CN102249675A - Novel microwave dielectric ceramic material for multilayer ceramic capacitor - Google Patents
Novel microwave dielectric ceramic material for multilayer ceramic capacitor Download PDFInfo
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- CN102249675A CN102249675A CN2011101058858A CN201110105885A CN102249675A CN 102249675 A CN102249675 A CN 102249675A CN 2011101058858 A CN2011101058858 A CN 2011101058858A CN 201110105885 A CN201110105885 A CN 201110105885A CN 102249675 A CN102249675 A CN 102249675A
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Abstract
The invention discloses a novel microwave dielectric ceramic material for a multilayer ceramic capacitor, and the raw material components and the molar percentage contents are: ZnTi(Ta1-xNbx)2O8 (x=0.30, 0.50); the preparation method comprises the following steps: (1) preparing materials; (2) performing ball milling, drying, and sieving; (3) calcining at 750 DEG C to synthesize a frit; (4) adding the frit into 0.35-0.75% polyvinyl alcohol, performing ball milling, drying, sieving, and compression moulding; (5) sintering at 1040-1140 DEG C; (6) testing the electric performance. The invention provides a microwave dielectric ceramic material for a multilayer ceramic capacitor, which has a sintering temperature of 1040-1140 DEG C, a dielectric constant of 34-40, a high quality factor, and good temperature stability. The invention is applicable to the fields of wireless local area network, satellite broadcast equipment, medical electron, missile system, airplane radar, navigation, etc.
Description
Technical field
The invention belongs to electronic information material and components and parts field, relate in particular to a kind of with ZnTi (Ta
1-xNb
x)
2O
8(x=0.30,0.50) is the novel intermediate sintering temperature microwave dielectric ceramic materials of chemical formula.
Technical background
Chip multilayer ceramic capacitor (MLCC) is one of three big passive electronic components and parts, it and chip resistor, chip inductor constitute the indispensable basic passive device of electronics and information industry, extensively apply to modern mobile communication and automobile electronic information machine product, play effects such as bypass, coupling, filtering, vibration.Along with the electronics and information industry continuous advancement in technology, electronic product is to aspect such as light, thin, short, little development, and MLCC also develops to directions such as miniaturization, large vol, high specific volume, high frequencyization, multifunction, reduce power consumption.Its medium-high frequencyization is one of emphasis of its development.For example: use in the mobile phone radio frequency signal transmitting and receiving module have high current carrying capacity, the high-Q microwave ceramic condenser, in the RF circuit of WLAN (wireless local area network), satellite broadcasting equipment, medical electronics, missile system, rebecca and navigationsystem etc., the frequency of using is more and more higher, so require supportingly have high quality factor (Qf value) with electronic component.
During MLCC in early days produces, have only precious metals pt, Au, Pd or their alloy could satisfy the requirement of making interior electrode, along with rapid increase of MLCC demand and Pd price skyrocket, for reducing cost, MLCC manufacturing enterprise uses the Ag/Pd metal system to make interior electrode mostly, and this has just proposed requirement to the sintering temperature of stupalith.Usually use the Ag/Pd metal system do in the MLCC of electrode require its sintering temperature Ts≤1150 ℃ with microwave ceramic material.
ZnTiTa
2O
8Microwave-medium ceramics have high quality factor (65,000GHz), good temperature stability (7.59 * 10
-6/ ℃), but its sintering temperature higher (1160 ℃).And ZnTi (Ta of the present invention
1-xNb
x)
2O
8(x=0.30,0.50) microwave-medium ceramics replaces Ta by Nb, has not only improved quality factor, also effectively reduces sintering temperature (＜1150 ℃) simultaneously, has prepared the microwave dielectric ceramic materials that can be used for MLCC.
Summary of the invention
The objective of the invention is to adapt to electronic information technology constantly to high frequencyization and digitizing direction development need, overcome the higher shortcoming of sintering temperature, the novel MLCC ZnTi (Ta of a kind of temperature stability height, medium dielectric constant microwave medium, high Qf value is provided
1-xNb
x)
2O
8(x=0.30,0.50) microwave dielectric ceramic materials.
The present invention is achieved by following technical solution.
The novel MLCC microwave dielectric ceramic materials of the present invention, feed composition and mole percent level thereof are ZnTi (Ta
1-xNb
x)
2O
8(x=0.30,0.50);
Its preparation process is as follows:
(1) with chemical feedstocks ZnO, Ta
2O
5, Nb
2O
5, TiO
2Press ZnTi (Ta respectively
1-xNb
x)
2O
8(x=0.30,0.50) chemical formula weigh batching;
(2) chemical feedstocks that step (1) is configured mixes, and puts into ball grinder, adds zirconia ball and deionized water, raw material: deionized water: the mass ratio of zirconium ball is 1: 1: 1.5, ball milling 1～12 hour is dried the raw material behind the ball milling in infrared drying oven, sieve;
(3) powder that step (2) is mixed is at 3 hours synthetic frits of 750 ℃ of calcinings;
(4) put into ball grinder with adding 0.35～0.75% polyvinyl alcohol in step (3) frit, add zirconia ball and deionized water, ball milling 4～12 hours sieves after the oven dry, is pressed into the cylinder shape base substrate of Ф 10mm * 5mm again with powder compressing machine;
(5) with the cylinder shape base substrate of step (4) compression moulding in 1040～1140 ℃ of sintering 2～6 hours, make ZnTi (Ta
1-xNb
x)
2O
8(x=0.30,0.50) microwave-medium ceramics;
(6) with the microwave dielectric property of network analyzer test microwave-medium ceramics.
The raw material of described step (1) is a purity greater than 99.9% analytical pure raw material.
The ball-grinding machine of described step (2) is a planetary ball mill, and rotating speed is 400r/min.
Raw material behind the ball milling of described step (2) is 100～120 ℃ of oven dry in infrared drying oven.
The base substrate of described step (4) is the cylinder shape base substrate of Ф 10mm * 5mm, and the gauge pressure of tabletting machine is 6～10MPa.
The invention has the beneficial effects as follows, a kind of MLCC is provided ZnTi (Ta
1-xNb
x)
2O
8(x=0.30,0.50) microwave-medium ceramics, its sintering temperature is 1040～1140 ℃, and specific inductivity is 34～40, and the quality factor height is 65,000～70,000GHz, temperature stability is good, and temperature coefficient of resonance frequency is-2.3～-28.3 * 10
-6/ ℃.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.
The present invention adopts purity greater than 99.9% analytical pure raw material, according to ZnTi (Ta
1-xNb
x)
2O
8(x=0.30,0.50) stoichiometric ratio prepare burden, mix, in mixing raw material: deionized water: the mass ratio of zirconium ball is that 1: 1: 1.5 ratio adds in the nylon ball grinder, at rotating speed is ball milling 1～12 hour on the 400r/min planetary ball mill, in the 1500W infrared drying oven in 100～120 ℃ of oven dry; In 750 ℃ of pre-burning 3h, make frit; Adding mass percent in this frit is that 0.35～0.75% polyvinyl alcohol is put into ball grinder, add zirconia ball and deionized water, ball milling 4～12 hours sieves after the oven dry, is pressed into the cylinder shape base substrate of Ф 10mm * 5mm again with the pressure of 6～10MPa with powder compressing machine; The cylinder shape base substrate in 1040～1140 ℃ of sintering 2～6 hours, is made microwave-medium ceramics.
The proportioning raw materials of the specific embodiment of the invention is: x=0.30:4.4361 gram ZnO, 16.8616 gram Ta
2O
5, 4.3554 the gram TiO
2, 4.3469 the gram Nb
2O
5X=0.50:4.7394 gram ZnO, 12.8674 gram Ta
2O
5, 4.6532 the gram TiO
2, 7.7401 the gram Nb
2O
5
The related process parameter of specific embodiment and the test result of microwave dielectric property see table 1 for details.
Table 1
The detection method of the embodiment of the invention is as follows:
1. the diameter of sample and thickness use milscale to measure.
2. by Agilent 8720ES network analyzer, adopt open type chamber parallel plate method to measure the specific inductivity of prepared cylindrical ceramic material, test fixture is put into the high cold cycle incubator of ESPEC MC-710F type carry out the measurement of temperature coefficient of resonance frequency, temperature range is that 25-85 ℃ of test frequency is in the 7-8.5GHz scope.
3. adopt enclosed chamber method to measure the quality factor of prepared cylindrical ceramic sample, test frequency is in the 5-6.5GHz scope.
The present invention is not limited to the foregoing description, 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 (5)
1. novel multi-layer ceramic condenser microwave dielectric ceramic materials, feed composition and mole percent level thereof are ZnTi (Ta
1-xNb
x)
2O
8(x=0.30,0.50);
Its preparation process is as follows:
(1) with chemical feedstocks ZnO, Ta
2O
5, Nb
2O
5, TiO
2Press ZnTi (Ta respectively
1-xNb
x)
2O
8(x=0.30,0.50) chemical formula weigh batching;
(2) chemical feedstocks that step (1) is configured mixes, and puts into ball grinder, adds zirconia ball and deionized water, raw material: deionized water: the mass ratio of zirconium ball is 1: 1: 1.5, ball milling 1～12 hour is dried the raw material behind the ball milling in infrared drying oven, sieve;
(3) powder that step (2) is mixed is at 3 hours synthetic frits of 750 ℃ of calcinings;
(4) put into ball grinder with adding 0.35～0.75% polyvinyl alcohol in step (3) frit, add zirconia ball and deionized water, ball milling 4～12 hours sieves after the oven dry, is pressed into the cylinder shape base substrate of Ф 10mm * 5mm again with powder compressing machine;
(5) with step (4) cylinder shape base substrate in 1040～1140 ℃ of sintering 2～6 hours, make ZnTi (Ta
1-xNb
x)
2O
8(x=0.30,0.50) microwave-medium ceramics;
(6) with the microwave dielectric property of network analyzer test microwave-medium ceramics.
2. according to the novel multi-layer ceramic condenser microwave dielectric ceramic materials of claim 1, it is characterized in that the chemical feedstocks of described step (1) is a purity greater than 99.9% analytical pure raw material.
3. according to the novel multi-layer ceramic condenser microwave dielectric ceramic materials of claim 1, it is characterized in that the ball-grinding machine of described step (2) is a planetary ball mill, rotating speed is 400r/min.
4. according to the novel multi-layer ceramic condenser microwave dielectric ceramic materials of claim 1, it is characterized in that the raw material behind the ball milling of described step (2) is 100～120 ℃ of oven dry in infrared drying oven.
5. according to the novel multi-layer ceramic condenser microwave dielectric ceramic materials of claim 1, it is characterized in that the base substrate of described step (4) is the cylinder shape base substrate of Ф 10mm * 5mm, the gauge pressure of tabletting machine is 6～10MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110105885 CN102249675B (en) | 2011-04-26 | 2011-04-26 | Novel microwave dielectric ceramic material for multilayer ceramic capacitor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110105885 CN102249675B (en) | 2011-04-26 | 2011-04-26 | Novel microwave dielectric ceramic material for multilayer ceramic capacitor |
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| Publication Number | Publication Date |
|---|---|
| CN102249675A true CN102249675A (en) | 2011-11-23 |
| CN102249675B CN102249675B (en) | 2013-07-10 |
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ID=44977297
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110105885 Expired - Fee Related CN102249675B (en) | 2011-04-26 | 2011-04-26 | Novel microwave dielectric ceramic material for multilayer ceramic capacitor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573056A (en) * | 2017-09-24 | 2018-01-12 | 天津大学 | Microwave dielectric material of temperature coefficient of resonance frequency nearly zero and preparation method thereof |
| CN107721421A (en) * | 2017-10-30 | 2018-02-23 | 电子科技大学 | A kind of Zn Nb Ti systems LTCC materials and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462874A (en) * | 2008-11-28 | 2009-06-24 | 西安交通大学 | Low temperature sintering middle-dielectric constant microwave-medium ceramic material and preparation method thereof |
| CN101857435A (en) * | 2010-06-11 | 2010-10-13 | 天津大学 | Medium-temperature sintered composite niobate high-frequency medium ceramic and preparation method thereof |
-
2011
- 2011-04-26 CN CN 201110105885 patent/CN102249675B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462874A (en) * | 2008-11-28 | 2009-06-24 | 西安交通大学 | Low temperature sintering middle-dielectric constant microwave-medium ceramic material and preparation method thereof |
| CN101857435A (en) * | 2010-06-11 | 2010-10-13 | 天津大学 | Medium-temperature sintered composite niobate high-frequency medium ceramic and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| DONG-WAN KIM ET AL.: "Origin of microwave dielectric loss in ZnNb2O6-TiO2", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
| MEI GUO ET AL.: "A new temperature stable microwave dielectric ceramics: ZnTiNb2O8 sintered at low temperatures", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| YINGCHUN ZHANG ET AL.: "Microwave dielectric properties of Zn(Nb1-xTax)2O6 ceramics", 《MATERIALS LETTERS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573056A (en) * | 2017-09-24 | 2018-01-12 | 天津大学 | Microwave dielectric material of temperature coefficient of resonance frequency nearly zero and preparation method thereof |
| CN107721421A (en) * | 2017-10-30 | 2018-02-23 | 电子科技大学 | A kind of Zn Nb Ti systems LTCC materials and preparation method thereof |
| CN107721421B (en) * | 2017-10-30 | 2020-09-25 | 电子科技大学 | Zn-Nb-Ti LTCC material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102249675B (en) | 2013-07-10 |
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