CN102603296B - Neodymium niobic acid microwave dielectric ceramic with high quality factor and method for preparing neodymium niobic acid microwave dielectric ceramic - Google Patents

Neodymium niobic acid microwave dielectric ceramic with high quality factor and method for preparing neodymium niobic acid microwave dielectric ceramic Download PDF

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CN102603296B
CN102603296B CN 201210076189 CN201210076189A CN102603296B CN 102603296 B CN102603296 B CN 102603296B CN 201210076189 CN201210076189 CN 201210076189 CN 201210076189 A CN201210076189 A CN 201210076189A CN 102603296 B CN102603296 B CN 102603296B
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microwave dielectric
niobic acid
dielectric ceramic
quality factor
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张平
王涛
李玲霞
夏往所
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Tianjin University
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Abstract

The invention discloses a neodymium niobic acid microwave dielectric ceramic with a high quality factor. The neodymium niobic acid microwave dielectric ceramic comprises raw material components including, by molar, 50% of Nd2O3, 50% of Nb2O5 and from 1 to 7% of CaF2. The Nd2O3 raw material and the Nb2O5 raw material are prepared according to a molar ratio of 1:1 and then are ball-milled, dried and calcined, then the CaF2 is added into the Nd2O3 and the Nd2O5 to realize granulation, and sintering is carried out at the temperature ranging from 1200 DEG C to 1325 DEG C. When the sintering temperature is 1225 DEG C, heat is retained for 4 hours, the dielectric constant of ceramic is 20.1 when the doping quantity of the CaF2 is 2wt.%, the resonance frequency temperature coefficient is -19.6ppm/DEG C, and the quality factor reaches 75000 GHz. The neodymium niobic acid microwave dielectric ceramic is widely used for manufacturing electric containers and photoelectronic devices.

Description

High quality factor niobic acid neodymium series microwave dielectric ceramic and preparation method thereof
Technical field
The invention belongs to a kind of the take ceramic composition that composition is feature, particularly a kind of high quality factor (Q value) niobic acid neodymium series microwave dielectric ceramic and preparation method thereof.
Background technology
The critical material that microwave-medium ceramics is the microwave devices such as modern mobile communication, satellite communication and military radar resonator used, filter, medium substrate.Constantly to high frequency and digitlization future development, to the miniaturization of components and parts, integrated so that modular requirement is also more and more urgent along with electronic information technology.Therefore pursue high quality factor, high-k, nearly zero or adjustable temperature coefficient and the low sintering temperature study hotspot that is current microwave dielectric ceramic materials.
The niobates material is important electronic material, has good photoelectric properties and non-linear optical property, good optical effect and peculiar properties such as electric property and metacrystal phase boundary, has been widely used in and has manufactured capacitor and opto-electronic device.This system material is originally for making multilayer ceramic capacitor, the people such as J.Cato studied their dielectric properties under microwave frequency afterwards, found that this class material has higher dielectric constant and Q value under microwave frequency, and temperature coefficient of resonance frequency is close to zero.One of unleaded focus that becomes ceramic material research in recent years, and niobate ceramics become one of emphasis of unleaded ceramic research.Rare earth niobium hydrochlorate (LnNbO 4) be the similar microwave dielectric material of a series of structures, phase-change characteristic and physical property, Ln wherein comprises whole rare earth elements of La to Lu.When being substituted by Nd, Ln is niobic acid neodymium (NdNbO 4) pottery.Research shows, niobic acid neodymium pottery belongs to the perovskite-like scheelite-type structure, has suitable DIELECTRIC CONSTANT ε r(19.6), nearly zero temperature coefficient of resonance frequency τ f(24ppm/ ℃), but quality factor q * f lower (33 000GHz), and sintering temperature is 1250 ℃.Therefore, lower quality factor are restriction niobic acid neodymium ceramic applications key points.But at present the research of its preparation method and modification be yet there are no to special report.The present invention adopts conventional solid-state method, with CaF 2for flux, under lower sintering temperature, prepared niobic acid neodymium microwave-medium ceramics, when dielectric constant and temperature coefficient of resonance frequency remain unchanged substantially, significantly having improved the niobic acid neodymium is ceramic quality factor.
Summary of the invention
The objective of the invention is with Nd 2o 3, Nb 2o 5for primary raw material, and add appropriate CaF 2as flux, overcome the defect that current quality factor q * f is lower, prepare the niobic acid neodymium series microwave dielectric ceramic with high quality factor by solid phase method.
The present invention is achieved by following technical solution.
A kind of high quality factor niobic acid of the present invention neodymium series microwave dielectric ceramic, its raw material components and mole percent level be, Nd 2o 350%, Nb 2o 550%, the CaF of added weight degree 1-7% 2.
The preparation method of high quality factor niobic acid neodymium series microwave dielectric ceramic of the present invention has following steps:
(1) by Nd 2o 3, Nb 2o 5raw material is prepared burden according to the mol ratio ratio of 1: 1, and according to percentage by weight, materials: deionized water: the ratio of abrading-ball=1: 7: 7 adds in the polyester tank, and on ball mill, ball milling is 4～6 hours;
(2) raw material after step (1) ball milling is placed in to drying box in 80～130 ℃ of oven dry, after drying, crosses 40 mesh sieves, obtain evengranular powder;
(3) powder step (2) mixed was 900～1100 ℃ of calcinings 4 hours;
(4) add the CaF that percentage by weight is 1-7% in the ceramic powder after step (3) calcining 2, then put into the polyester tank, after adding deionized water and zirconium ball, on ball mill, ball milling is 12～24 hours; The paraffin that added weight percentage is 6～10% in ceramic powder after oven dry carries out granulation as adhesive, cross 80 mesh sieves, then use the powder compressing machine pressure forming, then by green compact in 1200～1325 ℃ of sintering 2～6 hours, make microwave-medium ceramics;
(5) microwave dielectric property of the microwave-medium ceramics that test makes.
The Nd of described step (1) 2o 3, Nb 2o 5the purity of raw material is greater than 99.9%.
The ball mill of described step (1) and step (4) is planetary ball mill.
The operating pressure of the tablet press machine of described step (4) is 4MPa, the cylinder that the green compact specification is Φ 10mm * 5mm.
Described step (5) is to test the microwave dielectric property of microwave-medium ceramics by network analyzer.
The preferred calcined temperature of described step (3) is 900 ℃.
The preferred CaF of described step (4) 2addition is 2%.
The preferred sintering temperature of described step (4) is 1225 ℃, is incubated 4 hours.
The present invention is owing to having adopted CaF 2as flux, the NdNbO of preparation 4pottery, wherein generated useful second-phase CaNb 2o 6, with the existing CaF that do not add 2the preparation method of flux compares, and under lower sintering temperature, the bulk density of pottery obviously increases.When sintering temperature is 1225 ℃, temperature retention time 4h, CaF 2doping while being 2wt.%, dielectric constant is 20.1, temperature coefficient of resonance frequency is-19.6ppm/ ℃ that quality factor reach and are 75 000GHz to the maximum.
Embodiment
The chemical raw material Nd that the present invention adopts purity to be greater than 99.9% 2o 3, Nb 2o 5, CaF 2preparation NdNbO 4microwave-medium ceramics.
The present invention is first by Nd 2o 3, Nb 2o 5according to 1: 1 weigh batching of mol ratio, after mixing, raw material is added in the nylon tank to ball milling 4～6 hours; Raw material after ball milling is placed in to infrared drying oven in 80～130 ℃ of oven dry, crosses 40 mesh sieves, then in 900～1100 ℃ of calcinings 4 hours; To in the ceramic powder after calcining, add the CaF that percentage by weight is 1-7% again 2, put into ball grinder, add 12～24 hours post-dryings of zirconia ball and deionized water ball milling; The paraffin wax binder that in ceramic powder after oven dry, the added weight percentage composition is 6～10 is again carried out granulation, and after crossing 80 mesh sieves, powder being pressed into to diameter under the pressure of 4MPa with powder compressing machine is 10mm, the green compact that thickness is 5mm; Green compact, at 1200～1325 ℃ of sintering, are incubated to 2～6 hours, make microwave-medium ceramics; Finally by the microwave dielectric property of network analyzer and dependence test fixture test article.
The specific embodiment of the invention is as follows.
Embodiment 1:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, powder is calcined 4 hours in 1100 ℃, after the CaF2 0.4g that to take percentage by weight be 2% again mixes with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, by green compact at 1200 ℃ of sintering, be incubated 4 hours, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 2:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, powder is calcined 4 hours in 1000 ℃, after the CaF2 0.5g that to take percentage by weight be 2.5% again mixes with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, by green compact at 1300 ℃ of sintering, be incubated 4 hours, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 3:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, and powder, in 900 ℃ of calcinings 4 hours, then is taken to the CaF that percentage by weight is 2% 20.4g after mixing with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, at 1200 ℃ of sintering, be incubated 4 hours by green compact, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 4:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, and powder, in 900 ℃ of calcinings 4 hours, then is taken to the CaF that percentage by weight is 2% 20.4g after mixing with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, at 1225 ℃ of sintering, be incubated 4 hours by green compact, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 5:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, and powder, in 900 ℃ of calcinings 4 hours, then is taken to the CaF that percentage by weight is 2% 20.4g after mixing with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, at 1250 ℃ of sintering, be incubated 4 hours by green compact, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 6:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, and powder, in 900 ℃ of calcinings 4 hours, then is taken to the CaF that percentage by weight is 2% 20.4g after mixing with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, at 1300 ℃ of sintering, be incubated 4 hours by green compact, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 7:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, and powder, in 900 ℃ of calcinings 4 hours, then is taken to the CaF that percentage by weight is 2% 20.4g after mixing with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, at 1325 ℃ of sintering, be incubated 4 hours by green compact, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 8:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, and powder, in 900 ℃ of calcinings 4 hours, then is taken to the CaF that percentage by weight is 1% 20.2g after mixing with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, at 1225 ℃ of sintering, be incubated 4 hours by green compact, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 9:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, and powder, in 900 ℃ of calcinings 4 hours, then is taken to the CaF that percentage by weight is 3% 20.6g after mixing with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, at 1225 ℃ of sintering, be incubated 4 hours by green compact, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Embodiment 10:
According to microwave-medium ceramics component NdNbO 4, take Nd 2o 311.17g, Nb 2o 58.83g batching, mixed powder adds in the polyester tank, after adding 150ml deionized water and 150g zirconium ball, on planetary ball mill, ball milling is 6 hours, rotating speed is 1000 rev/mins, discharging is placed in drying box 120 ℃ and dries and cross 40 mesh sieves, and powder, in 900 ℃ of calcinings 4 hours, then is taken to the CaF that percentage by weight is 7% 21.4g after mixing with powder, secondary ball milling is 24 hours, the discharging post-drying also adds the paraffin that percentage by weight is 8% to carry out granulation as adhesive in powder, and mistake 80 mesh sieves, take the pressure of 4MPa with powder compressing machine again and be pressed into diameter as 10mm, the green compact that thickness is 5mm, at 1225 ℃ of sintering, be incubated 4 hours by green compact, make microwave-medium ceramics, measure the microwave dielectric property of sample.
Every key parameter and the dielectric property testing result of the embodiment of the present invention refer to table 1.
Table 1
Figure BDA0000145693120000051
The detection method of the embodiment of the present invention is as follows:
1. the diameter of sample and thickness are used micrometer to be measured.
2. by Agilent 8720ES network analyzer, employing starts to rob the economize on electricity constant that parallel plate method is measured prepared cylindrical ceramic material, test fixture is put into to the high low temperature circulation warm of ESPEC MC-710F type case and carry out the measurement of temperature coefficient of resonance frequency, temperature range is that 25-85 ℃ of test frequency is in the 9-12GHz scope.
3. adopt enclosed chamber method to measure the quality factor of prepared cylindrical ceramic sample, test frequency is in the 6-10GHz scope.
The present invention is not limited to above-described embodiment, and the variation of a lot of details is possible, but therefore this do not run counter to scope and spirit of the present invention.

Claims (8)

1. a high quality factor niobic acid neodymium series microwave dielectric ceramic, its raw material components and mole percent level be, Nd 2o 350%, Nb 2o 550%, the CaF of added weight degree 1-7% 2;
The preparation method of this high quality factor niobic acid neodymium series microwave dielectric ceramic has following steps:
(1) by Nd 2o 3, Nb 2o 5raw material is prepared burden according to the ratio of mol ratio 1:1, and according to percentage by weight, the ratio of materials: deionized water: abrading-ball=1:7:7 adds in the polyester tank, and on ball mill, ball milling is 4～6 hours;
By step (1) the raw material after ball milling be placed in drying box in 80～130 ℃ of oven dry, cross 40 mesh sieves after drying, obtain evengranular powder;
(3) the powder (2) step mixed was 900～1100 ℃ of calcinings 4 hours;
(4) add the CaF that percentage by weight is 1-7% in the ceramic powder after (3) step calcines 2, then put into the polyester tank, after adding deionized water and zirconium ball, on ball mill, ball milling is 12～24 hours; The paraffin that added weight percentage is 6～10% in ceramic powder after oven dry carries out granulation as adhesive, cross 80 mesh sieves, then use the powder compressing machine pressure forming, then by green compact in 1200～1325 ℃ of sintering, be incubated 2～6 hours, make microwave-medium ceramics;
(5) test the microwave dielectric property of microwave-medium ceramics.
2. according to the high quality factor niobic acid neodymium series microwave dielectric ceramic of claim 1, it is characterized in that described step Nd (1) 2o 3, Nb 2o 5the purity of raw material is greater than 99.9%.
3. according to the high quality factor niobic acid neodymium series microwave dielectric ceramic of claim 1, it is characterized in that, (1) described step is planetary ball mill with step ball mill (4).
4. according to the high quality factor niobic acid neodymium series microwave dielectric ceramic of claim 1, it is characterized in that, the operating pressure of described step tablet press machine (4) is 4MPa, the cylinder that the green compact specification is Φ 10mm * 5mm.
5. according to the high quality factor niobic acid neodymium series microwave dielectric ceramic of claim 1, it is characterized in that, (5) described step is to test the microwave dielectric property of microwave-medium ceramics by network analyzer.
6. according to the high quality factor niobic acid neodymium series microwave dielectric ceramic of claim 1, it is characterized in that, described step (3) preferred calcined temperature is 900 ℃.
7. according to the high quality factor niobic acid neodymium series microwave dielectric ceramic of claim 1, it is characterized in that, described step is preferred CaF (4) 2addition is 2%.
8. according to the high quality factor niobic acid neodymium series microwave dielectric ceramic of claim 1, it is characterized in that, described step (4) preferred sintering temperature is 1225 ℃, is incubated 4 hours.
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