CN1907912A - ZnO-TiO2 series low-temperature co-burning ceramic material and preparation method thereof - Google Patents
ZnO-TiO2 series low-temperature co-burning ceramic material and preparation method thereof Download PDFInfo
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- CN1907912A CN1907912A CN 200610052930 CN200610052930A CN1907912A CN 1907912 A CN1907912 A CN 1907912A CN 200610052930 CN200610052930 CN 200610052930 CN 200610052930 A CN200610052930 A CN 200610052930A CN 1907912 A CN1907912 A CN 1907912A
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Abstract
The invention relates to a microwave dielectric ceramic material and its preparation method, particularly relates to a zinc oxide-titanium dioxide system low temperature cofired ceramic material and its preparation method. The ceramic material uses zinc titanate and titanium dioxide as main crystal phase and zinc borosilicate glass as a flux. The product can be fired with silver electrode at 900DEG C, and has frequency temperature coefficient tf of 0+-10ppm/DEG C, dielectric constant of 24~35.3, and Q*f of 13000 GHz. The material solves the process problem of casting process and material problem of production of small size multilayer ceramic dielectric microwave Filter. The LTCC technology is used to manufacture multilayer ceramic dielectric microwave Filter with high performance, small size and good consistency and multilayer products like Balun, Antenna and Coupling. The invention also discloses a preparation method for zinc oxide-titanium dioxide system low temperature cofired ceramic material.
Description
Technical field
The present invention is a kind of microwave dielectric ceramic materials and preparation method thereof, relates in particular to a kind of ZnO-TiO
2Series low-temperature co-burning pottery LTCC (Low Temperature Co-fired Ceramics) material and preparation method thereof.
Background technology
Along with the develop rapidly of micro-wave communication industry, its end product also is with rapid changepl. never-ending changes and improvements, and also must catch up with the development of complete machine or end product as the electronic devices and components of end product parts.Having entered the ultimate challenge that multilayer ceramic medium microwave Filter (wave filter) and multilayer Balun (balun), Bluetooth (bluetooth), antenna products such as (antennas) face since 2002 is high-performance, small volume requirement.Current research shows: multilayer ceramic medium microwave Filter small size new product development cycle is in quick shortening, and the dimensional requirement to ceramic dielectic microwave Filter in 1994 is 4.5mm * 3.2mm; 2000 is 3.2mm * 2.5mm; 2002 is 2.5mm * 2.0mm; 2003 be the 2.0mm * 1.25mm or the 1.6mm * 0.8mm of small volume more.Widely used traditional technology production " solely stone type " is gone up in communication now, and the structure minimum volume is 2.8mm * 1.3mm, and more the small volume product just requires product must adopt new production technique (as LTCC technology) better to realize.
The research worker of microwave ceramic material is at research ZnO-TiO
2Based material adopts non-zinc borosilicate glass (ZnO-B
2O
3-SiO
2Glass) other contains the salt or the oxide compound of element B and makes fusing assistant, runs into the technology difficult problem of curtain coating in being converted into production process; And adopting other salt that does not contain element B or oxide compound to make fusing assistant or additive, the performance of material or technology all are difficult to reach requirement.
Summary of the invention
In order to solve the technical problem that above-mentioned microwave ceramic material exists in producing and using, the purpose of this invention is to provide a kind of ZnO-TiO can be low temperature co-fired, good manufacturability, low cost, high-performance and high stability
2Series low-temperature co-burning ceramic material.
Another object of the present invention provides above-mentioned ZnO-TiO
2The preparation method of series low-temperature co-burning ceramic material.
In order to realize first purpose of the present invention, the present invention adopts following technical scheme:
ZnO-TiO
2Series low-temperature co-burning ceramic material, prescription by weight percentage is composed as follows:
Zinc titanate (ZnTiO
3) 79.5～98.5%
Titanium dioxide (TiO
2) 0.95～16.50%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 0.5～4.8%.
As preferably: above-mentioned ZnO-TiO
2Series low-temperature co-burning ceramic material, can form by the prescription of following weight percent:
Zinc titanate (ZnTiO
3) 90.0～98.5%
Titanium dioxide (TiO
2) 0.95～7.0%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 0.5～3.0%.
As preferably: above-mentioned ZnO-TiO
2Series low-temperature co-burning ceramic material, also can form by the prescription of following weight percent:
Zinc titanate (ZnTiO
3) 83.0～90.0%
Titanium dioxide (TiO
2) 6.9～14.0%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 0.5～3.0%.
As preferably: above-mentioned ZnO-TiO
2Series low-temperature co-burning ceramic material, also can form by the prescription of following weight percent:
Zinc titanate (ZnTiO
3) 83.0～90.0%
Titanium dioxide (TiO
2) 6.9～12.9%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 3.0～4.8%.
As preferably: above-mentioned ZnO-TiO
2Series low-temperature co-burning ceramic material, also can form by the prescription of following weight percent:
Zinc titanate (ZnTiO
3) 79.5～83.0%
Titanium dioxide (TiO
2) 12.9～16.5%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 3.0～4.8%.
As preferably: ZnO, the B of the zinc borosilicate glass in above-mentioned each scheme
2O
3, SiO
2By its molar percentage is that ZnO accounts for 40%～65%, B
2O
3Account for 25%～45%, SiO
2Account for 8%～20%.
In order to realize another object of the present invention, the present invention has adopted following technical scheme:
The described ZnO-TiO of above-mentioned any one technical scheme
2The preparation method of series low-temperature co-burning ceramic material comprises the steps:
1) rich titanium zinc titanate ZnTiO
3(TiO
2) preparation, with zinc oxide (ZnO), titanium dioxide (TiO
2) be mixed into uniform mixture by prescription and deionized water, mixture is crossed screen cloth and carried out drying, again dry powder is ground into even fine powder, to calcine 2～4 hours down at 780 ℃, agitated ball mill is pulverized, again dry for standby;
2) zinc borosilicate glass (ZnO-B
2O
3-SiO
2) preparation, ZnO, B
2O
3, SiO
2Be mixed into uniform mixture by prescription and deionized water, cross screen cloth and carry out drying, dry powder is ground into even fine powder again, with above-mentioned identical method mixing, drying, liquid glass is founded in calcining under 1100 ± 30 ℃, quenches, and pulverizes standby;
3) with above-mentioned rich titanium zinc titanate ZnTiO
3(TiO
2), the zinc borosilicate glass, put into vertical ball mill by prescription and pulverized 3～6 hours, obtain fine powder;
4) adopt the method for flow casting molding to laminate above-mentioned fine powder, laminated shim, employing waits the method for static pressure or mechanical workout to make finished product, and under 900 ± 20 ℃, calcines 2～4 hours.
Scheme as an alternative: step 2) B
2O
3Can use H
3BO
3Substitute.
As preferred version: zinc oxide (ZnO), titanium dioxide (TiO above-mentioned steps 1)
2) in the agitated ball mill that is provided with the Polyurethane liner, be mixed into uniform mixture with deionized water.
As preferred version: above-mentioned steps 3) described fine powder D50=1.1 μ m～1.3 μ m, specific surface area S/V=50000cm
2/ cm
3～61000cm
2/ cm
3
In the prescription of the present invention, with the ZnTiO of rich titanium
3(TiO
2) be principal crystalline phase, its sintering temperature is low, and the present invention can burn with silver electrode below 900 ℃ altogether; The quality factor height; Mol ratio TiO in the prescription
2: ZnO is a frequency-temperature coefficient of adjusting principal crystalline phase greater than 1; The zinc borosilicate glass are fusing assistant, reduce the sintering temperature of material, can solve the technological problems of curtain coating operation.
The present invention who adopts above-mentioned prescription to form, the DIELECTRIC CONSTANT of material
r=24～35.3, the frequency-temperature coefficient τ of material
f=0 ± 10ppm/ ℃, has higher quality factor.Adopt the present invention can better realize LTCC technology, be mainly used in multilayer ceramic medium microwave Filter and productions such as multilayer Balun, Bluetooth, antenna, have the following advantages:
1, showed LTCC technology preferably.LTCC microwave dielectric material sintering temperature of the present invention is 900 ℃, and energy and cheap Ag metal burn altogether, adopts the LTCC explained hereafter, and minimum volume ceramic dielectic microwave Filter product is of a size of 2.0mm * 1.25mm; Success of the present invention also makes microwave Filter design a model simultaneously or structure becomes more flexible, and the performance of Filter is more superior, stable.
2, solved technological problems in the curtain coating operation.Material of the present invention has solved the technological problems that occurs in the curtain coating operation in the production process, and it is more stable to make curtain coating produce.
3, low cost.Utilize the multilayer ceramic medium microwave Filter product excellent electrical properties of material preparation of the present invention, and the price of ceramic raw material is low, greatly reduces product material costs such as microwave Filter.
4, high stability.Material of the present invention has the good characteristics of frequency-temperature coefficient, by the zinc borosilicate glass of adding negative frequency temperature factor and the TiO of positive frequency temperature factor
2, the frequency-temperature coefficient of adjusting material is τ
f=0 ± 10ppm/ ℃, use various product dielectric properties under different envrionment temperatures of material preparation of the present invention to keep stable.
5, high-performance.Material of the present invention has high Q*f value, and the highest Q*f value reaches 13000GHz, utilizes the product excellent electrical properties such as multilayer ceramic medium microwave Filter of material preparation of the present invention.
Embodiment
Further describe the ZnO-TiO of various embodiments of the present invention to of the present invention below in conjunction with example
2The prescription of series low-temperature co-burning ceramic material is as shown in table 1.
Table 1
Its preparation method is as follows:
1, the principal crystalline phase ZnTiO of rich titanium
3(TiO
2) be with zinc oxide (ZnO), titanium dioxide (TiO
2) in the agitated ball mill that the Polyurethane liner is arranged, be mixed into uniform mixture by the prescription in the table 1 with deionized water, mixture is crossed 120 eye mesh screens in stainless steel cask, carry out drying, again dry powder is ground into even fine powder, Al packs into
2O
3In the corundum crucible, calcined 2～4 hours down, in agitated ball mill, pulverize again, again dry for standby at 780 ℃.
2, zinc borosilicate glass (ZnO-B
2O
3-SiO
2) be with ZnO, B
2O
3, SiO
2By its molar percentage than 50%, 40%, 10% and deionized water be mixed into uniform mixture, mixture is crossed 120 eye mesh screens in stainless steel cask, carry out drying, again dry powder is ground into even fine powder, pack in the platinum crucible, liquid glass was founded in calcining in 60 minutes under 1100 ± 30 ℃, quench, pulverize standby.
3, with the principal crystalline phase ZnTiO of above-mentioned rich titanium
3(TiO
2), the zinc borosilicate glass, put into vertical ball mill by certain weight ratio and pulverized 3～6 hours, obtain D50=1.1 μ m～1.3 μ m, specific surface area S/V=50000cm
2/ cm
3～61000cm
2/ cm
3Fine powder.
Adopt the method for flow casting molding to laminate above-mentioned fine powder, laminated shim, the method of static pressure such as employing, mechanical workout is made diameter phi=12mm, it highly is the sample of H=5.5～7mm, under 895 ± 20 ℃, calcined 2～4 hours, and adopted Agilent 8719ET network analyzer, measure DIELECTRIC CONSTANT according to the Hakki-Coleman method
rAnd quality factor q, temperature coefficient of resonance frequency τ
fAdopt the cavity method to measure, the result is as shown in the table:
Claims (10)
1.ZnO-TiO
2Series low-temperature co-burning ceramic material is characterized in that its prescription by weight percentage is composed as follows:
Zinc titanate (ZnTiO
3) 79.5～98.5%
Titanium dioxide (TiO
2) 0.95～16.50%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 0.5～4.8%.
2. ZnO-TiO according to claim 1
2Series low-temperature co-burning ceramic material is characterized in that its prescription by weight percentage is composed as follows:
Zinc titanate (ZnTiO
3) 90.0～98.5%
Titanium dioxide (TiO
2) 0.95～7.0%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 0.5～3.0%.
3. ZnO-TiO according to claim 1
2Series low-temperature co-burning ceramic material is characterized in that its prescription by weight percentage is composed as follows:
Zinc titanate (ZnTiO
3) 83.0～90.0%
Titanium dioxide (TiO
2) 6.9～14.0%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 0.5～3.0%.
4. ZnO-TiO according to claim 1
2Series low-temperature co-burning ceramic material is characterized in that its prescription by weight percentage is composed as follows:
Zinc titanate (ZnTiO
3) 83.0～90.0%
Titanium dioxide (TiO
2) 6.9～12.9%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 3.0～4.8%.
5. ZnO-TiO according to claim 1
2Series low-temperature co-burning ceramic material is characterized in that its prescription by weight percentage is composed as follows:
Zinc titanate (ZnTiO
3) 79.5～83.0%
Titanium dioxide (TiO
2) 12.9～16.5%
Zinc borosilicate glass (ZnO-B
2O
3-SiO
2) 3.0～4.8%.
6. according to the described ZnO-TiO of any claim of claim 1～5
2ZnO, B in the series low-temperature co-burning ceramic material zinc borosilicate glass
2O
3, SiO
2By its molar percentage is that ZnO accounts for 40%～65%, B
2O
3Account for 25%～45%, SiO
2Account for 8%～20%.
7. according to the described ZnO-TiO of any claim of claim 1～5
2The preparation method of series low-temperature co-burning ceramic material is characterized in that comprising the steps:
1) rich titanium zinc titanate ZnTiO
3(TiO
2) preparation, with zinc oxide (ZnO), titanium dioxide (TiO
2) be mixed into uniform mixture by prescription and deionized water, mixture is crossed screen cloth and carried out drying, again dry powder is ground into even fine powder, to calcine 2～4 hours down at 780 ℃, agitated ball mill is pulverized, again dry for standby;
2) zinc borosilicate glass (ZnO-B
2O
3-SiO
2) preparation, ZnO, B
2O
3, SiO
2Be mixed into uniform mixture by prescription and deionized water, cross screen cloth and carry out drying, dry powder is ground into even fine powder again, with above-mentioned identical method mixing, drying, liquid glass is founded in calcining under 1100 ± 30 ℃, quenches, and pulverizes standby;
3) with above-mentioned rich titanium zinc titanate ZnTiO
3(TiO
2), the zinc borosilicate glass, put into vertical ball mill by prescription and pulverized 3～6 hours, obtain fine powder;
4) adopt the method for flow casting molding to laminate above-mentioned fine powder, laminated shim, employing waits the method for static pressure or mechanical workout to make finished product, and under 900 ± 20 ℃, calcines 2～4 hours.
8. ZnO-TiO according to claim 7
2The preparation method of series low-temperature co-burning ceramic material is characterized in that step 2) B
2O
3Can use H
3BO
3Substitute.
9. ZnO-TiO according to claim 7
2The preparation method of series low-temperature co-burning ceramic material is characterized in that zinc oxide in the step 1) (ZnO), titanium dioxide (TiO
2) in the agitated ball mill that is provided with the Polyurethane liner, be mixed into uniform mixture with deionized water.
10. ZnO-TiO according to claim 7
2The preparation method of series low-temperature co-burning ceramic material is characterized in that the described fine powder D50=1.1 of step 3) μ m～1.3 μ m, specific surface area S/V=50000cm
2/ cm
3～61000cm
2/ cm
3
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|---|---|---|---|
| CNB2006100529307A CN100417622C (en) | 2006-08-15 | 2006-08-15 | ZnO-TiO2 series low-temperature co-burning ceramic material and preparation method thereof |
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| CN100417622C CN100417622C (en) | 2008-09-10 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146345A (en) * | 2013-01-30 | 2013-06-12 | 云南云天化股份有限公司 | Microwave dielectric materials capable of burning with copper electrodes together, preparation method and application thereof |
| CN104193326A (en) * | 2014-07-16 | 2014-12-10 | 电子科技大学 | LTCC material and preparation method thereof |
| CN104193324A (en) * | 2014-08-14 | 2014-12-10 | 电子科技大学 | ZnO-MgO-TiO2 serial LTCC (low temperature co-fired ceramic) material |
| CN107867841A (en) * | 2016-09-22 | 2018-04-03 | 施海月 | A kind of TiO2Adulterate ZnO/SiO2The preparation method of microwave-medium ceramics |
| CN110229002A (en) * | 2019-07-04 | 2019-09-13 | 贵州振华电子信息产业技术研究有限公司 | A kind of low-temperature co-burning ceramic material and preparation method |
| CN113943147A (en) * | 2021-12-07 | 2022-01-18 | 无锡市惠丰电子有限公司 | Preparation method of dielectric ceramic material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3103296B2 (en) * | 1995-06-30 | 2000-10-30 | ティーディーケイ株式会社 | Dielectric porcelain, method of manufacturing the same, and electronic component using the same |
-
2006
- 2006-08-15 CN CNB2006100529307A patent/CN100417622C/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146345A (en) * | 2013-01-30 | 2013-06-12 | 云南云天化股份有限公司 | Microwave dielectric materials capable of burning with copper electrodes together, preparation method and application thereof |
| CN103146345B (en) * | 2013-01-30 | 2014-08-27 | 云南云天化股份有限公司 | Microwave dielectric materials capable of burning with copper electrodes together, preparation method and application thereof |
| CN104193326A (en) * | 2014-07-16 | 2014-12-10 | 电子科技大学 | LTCC material and preparation method thereof |
| CN104193326B (en) * | 2014-07-16 | 2015-10-28 | 电子科技大学 | A kind of LTCC material and preparation method thereof |
| CN104193324A (en) * | 2014-08-14 | 2014-12-10 | 电子科技大学 | ZnO-MgO-TiO2 serial LTCC (low temperature co-fired ceramic) material |
| CN107867841A (en) * | 2016-09-22 | 2018-04-03 | 施海月 | A kind of TiO2Adulterate ZnO/SiO2The preparation method of microwave-medium ceramics |
| CN110229002A (en) * | 2019-07-04 | 2019-09-13 | 贵州振华电子信息产业技术研究有限公司 | A kind of low-temperature co-burning ceramic material and preparation method |
| CN113943147A (en) * | 2021-12-07 | 2022-01-18 | 无锡市惠丰电子有限公司 | Preparation method of dielectric ceramic material |
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|---|---|
| CN100417622C (en) | 2008-09-10 |
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