CN103979953A - Novel rare earth modified microwave dielectric ceramic and preparation method thereof - Google Patents
Novel rare earth modified microwave dielectric ceramic and preparation method thereof Download PDFInfo
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- CN103979953A CN103979953A CN201410141803.9A CN201410141803A CN103979953A CN 103979953 A CN103979953 A CN 103979953A CN 201410141803 A CN201410141803 A CN 201410141803A CN 103979953 A CN103979953 A CN 103979953A
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Abstract
The invention provides a novel rare earth modified microwave dielectric ceramic and a preparation method thereof. The ceramic comprises main materials--BaCO3 and TiO2, a modifier--La2O3, a sintering aid--MnO2, wherein a mass ratio of BaCO3 to TiO2 is 1:4, the proportion of the modifier La2O3 is 1 to 3% of total BaCO3 and TiO2, and the proportion of the sintering aid MnO2 is 0.12% of total BaCO3 and TiO2. The preparation method comprises the following steps: weighing the above-mentioned components in proportion; adding deionized water into BaCO3 and TiO2 and carrying out ball milling and drying; then adding the sintering aid MnO2, carrying out ball milling and drying and then carrying out dry-pressing molding so as to obtain a substrate; and sintering the substrate, cooling the substrate in furnace and carrying out surface processing so as to prepare the microwave dielectric ceramic. The method greatly reduces sintering temperature and sintering time, decreases energy consumption, improves ceramic compactness, broadens production and application process conditions and reduces production cost and process difficulty.
Description
Technical field
The present invention relates to media ceramic field, relate in particular to a kind of novel rare-earth modification microwave-medium ceramics and preparation method thereof.
Background technology
Microwave-medium ceramics be a kind of in microwave frequency band circuit the new function electronic ceramics as dielectric material, it has the features such as specific inductivity is high, loss is low, frequency-temperature coefficient is little.Microwave-medium ceramics can be made the microwave devices such as dielectric resonator, duplexer, dielectric filter, be applied to the fields such as mobile communication, satellite communication military radar and NAVSTAR, to meet the needs of filter unit miniaturization and the contour performance index of loss in above-mentioned base station antenna feeder system.In recent years along with the high speed development of micro-wave communication technology, microwave communication is also more and more higher to the requirement of device and material, except requiring high-k, high quality factor and close to zero resonant frequency and temperature factor, miniaturization, the material integrated, high reliability of pursuing device have become one of the primary study direction in hi-tech microwave ceramics field.Microwave-medium ceramics, as short-wave communication tedhnology key components material, with its good high-frequency dielectric performance, has larger using value in technical field of micro communication.
The preparation method who mostly adopts mechanically mixing to be combined with solid state sintering in prior art, after fully mixing in stirring-type ball milling by solid powder raw material, under high-temperature calcination condition, there is solid state reaction and prepare required ceramic powder, be pressed, solid state sintering becomes medium ceramic material.In traditional preparation method, there are aluminum oxide interpolation properties-correcting agent magnesium oxide, calcium carbonate, silicon-dioxide, boron oxide to carry out modification and make microwave-medium ceramics, also there is tungstate interpolation properties-correcting agent Samarium trioxide to carry out modification and make microwave-medium ceramics.In this traditional preparation method's high-temperature sintering process, powder reactive behavior is poor, and sintering temperature that need to be above up to 900 DEG C and 4 hours above sintering times, caused high production energy consumption.
Summary of the invention
The object of the present invention is to provide a kind of novel rare-earth modification microwave-medium ceramics and preparation method thereof, thereby solve the problem existing in background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of novel rare-earth modification microwave-medium ceramics, is characterized in that: its composition comprises main material BaCO
3and TiO
2, modifer L a
2o
3, sintering aid MnO
2, described BaCO
3with TiO
2mass ratio be 1:4, modifer L a
2o
3proportioning be BaCO
3and TiO
2the 1%-3% of total amount, sintering aid MnO
2proportioning be BaCO
3and TiO
20.12% of total amount.
Lanthanum (La) is a kind of rare earth element, and in the periodic table of elements, lanthanum (La) is adjacent with barium (Ba), and the chemical property of lanthanoid metal is vivaciously oxidizable in air, and it is dimmed rapidly that air is met on fresh surface; Generate oxide compound La
2o
3, La
2o
3chemical property is active, by the BaCO to according to a certain ratio
3and TiO
2material carries out modification, can increase activity and electroconductibility.Logical doping 0.12wt%MnO
2sintering aid reduces ceramic firing temperature and cost, thereby prepares compact structure, the BaTi that sintering temperature is low
4o
9microwave ceramics medium substrate, order polarization later and metallization process obtain microwave-medium ceramics.
A preparation method for novel rare-earth modification microwave-medium ceramics, specifically comprises the steps:
(1) by BaCO
3and TiO
2the proportioning of pressing 1:4 weighs, by modifer L a
2o
3the proportioning of pressing 1%-3% weighs, and mixes, and adds deionized water, the mixing raw material of putting into spherical tank and carrying out ball milling and obtain for 6 hours even refinement;
(2) in air, rise at 1150 DEG C pre-burning after 2 hours with 4 DEG C of per minutes, furnace cooling;
(3) again by (1) step gained mixing raw material fragmentation, carry out ball milling for the second time, cross 80 mesh sieves and dry again, make BaTi
4o
9powder;
(4) press 0.12wt% proportioning weigh MnO
2add BaTi to
4o
9powder, carries out ball milling for the third time, crosses 80 mesh sieves and dries;
(5) powder obtaining in step (4) is added to 10%PVA(polyvinyl alcohol) utilize tablets press to carry out granulation, sieve;
(6) under 30MPa, utilize pressing machine to carry out dry-pressing formed, obtain substrate;
(7) described substrate is carried out to sintering, with the heat-up rate to 600 DEG C of 3 DEG C of per minutes, and be incubated 40 minutes, then with heat-up rate to 680～800 of 5 DEG C of per minutes DEG C and be incubated 2 hours, furnace cooling;
(8) again by surface working, obtain microwave-medium ceramics.
The present invention has following beneficial effect:
The present invention is with BaCO
3and TiO
2for main raw, by doping 0.12wt%MnO
2modification and firing process technological adjustment scheme, thus prepare compact structure, the BaTiO that sintering temperature is low
3microwave ceramics medium substrate.This substrate specific inductivity reaches 38.8, sintering temperature is 680～800 DEG C, polarize and metallization process by postorder, this substrate can meet satellite antenna and mobile base station wave filter dielectric substrate material completely, the present invention has reduced to a great extent sintering temperature and has shortened sintering time, has reduced energy consumption, has improved ceramic compactness, widen production and operation condition, reduced production cost and technical difficulty.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1:
(1) take BaCO
320 parts, TiO
280 parts, La
2o
31 part is mixed, and adds deionized water, the mixing raw material of putting into spherical tank and carrying out ball milling and obtain for 6 hours even refinement;
(2) in air, rise at 1150 DEG C pre-burning after 2 hours with 4 DEG C of per minutes, furnace cooling;
(3) again by (1) step gained mixing raw material fragmentation, carry out ball milling for the second time, cross 80 mesh sieves and dry again, make BaTi
4o
9powder;
(4) take the MnO of 0.12 part
2add BaTi to
4o
9powder, carries out ball milling for the third time, crosses 80 mesh sieves and dries;
(5) powder obtaining in step (4) is added to 10%PVA(polyvinyl alcohol) utilize tablets press to carry out granulation, sieve;
(6) under 30MPa, utilize pressing machine to carry out dry-pressing formed, obtain substrate;
(7) described substrate is carried out to sintering, with the heat-up rate to 600 DEG C of 3 DEG C of per minutes, and be incubated 40min, then with the heat-up rate to 680 of 5 DEG C of per minutes DEG C and be incubated 2h, furnace cooling;
(8) again by surface working, obtain microwave-medium ceramics.
Embodiment 2:
(1) take BaCO
340 parts, TiO
2160 parts, La
2o
34 parts are mixed, and add deionized water, the mixing raw material of putting into spherical tank and carrying out ball milling and obtain for 6 hours even refinement;
(2) in air, rise at 1150 DEG C pre-burning after 2 hours with 4 DEG C of per minutes, furnace cooling;
(3) again by (1) step gained mixing raw material fragmentation, carry out ball milling for the second time, cross 80 mesh sieves and dry again, make BaTi
4o
9powder;
(4) take the MnO of 0.24 part
2add BaTi to
4o
9powder, carries out ball milling for the third time, crosses 80 mesh sieves and dries;
(5) powder obtaining in step (4) is added to 10%PVA(polyvinyl alcohol) utilize tablets press to carry out granulation, sieve;
(6) under 30MPa, utilize pressing machine to carry out dry-pressing formed, obtain substrate;
(7) described substrate is carried out to sintering, with the heat-up rate to 600 DEG C of 3 DEG C of per minutes, and be incubated 40min, then with the heat-up rate to 750 of 5 DEG C of per minutes DEG C and be incubated 2h, furnace cooling;
(8) again by surface working, obtain microwave-medium ceramics.
Embodiment 3
(1) take BaCO
380 parts, TiO
2320 parts of La
2o
312 parts, mix, add deionized water, the mixing raw material of putting into spherical tank and carrying out ball milling and obtain for 6 hours even refinement;
(2) in air, rise at 1150 DEG C pre-burning after 2 hours with 4 DEG C of per minutes, furnace cooling;
(3) again by (1) step gained mixing raw material fragmentation, carry out ball milling for the second time, cross 80 mesh sieves and dry again, make BaTi
4o
9powder;
(4) take the MnO of 0.48 part
2add BaTi to
4o
9powder, carries out ball milling for the third time, crosses 80 mesh sieves and dries;
(5) powder obtaining in step (4) is added to 10%PVA(polyvinyl alcohol) utilize tablets press to carry out granulation, sieve;
(6) under 30MPa, utilize pressing machine to carry out dry-pressing formed, obtain substrate;
(7) described substrate is carried out to sintering, with the heat-up rate to 600 DEG C of 3 DEG C of per minutes, and be incubated 40min, then with the heat-up rate to 800 of 5 DEG C of per minutes DEG C and be incubated 2h, furnace cooling;
(8) again by surface working, obtain microwave-medium ceramics.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (2)
1. novel rare-earth modification microwave-medium ceramics and preparation method thereof, is characterized in that: the composition of described microwave-medium ceramics comprises main material BaCO
3and TiO
2, modifer L a
2o
3, sintering aid MnO
2, described BaCO
3with TiO
2mass ratio be 1:4, modifer L a
2o
3proportioning be BaCO
3and TiO
2the 1%-3% of total amount, sintering aid MnO
2proportioning be BaCO
3and TiO
20.12% of total amount.
2. novel rare-earth modification microwave-medium ceramics and preparation method thereof, is characterized in that: described preparation method comprises the steps:
(1) by BaCO
3and TiO
2the proportioning of pressing 1:4 weighs, by modifer L a
2o
3the proportioning of pressing 1%-3% weighs, and mixes, and adds deionized water, the mixing raw material of putting into spherical tank and carrying out ball milling and obtain for 6 hours even refinement;
(2) in air, rise at 1150 DEG C pre-burning after 2 hours with 4 DEG C of per minutes, furnace cooling;
(3) again by (1) step gained mixing raw material fragmentation, carry out ball milling for the second time, cross 80 mesh sieves and dry again, make BaTi
4o
9powder;
(4) press 0.12wt% proportioning weigh MnO
2add BaTi to
4o
9powder, carries out ball milling for the third time, crosses 80 mesh sieves and dries;
(5) powder obtaining in step (4) is added to 10%PVA(polyvinyl alcohol) utilize tablets press to carry out granulation, sieve;
(6) under 30MPa, utilize pressing machine to carry out dry-pressing formed, obtain substrate;
(7) described substrate is carried out to sintering, with the heat-up rate to 600 DEG C of 3 DEG C of per minutes, and be incubated 40 minutes, then with heat-up rate to 680～800 of 5 DEG C of per minutes DEG C and be incubated 2 hours, furnace cooling;
(8) again by surface working, obtain microwave-medium ceramics.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236959A (en) * | 2015-08-25 | 2016-01-13 | 成都顺康三森电子有限责任公司 | Process for producing microwave electronic ceramics with low dielectric loss and low temperature coefficient |
| CN111099892A (en) * | 2020-01-03 | 2020-05-05 | 山东国瓷功能材料股份有限公司 | Barium titanate-based two-phase composite microwave dielectric ceramic material and preparation method thereof |
| CN111153694A (en) * | 2020-01-06 | 2020-05-15 | 浙江嘉康电子股份有限公司 | Microwave dielectric ceramic material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1397957A (en) * | 2002-08-14 | 2003-02-19 | 清华大学 | Multi-layer ceramic capacitor material with ultrahigh dielectric constant and temp stability and its preparing process |
| CN101323523A (en) * | 2008-07-21 | 2008-12-17 | 贵州大学 | Lanthanum oxide doping barium titanate electronic function ceramic and method for preparing the same |
-
2014
- 2014-04-10 CN CN201410141803.9A patent/CN103979953A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1397957A (en) * | 2002-08-14 | 2003-02-19 | 清华大学 | Multi-layer ceramic capacitor material with ultrahigh dielectric constant and temp stability and its preparing process |
| CN101323523A (en) * | 2008-07-21 | 2008-12-17 | 贵州大学 | Lanthanum oxide doping barium titanate electronic function ceramic and method for preparing the same |
Non-Patent Citations (1)
| Title |
|---|
| 凌栋: "BT4/BST高频介电陶瓷的掺杂研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236959A (en) * | 2015-08-25 | 2016-01-13 | 成都顺康三森电子有限责任公司 | Process for producing microwave electronic ceramics with low dielectric loss and low temperature coefficient |
| CN111099892A (en) * | 2020-01-03 | 2020-05-05 | 山东国瓷功能材料股份有限公司 | Barium titanate-based two-phase composite microwave dielectric ceramic material and preparation method thereof |
| CN111153694A (en) * | 2020-01-06 | 2020-05-15 | 浙江嘉康电子股份有限公司 | Microwave dielectric ceramic material and preparation method thereof |
| CN111153694B (en) * | 2020-01-06 | 2022-04-15 | 浙江嘉康电子股份有限公司 | Microwave dielectric ceramic material and preparation method thereof |
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Application publication date: 20140813 |
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