CN104402437A - Low-temperature sintered NdNbO4-CaTiO3 series microwave dielectric ceramic and preparation method thereof - Google Patents

Low-temperature sintered NdNbO4-CaTiO3 series microwave dielectric ceramic and preparation method thereof Download PDF

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CN104402437A
CN104402437A CN201410484068.1A CN201410484068A CN104402437A CN 104402437 A CN104402437 A CN 104402437A CN 201410484068 A CN201410484068 A CN 201410484068A CN 104402437 A CN104402437 A CN 104402437A
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张平
赵永贵
宋振坤
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Tianjin University
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Abstract

The invention discloses a low temperature sintered NdNbO4-CaTiO3 series microwave dielectric ceramic, which has a composition of 0.6 wt.% of NdNbO4, m wt.% of CaTiO3 and 0.2-8 wt.% of Bi2O3, wherein M satisfies the relation of 0.2<=m<=8. The method is as below: first preparing the raw materials of Nd2O3 and Nb2O5 according to the NdNbO4 chemical formula; conducting ball milling, drying, sieving and sintering; adding 0.6wt.% of CaTiO3 and 0.2-8 wt% of Bi2O3, and conducting secondary material preparation; then conducting granulation and compacting moulding; and sintering the blank at 950 to 1100 DEG C NdNbO4 CaTiO3 to prepare the low-temperature sintered microwave dielectric ceramic. According to the invention, the sintering temperature is successfully reduced to 1000 DEG C; and the microwave dielectric ceramic has dielectric constant of 20.3, temperature coefficient of resonant frequency of 29.7 ppm / DEG C and quality factor Q*f reaching a maximum of 52780 GHz. The invention has the advantages of simple preparation process and no pollution in the process; and the microwave dielectric material has promising prospects.

Description

Low-temperature sintering NdNbO 4-CaTiO 3series microwave dielectric ceramic and preparation method thereof
Technical field
The invention belongs to electronic information material and components and parts field, particularly relate to a kind of novel high q-factor (quality factor) NdNbO 4-CaTiO 3the low-temperature sintering method of series microwave dielectric ceramic.
Background technology
Along with the fast development of satellite broadcasting and microwave communication techniques, many microwave equipments based on dielectric resonator, and can as independently element application in microwave telecommunication system by good development and application.And electronic information technology is constantly to high frequency and digitizing future development, to the miniaturization of components and parts, integrated so that modular requirement is also more and more urgent.Therefore, the dielectric material of microwave application requires to have high-k, low-dielectric loss and near-zero resonance frequency temperature coefficient, can fire at a lower temperature simultaneously.
Niobate material is important electronic material, has excellent photoelectric properties and non-linear optical property, good optical effect and the peculiar property such as electric property and metacrystal phase boundary, has been widely used in and has manufactured electrical condenser and opto-electronic device.Usually, platinum and Jin Chang are used as the interior electrode of the equipment prepared by high sintering temperature (>1200 DEG C) material.High temperature sintering not only makes preparation process spend to be increased, and wastes more resource.Prepare the research that micro-wave dielectric equipment should be tending towards the material of high energy efficiency and dominance energy, so, reduce the sintering temperature of material, make again the dielectric properties of material not be subject to large impact simultaneously, to lay the foundation with energy consumption for using low-melting base metal (as copper, silver) to reduce costs.
Niobic acid neodymium pottery has perovskite-like scheelite-type structure, has suitable DIELECTRIC CONSTANT ε r(19.6), the temperature coefficient of resonance frequency τ of nearly zero f(-24ppm/ DEG C), but quality factor q × f lower (33000GHz), and sintering temperature is 1250 DEG C.Visible, the lower and higher application that govern niobic acid neodymium microwave-medium ceramics of sintering temperature of quality factor.The present invention adopts conventional solid-state method, with CaTiO 3for additive and Bi 2o 3for sintering aid, prepare high Q niobic acid neodymium series microwave dielectric ceramic, while specific inductivity and temperature coefficient of resonance frequency remain unchanged substantially, improved the quality factor of niobic acid neodymium system pottery, reduce sintering temperature.
The applicant once disclosed a kind of High-quality-factor neodymium niobate microwave dielectric ceramic and preparation method thereof (CN102603296A) in 2012, and this application is with Nd 2o 3, Nb 2o 5for raw material, and add CaF 2as fusing assistant, overcome the defect that quality factor q × f is lower, by solid phase method preparation, there is high quality factor (75000GHz.) niobic acid neodymium series microwave dielectric ceramic.
The applicant also once disclosed another kind of High-quality-factor neodymium niobate microwave dielectric ceramic and preparation method thereof (201310047133X) in 2013, with Nd 2o 3, Nb 2o 5for raw material, add CaTiO 3for additive, adopt conventional solid-state method, provide the niobic acid neodymium microwave-medium ceramics that one has higher figure of merit (70000GHz).The shortcoming of above-mentioned two kinds of niobic acid neodymium microwave-medium ceramics is that sintering temperature is higher, and respectively at 1250 ~ 1300 DEG C and 1200 ~ 1325 DEG C of sintering, the present invention, on this basis, adds Bi 2o 3fusing assistant, makes its sintering temperature obviously reduce (950 ~ 1000 DEG C), and maintains its good dielectric properties, can meet the requirement of practical application.
Summary of the invention
The object of the invention, being that quality factor for overcoming prior art are lower and sintering temperature is higher, govern the shortcoming of niobic acid neodymium microwave-medium ceramics application, provides a kind of with Nd 2o 3, Nb 2o 5for main raw material, with CaTiO 3for additive, with Bi 2o 3for sintering aid, keep the low-temperature sintering high q-factor NdNbO of excellent microwave dielectric property simultaneously 4-CaTiO 3the method of series microwave dielectric ceramic
The present invention is achieved by following technical solution.
A kind of low-temperature sintering NdNbO 4-CaTiO 3series microwave dielectric ceramic, it consists of NdNbO 4-0.6wt.%CaTiO 3-m wt.%Bi 2o 3, wherein, 0.2≤m≤8;
This low-temperature sintering NdNbO 4-CaTiO 3the preparation method of series microwave dielectric ceramic, has following steps:
(1) by chemical feedstocks Nd 2o 3and Nb 2o 5according to NdNbO 4chemical formula weigh batching;
(2) mixed powder of step (1) is put into ball grinder, add deionized water and zirconia ball, ball milling 6 hours; Again by the raw material after ball milling in 110 DEG C of oven dry, cross 40 mesh sieves, obtain evengranular powder;
(3) by the powder after the sieving of step (2) in 950 DEG C of pre-burnings 3 hours, and be incubated 4 hours at this temperature;
(4) to additional 0.6wt.%CaTiO in the ceramic powder after the pre-burning of step (3) 3, and the low melting point sintering aid Bi of 0.2 ~ 8wt% 2o 3, second batch.
(5) powder of step (4) second batch is put into ball grinder, add deionized water and zirconia ball, ball milling 6 ~ 12 hours, after drying, additional mass percent is that the paraffin of 6 ~ 10% is as tackiness agent granulation, cross 80 mesh sieves, be pressed into base substrate with powder compressing machine;
(6) by the base substrate of step (5) in 950 ~ 1100 DEG C of sintering, be incubated 2 ~ 6 hours, make low-temperature sintering high q-factor NdNbO 4-CaTiO 3series microwave dielectric ceramic;
(7) by the microwave property of network analyzer test article.
The raw material of described step (1) is analytical pure raw material.
The base substrate of described step (5) is the green body cylinders of Φ 10mm × 5mm.
The pressure of the powder compressing machine of described step (5) is 4 ~ 6Mpa.
Described step (5) sintering temperature is 1000 DEG C.
The present invention is with NdNbO 4based on-series microwave dielectric ceramic, adopt conventional solid-state method, add 0.6wt.%CaTiO 3additive improves quality factor effectively; Add Bi 2o 3for sintering aid, successfully its sintering temperature is reduced to 1000 DEG C.
When sintering temperature is 1000 DEG C, soaking time 4h, Bi 2o 3doping when being 5wt.%, specific inductivity is 20.3, and temperature coefficient of resonance frequency is-29.7ppm/ DEG C, and quality factor q × f reaches and is 52,780GHz to the maximum.In addition, preparation technology of the present invention is simple, and process is pollution-free, improves its dielectric properties, reduces sintering temperature, is the promising microwave dielectric material of a kind of tool.
Embodiment
The raw material Nd that the present invention adopts 2o 3, Nb 2o 5, CaTiO 3and Bi 2o 3be analytical pure raw material, purity is greater than 99.9%, and specific embodiment is as follows:
Embodiment 1
(1) by Nd 2o 3, Nb 2o 5nd in molar ratio 2o 3: Nb 2o 5=1:1 is configured to main powder.
(2) mixed powder of main powder is put into ball grinder, add deionized water and zirconia ball, ball milling 6 hours on planetary ball mill, then the raw material after ball milling is dried in 110 DEG C of loft drier, after oven dry, raw material is crossed 40 mesh sieves.
(3) powder pre-burning 3 hours at 950 DEG C of will cross sieve, and be incubated 4 hours at this temperature.
(4) the powder 20g after pre-burning is taken, additional 0.6wt.%CaTiO 3and 5.0wt%Bi 2o 3, second batch.
(5) above-mentioned second batch gained powder is put into ball grinder, add deionized water and zirconia ball, ball milling 8 hours, after oven dry, additional mass percent is that the paraffin of 8% is as tackiness agent granulation again, cross 80 mesh sieves, depress to the green body cylinders of Φ 10mm × 5mm with powder compressing machine with the pressure of 6MPa.
(6) by green body cylinders in 1000 DEG C of sintering, be incubated 4 hours, make low-temperature sintering high q-factor NdNbO 4-CaTiO 3series microwave dielectric ceramic.
(7) by the microwave property of network analyzer test article: specific inductivity is 20.3, quality factor q × f is 52,780GHz, and temperature coefficient of resonance frequency is-29.7ppm/ DEG C.
Embodiment 2
(1) by Nd 2o 3, Nb 2o 5nd in molar ratio 2o 3: Nb 2o 5=1:1 is configured to main powder.
(2) mixed powder of main powder is put into ball grinder, add deionized water and zirconia ball, ball milling 6 hours on planetary ball mill, then the raw material after ball milling is dried in 110 DEG C of loft drier, after oven dry, raw material is crossed 40 mesh sieves.
(3) powder pre-burning 3 hours at 950 DEG C of will cross sieve, and be incubated 4 hours at this temperature.
(4) the powder 20g after pre-burning is taken, additional 0.6wt.%CaTiO 3and 0.2wt%Bi 2o 3, second batch.
(5) above-mentioned second batch gained powder is put into ball grinder, adds deionized water and zirconia ball, ball milling 12 hours, after oven dry more additional mass percent be the paraffin of 8% as tackiness agent granulation, cross 80 mesh sieves, with powder compressing machine with 6MP apressure depress to the green body cylinders of Φ 10mm × 5mm.
(6) by green body cylinders in 1100 DEG C of sintering, be incubated 4 hours, make low-temperature sintering high q-factor NdNbO 4-CaTiO 3series microwave dielectric ceramic.
(7) by the microwave property of network analyzer test article: specific inductivity is 21.2, quality factor q × f is 38,696GHz, and temperature coefficient of resonance frequency is-28.3ppm/ DEG C.
Embodiment 3
(1) by Nd 2o 3, Nb 2o 5nd in molar ratio 2o 3: Nb 2o 5=1:1 is configured to main powder.
(2) mixed powder of main powder is put into ball grinder, add deionized water and zirconia ball, ball milling 6 hours on planetary ball mill, then the raw material after ball milling is dried in 110 DEG C of loft drier, after oven dry, raw material is crossed 40 mesh sieves.
(3) powder pre-burning 3 hours at 950 DEG C of will cross sieve, and be incubated 4 hours at this temperature.
(4) the powder 20g after pre-burning is taken, additional 0.6wt.%CaTiO 3and 2.0wt%Bi 2o 3, second batch.
(5) above-mentioned second batch gained powder is put into ball grinder, adds deionized water and zirconia ball, ball milling 10 hours, after oven dry more additional mass percent be the paraffin of 8% as tackiness agent granulation, cross 80 mesh sieves, with powder compressing machine with 6MP apressure depress to the green body cylinders of Φ 10mm × 5mm.
(6) by green body cylinders in 1050 DEG C of sintering, be incubated 4 hours, make low-temperature sintering high q-factor NdNbO 4-CaTiO 3series microwave dielectric ceramic.
(7) by the microwave property of network analyzer test article: specific inductivity is 20.6, quality factor q × f is 42,382GHz, and temperature coefficient of resonance frequency is-28.9ppm/ DEG C.
Embodiment 4
(1) by Nd 2o 3, Nb 2o 5nd in molar ratio 2o 3: Nb 2o 5=1:1 is configured to main powder.
(2) mixed powder of main powder is put into ball grinder, add deionized water and zirconia ball, ball milling 6 hours on planetary ball mill, then the raw material after ball milling is dried in 110 DEG C of loft drier, after oven dry, raw material is crossed 40 mesh sieves.
(3) powder pre-burning 3 hours at 950 DEG C of will cross sieve, and be incubated 4 hours at this temperature.
(4) the powder 20g after pre-burning is taken, additional 0.6wt.%CaTiO 3and 8.0wt%Bi 2o 3, second batch.
(5) above-mentioned second batch gained powder is put into ball grinder, add deionized water and zirconia ball, ball milling 6 hours, after oven dry, additional mass percent is that the paraffin of 8% is as tackiness agent granulation again, cross 80 mesh sieves, depress to the green body cylinders of Φ 10mm × 5mm with powder compressing machine with the pressure of 6MPa.
(6) by green body cylinders in 950 DEG C of sintering, be incubated 4 hours, make low-temperature sintering high q-factor NdNbO 4-CaTiO 3series microwave dielectric ceramic.
(7) by the microwave property of network analyzer test article: specific inductivity is 18.2, quality factor q × f is 39,238GHz, and temperature coefficient of resonance frequency is-33.2ppm/ DEG C.

Claims (5)

1. a low-temperature sintering NdNbO 4-CaTiO 3series microwave dielectric ceramic, it consists of NdNbO 4-0.6wt.%CaTiO 3-mwt.%Bi 2o 3, wherein, 0.2≤m≤8;
This low-temperature sintering NdNbO 4-CaTiO 3the preparation method of series microwave dielectric ceramic, has following steps:
(1) by chemical feedstocks Nd 2o 3and Nb 2o 5according to NdNbO 4chemical formula weigh batching;
(2) mixed powder of step (1) is put into ball grinder, add deionized water and zirconia ball, ball milling 6 hours; Again by the raw material after ball milling in 110 DEG C of oven dry, cross 40 mesh sieves, obtain evengranular powder;
(3) by the powder after the sieving of step (2) in 950 DEG C of pre-burnings 3 hours, and be incubated 4 hours at this temperature;
(4) to additional 0.6wt.%CaTiO in the ceramic powder after the pre-burning of step (3) 3, and the low melting point sintering aid Bi of 0.2 ~ 8wt% 2o 3, second batch.
(5) powder of step (4) second batch is put into ball grinder, add deionized water and zirconia ball, ball milling 6 ~ 12 hours, after drying, additional mass percent is that the paraffin of 6 ~ 10% is as tackiness agent granulation, cross 80 mesh sieves, be pressed into base substrate with powder compressing machine;
(6) by the base substrate of step (5) in 950 ~ 1100 DEG C of sintering, be incubated 2 ~ 6 hours, make low-temperature sintering high q-factor NdNbO 4-CaTiO 3series microwave dielectric ceramic;
(7) by the microwave property of network analyzer test article.
2. low-temperature sintering NdNbO according to claim 1 4-CaTiO 3series microwave dielectric ceramic, is characterized in that, the raw material of described step (1) is analytical pure raw material.
3. low-temperature sintering NdNbO according to claim 1 4-CaTiO 3series microwave dielectric ceramic, is characterized in that, the base substrate of described step (5) is the green body cylinders of Φ 10mm × 5mm.
4. low-temperature sintering NdNbO according to claim 1 4-CaTiO 3series microwave dielectric ceramic, is characterized in that, the pressure of the powder compressing machine of described step (5) is 4 ~ 6Mpa.
5. low-temperature sintering NdNbO according to claim 1 4-CaTiO 3series microwave dielectric ceramic, is characterized in that, described step (5) sintering temperature is 1000 DEG C.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105060887A (en) * 2015-07-24 2015-11-18 天津大学 Low-temperature sintering low loss microwave dielectric ceramic material
CN105060888A (en) * 2015-08-31 2015-11-18 天津大学 Low-loss stable niobic acid neodymium ceramic prepared through aluminum oxide doping
CN106986635A (en) * 2017-03-31 2017-07-28 天津大学 A kind of intermediate sintering temperature ceramics as low-loss microwave medium material and preparation method thereof
CN107311646A (en) * 2017-06-19 2017-11-03 天津大学 A kind of preparation method for improving strontium titanate ceramicses dielectric material performance
CN107434411A (en) * 2017-08-29 2017-12-05 电子科技大学 Low Jie's high quality factor LTCC microwave dielectric materials and preparation method thereof
CN107586133A (en) * 2017-09-20 2018-01-16 中国矿业大学 A kind of high performance microwave medium ceramic material, preparation method and application
CN116535212A (en) * 2023-05-15 2023-08-04 中国矿业大学 High-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and preparation method thereof

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CN101913859A (en) * 2010-08-13 2010-12-15 桂林理工大学 Li2Zn3Ti4O12 microwave dielectric ceramic material and low temperature sintering method thereof
CN103073292A (en) * 2013-02-05 2013-05-01 天津大学 High-quality-factor neodymium niobate microwave dielectric ceramic and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101913859A (en) * 2010-08-13 2010-12-15 桂林理工大学 Li2Zn3Ti4O12 microwave dielectric ceramic material and low temperature sintering method thereof
CN103073292A (en) * 2013-02-05 2013-05-01 天津大学 High-quality-factor neodymium niobate microwave dielectric ceramic and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105060887A (en) * 2015-07-24 2015-11-18 天津大学 Low-temperature sintering low loss microwave dielectric ceramic material
CN105060888A (en) * 2015-08-31 2015-11-18 天津大学 Low-loss stable niobic acid neodymium ceramic prepared through aluminum oxide doping
CN106986635A (en) * 2017-03-31 2017-07-28 天津大学 A kind of intermediate sintering temperature ceramics as low-loss microwave medium material and preparation method thereof
CN107311646A (en) * 2017-06-19 2017-11-03 天津大学 A kind of preparation method for improving strontium titanate ceramicses dielectric material performance
CN107434411A (en) * 2017-08-29 2017-12-05 电子科技大学 Low Jie's high quality factor LTCC microwave dielectric materials and preparation method thereof
CN107586133A (en) * 2017-09-20 2018-01-16 中国矿业大学 A kind of high performance microwave medium ceramic material, preparation method and application
CN107586133B (en) * 2017-09-20 2019-06-21 中国矿业大学 A kind of high performance microwave medium ceramic material, preparation method and application
CN116535212A (en) * 2023-05-15 2023-08-04 中国矿业大学 High-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and preparation method thereof
CN116535212B (en) * 2023-05-15 2023-12-26 中国矿业大学 High-performance microwave dielectric ceramic material applied to LTCC (Low temperature Co-fired ceramic) and preparation method thereof

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