medium, is characterized in that porcelain consists of: Al
2o
3+ awt%BaLa
2(Zr
0.1ti
0.9)
4o
12+ bwt%BaWO
4+ cwt%[xBaO+yWO
3], wherein: 0 < a≤20,0 < b+c≤15,1≤y/x≤2; Awt%, bwt%, cwt% is for accounting for Al
2o
3weight fraction.
2. a kind of dielectric constant microwave ceramic medium according to claim 1, is characterized in that porcelain consists of: Al
2o
3+ awt%BaLa
2(Zr
0.1ti
0.9)
4o
12+ bwt%BaWO
4+ cwt%[xBaO+yWO
3], wherein: 0 < a≤12,0 < b+c≤10,1≤y/x≤1.2; Awt%, bwt%, cwt% is for accounting for Al
2o
3weight fraction.
3. a kind of dielectric constant microwave ceramic medium according to claim 1, is characterized in that porcelain consists of: Al
2o
3+ awt%BaLa
2(Zr
0.1ti
0.9)
4o
12+ bwt%BaWO
4+ cwt%[xBaO+yWO
3], wherein: 0 < a≤10,0 < b+c≤8,0.8≤y/x≤1; Awt%, bwt%, cwt% is for accounting for Al
2o
3weight fraction.
4. the preparation method of a kind of dielectric constant microwave ceramic medium claimed in claim 1, is characterized in that:
1. by BaCO
3, La
2o
3, ZrO
2and TiO
21: 1: 0.4 in molar ratio: 3.6 batchings, be placed in urethane ball milling bucket, add zirconia ball and deionized water ball milling mixings 24h, after oven dry at box-type furnace or continuous tunnel furnace in 1130 ℃ of precalcining 4h, synthesize BaLa
2(Zr
0.1ti
0.9)
4o
12;
2. by BaCO
3and WO
31: 1 in molar ratio batching, is placed in urethane ball milling bucket, adds zirconia ball and deionized water ball milling mixings 24h, after oven dry at box-type furnace or continuous tunnel furnace in 750 ℃ of precalcining 4h, synthesize BaWO
4;
3. by synthetic BaLa
2(Zr
0.1ti
0.9)
4o
12and BaWO
4additive and Al
2o
3, BaCO
3and WO
3raw material carries out ball milling by described porcelain composition and mixes 24～48h, 100 ℃ of oven dry, add the granulation of 5wt% PVAC polyvinylalcohol tackiness agent, be pressed in 100～150MPa the circle sheet that diameter 10mm, thickness are 5mm, at box-type furnace or continuous tunnel furnace in 1500～1600 ℃ of sintering, insulation 1～4h, can obtain material of the present invention.
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| CN201110416939.2A CN102515721B (en) | 2011-11-25 | 2011-11-25 | Low-dielectric-constant microwave medium ceramic and preparation method thereof |
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| CN102515721B true CN102515721B (en) | 2014-05-21 |
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