CN104692800A - Temperature-stable lead-free giant dielectric constant ceramic material - Google Patents
Temperature-stable lead-free giant dielectric constant ceramic material Download PDFInfo
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- CN104692800A CN104692800A CN201510057763.4A CN201510057763A CN104692800A CN 104692800 A CN104692800 A CN 104692800A CN 201510057763 A CN201510057763 A CN 201510057763A CN 104692800 A CN104692800 A CN 104692800A
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Abstract
The invention discloses a temperature-stable lead-free giant dielectric constant ceramic material. The chemical composition is (1-x)LiCuNb3O9-xBi(Mg0.5Zr0.5)O3, wherein x is molar ratio and is not less than 0.02 and not more than 0.08; Li2CO3, CuO, Nb2O5, Bi2O3, MgO and ZrO2 with the purity of not less than 99% are taken as original powder and are respectively weighed according to the composition of LiCuNb3O9 and Bi(Mg0.5Zr0.5)O3; main powder is synthesized by ball-milling, mixing and then calcining at 900 DEG C and 750 DEG C respectively for 8h; Bi(Mg0.5Zr0.5)O3 powder is added into the LiCuNb3O9 main powder so that the dielectric constant of LiCuNb3O9-based ceramic is higher than 23000, and particularly when x=0.04, the dielectric constant is higher than 48000, and when the test temperature is 100-250 DEG C, the temperature change rate of the dielectric constant (delta epsilon/epsilon 100 DEG C) is small (within plus or minus 15%). The temperature-stable lead-free giant dielectric constant ceramic material disclosed by the invention has the advantages of simple preparation process and low preparation cost, as well as strong practicality.
Description
Technical field
The invention belongs to function ceramics preparing technical field, relate to a kind of dielectric ceramic material, the unleaded giant dielectric stupalith of especially a kind of temperature-stable.
Background technology
High dielectric constant ceramic material has high energy storage density, is widely used in the critical electronic components and parts of numerous high-tech area such as electronics, communication, as resistor, electrical condenser, wave filter, sensor.The develop rapidly of electronic information technology makes electronic industry more and more higher for the requirement of integrated level, impels the microminiaturization of electronic devices and components, miniaturization, high stability and integratedly becomes inexorable trend.Huge dielectric constant material has very high specific inductivity, can store very high electric capacity at very little volume, and thus, have very large volume advantage, greatly reduce material cost, integrated level also improves greatly.Therefore, research and develop efficient, repeated huge dielectric constant material preferably miniaturize electronic circuitry and microminiaturization are had very important significance.
The huge dielectric constant pottery studied the earliest is BaTiO
3base and Pb based perovskite is ferroelectric or relaxation ferroelectric, as Pb (Zr, Ti) O
3, Pb (Mg
1/3nb
2/3) O
3-PbTiO
3deng.The specific inductivity of above-mentioned materials near ferroelectric-paraelectric phase temperature is often higher than more than one, the non-phase change zone order of magnitude, and specific inductivity along with the change of temperature, acute variation can occur, and is unfavorable for the thermostability keeping microelectronic device and semiconducter device.In addition, Pb base ferroelectric material is in preparation and use procedure, and Pb not only can to environment, and also can bring very large harm to human body, is unfavorable for the enforcement of the strategy of sustainable development.Therefore increasing research has been placed on and has explored in the high dielectric constant material system not leaded, specific inductivity is stable.
Based on above analysis, the present invention devises (1-
x) LiCuNb
3o
9-
xbi (Mg
0.5zr
0.5) O
3pottery, wherein,
xfor mol ratio, 0.02≤
x≤ 0.08.Result shows this pottery and has higher specific inductivity (>=23000), particularly exists
xwhen=0.04, specific inductivity up to 48000, in 100-250 DEG C of Range of measuring temp, specific inductivity rate of temperature change (Δ ε/ε
100 o c) within ± 15%, be a kind of unleaded huge dielectric constant pottery of excellent property.
Summary of the invention
The present invention has the Bi (Mg of same calcium perovskite like structure by introducing
0.5zr
0.5) O
3with LiCuNb
3o
9form sosoloid to improve specific inductivity and the temperature stability thereof of stupalith, thus obtain the unleaded huge dielectric constant stupalith of a kind of low cost, excellent performance.
The present invention relates to the unleaded huge dielectric constant stupalith of a kind of temperature-stable, its chemical constitution formula is: (1-
x) LiCuNb
3o
9-
xbi (Mg
0.5zr
0.5) O
3, wherein
xfor mol ratio, 0.02≤
x≤ 0.08.
A preparation method for the unleaded huge dielectric constant stupalith of temperature-stable, comprises the following steps:
(1) with the Li of purity>=99%
2cO
3, CuO, Nb
2o
5, Bi
2o
3, MgO, ZrO
2for starting powder, press LiCuNb respectively
3o
9with Bi (Mg
0.5zr
0.5) O
3composition weigh batching; Take ethanol as ball-milling medium, adopt wet milling process to mix 4 hours, after drying, be pressed into bulk, then by the pre-burning 8 hours under 900 DEG C and 750 DEG C of air atmospheres respectively of two kinds of briquettings;
(2) briquetting step (1) made is pulverized, by (1-
x) LiCuNb
3o
9-
xbi (Mg
0.5zr
0.5) O
3stoichiometric ratio weigh, wherein,
xfor mol ratio, 0.02≤
x≤ 0.08; Take ethanol as ball-milling medium, put into nylon tank ball milling to take out after 4 hours, put into baker to dry at 120 ~ 140 DEG C, add binding agent after granulation, being pressed into diameter is 12mm, thickness is the disk of 1mm, disk is placed in 500 ~ 600 DEG C of binder removals and sinters at 975 ~ 1110 DEG C after 4 hours, be incubated 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and dosage accounts for 5% ~ 7% of powder total mass.
Phase structure after said temperature stable form unleaded huge dielectric constant stupalith burns till is single Emission in Cubic.
Unleaded huge dielectric constant pottery prepared by the present invention, its dielectric properties are excellent: specific inductivity>=23000, particularly exist
xwhen=0.04, specific inductivity up to 48000, in the Range of measuring temp of 100-250 DEG C, specific inductivity rate of temperature change (Δ ε/ε
100 o c) within ± 15%; Can be used for the manufacture of the dielectric devices such as electrical condenser, wave filter, dynamic RAM (DRAM).
Embodiment
embodiment:
Table 1 shows and forms different B i (Mg of the present invention
0.5zr
0.5) O
34 specific embodiments of addition and dielectric properties thereof.Its preparation method is described above, is carried out the test of dielectric properties by precise impedance analyser Agilent (4294A) type precise impedance analyser.
This pottery can be widely used in the manufacture of the dielectric device such as dynamic RAM (DRAM) and laminated ceramic capacitor (MLCC).
Table 1:
Claims (1)
1. the unleaded huge dielectric constant stupalith of temperature-stable, is characterized in that described huge dielectric constant stupalith chemical formula is (1-
x) LiCuNb
3o
9-
xbi (Mg
0.5zr
0.5) O
3, wherein,
xfor mol ratio, 0.02≤
x≤ 0.08;
The synthesis step of described huge dielectric constant stupalith is:
(1) with the Li of purity>=99%
2cO
3, CuO, Nb
2o
5, Bi
2o
3, MgO, ZrO
2for starting powder, press LiCuNb respectively
3o
9with Bi (Mg
0.5zr
0.5) O
3composition weigh batching; Take ethanol as ball-milling medium, adopt wet milling process to mix 4 hours, after drying, be pressed into bulk, then by the pre-burning 8 hours under 900 DEG C and 750 DEG C of air atmospheres respectively of two kinds of briquettings;
(2) burning block step (1) made is pulverized, by (1-
x) LiCuNb
3o
9-
xbi (Mg
0.5zr
0.5) O
3batching, wherein,
xfor mol ratio, 0.02≤
x≤ 0.08; Take ethanol as ball-milling medium, put into nylon tank ball milling to take out after 4 hours, put into baking oven to dry at 120 ~ 140 DEG C, after adding binding agent granulation, being pressed into diameter is 12mm, thickness is the disk of 1mm, disk is placed in 500 ~ 600 DEG C of binder removals and at 975 ~ 1110 DEG C, sinters 4 hours after 4 hours, namely obtain material requested; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and dosage accounts for 5% ~ 7% of powder total mass.
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|---|---|---|---|
| CN201510057763.4A CN104692800B (en) | 2015-02-04 | 2015-02-04 | A kind of temperature-stable unleaded huge dielectric constant ceramic material |
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|---|---|---|---|
| CN201510057763.4A CN104692800B (en) | 2015-02-04 | 2015-02-04 | A kind of temperature-stable unleaded huge dielectric constant ceramic material |
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|---|---|
| CN104692800A true CN104692800A (en) | 2015-06-10 |
| CN104692800B CN104692800B (en) | 2016-08-24 |
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ID=53340402
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926303A (en) * | 2015-06-15 | 2015-09-23 | 桂林理工大学 | Bismuth-based perovskite mine dielectric ceramic material with temperature stability and preparation method thereof |
| CN108689703A (en) * | 2018-06-26 | 2018-10-23 | 桂林电子科技大学 | A kind of Lead-free ferroelectric ceramics material and preparation method thereof for adjusting characteristic with huge dielectric constant and electricity |
| CN112080732A (en) * | 2020-07-29 | 2020-12-15 | 西安交通大学 | Silicon integrated BT-BMZ film, capacitor and manufacturing method thereof |
| CN116813335A (en) * | 2023-07-20 | 2023-09-29 | 广东工业大学 | Bismuth sodium titanate based relaxation ferroelectric ceramic material with wide temperature range and high electric clamping effect, and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102568821A (en) * | 2012-02-16 | 2012-07-11 | 江苏大学 | High-voltage ceramic capacitor dielectric with high dielectric constant |
| CN102584234A (en) * | 2012-03-13 | 2012-07-18 | 嘉兴佳利电子股份有限公司 | Environment-friendly low-temperature sintered high-epsilon microwave dielectric ceramic and preparation method thereof |
| CN103232239A (en) * | 2013-04-22 | 2013-08-07 | 江苏大学 | Microwave dielectric ceramic material and preparation method thereof |
-
2015
- 2015-02-04 CN CN201510057763.4A patent/CN104692800B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102568821A (en) * | 2012-02-16 | 2012-07-11 | 江苏大学 | High-voltage ceramic capacitor dielectric with high dielectric constant |
| CN102584234A (en) * | 2012-03-13 | 2012-07-18 | 嘉兴佳利电子股份有限公司 | Environment-friendly low-temperature sintered high-epsilon microwave dielectric ceramic and preparation method thereof |
| CN103232239A (en) * | 2013-04-22 | 2013-08-07 | 江苏大学 | Microwave dielectric ceramic material and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926303A (en) * | 2015-06-15 | 2015-09-23 | 桂林理工大学 | Bismuth-based perovskite mine dielectric ceramic material with temperature stability and preparation method thereof |
| CN108689703A (en) * | 2018-06-26 | 2018-10-23 | 桂林电子科技大学 | A kind of Lead-free ferroelectric ceramics material and preparation method thereof for adjusting characteristic with huge dielectric constant and electricity |
| CN108689703B (en) * | 2018-06-26 | 2021-01-05 | 桂林电子科技大学 | Lead-free ferroelectric ceramic material with giant dielectric constant and electric tuning characteristics and preparation method thereof |
| CN112080732A (en) * | 2020-07-29 | 2020-12-15 | 西安交通大学 | Silicon integrated BT-BMZ film, capacitor and manufacturing method thereof |
| CN116813335A (en) * | 2023-07-20 | 2023-09-29 | 广东工业大学 | Bismuth sodium titanate based relaxation ferroelectric ceramic material with wide temperature range and high electric clamping effect, and preparation method and application thereof |
| CN116813335B (en) * | 2023-07-20 | 2024-03-29 | 广东工业大学 | Bismuth sodium titanate based relaxation ferroelectric ceramic material with wide temperature range and high electric clamping effect, and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN104692800B (en) | 2016-08-24 |
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