CN100494117C - Low dielectric comsumption CaCu3Ti4O12 ceramic preparing method - Google Patents
Low dielectric comsumption CaCu3Ti4O12 ceramic preparing method Download PDFInfo
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- CN100494117C CN100494117C CNB2007100091119A CN200710009111A CN100494117C CN 100494117 C CN100494117 C CN 100494117C CN B2007100091119 A CNB2007100091119 A CN B2007100091119A CN 200710009111 A CN200710009111 A CN 200710009111A CN 100494117 C CN100494117 C CN 100494117C
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Abstract
This invention relates to preparation method of a low electric loss CaCu3Ti4O12 ceramic.Firstly mix the raw material calcium carbonate, titanium dioxide and cupric oxide according to molar ratio of 1:4:3, wet method ball mill to gain mixture powder. Drythe mixture powder, then preburn at 850 to 1000deg. Ball mill the mixture powder after preburning, past at least 80 orders screen mesh, dry, add polyvinyl alcohol and grind, corning, dry pressing and moulding, then cold equal steady pressure for shaping, sintering the body, then furnace cool.
Description
Technical field
The present invention relates to a kind of CaCu
3Ti
4O
12(C TO) pottery especially relates to a kind of employing cold isostatic pressing method and prepares low-dielectric loss CaCu
3Ti
4O
12Pottery.
Background technology
Nearest CaCu
3Ti
4O
12Material has caused people's extensive concern, and it has unusual high specific inductivity, about 10 near room temperature
4～10
5, and good thermostability is arranged in the temperature range of 100～600K.Temperature is reduced to below the 100K, ε sharply is reduced to about 100, but do not observe the long-range structure phase transformation (1, Subramanian M A, Li D, Duan N, et al.Highdielectric constant ACu3Ti4O12 and ACu3Ti3FeO12 phases[J] .Solid State Chem, 2000,15:323-325; 2, Ramirez A P, Subramanian M A, Gardel M, et al.Giant dielectr constant response in acopper-titanate[J] .Solid State Commun, 2001,15:217-220; 3, Subramanian M A, Sleight A W.ACu3Ti4O12 and ACu3Ru4O perovskites:high dielectric constants and valence degeneracy[J] .Sol State Sci, 2002,4:347-351; 4, Homes C C, Vogt T, Shapiro S M, et al.Optical responsehigh-dielectric-constant perovskite-related oxide[J] .Science, 2001,12:625-629; 5, Moussa S M, Kennedy B J.Structural studies of the distorted perovski Ca0.25Cu0.75TiO3[J] .Mater Res Bull, 2001,36:2525-2529) these character make it be with a wide range of applications in electronics industry.
Different experimentations, experimental technique and preparation technology have remarkable influence to the dielectric properties of CCTO material.At present in the preparation process of the CCTO pottery of reporting in the document, many employing long-time pre-burnings (8h), perhaps pre-sinter process repeatedly, sintering time is very long, from 10h to tens hour even up to a hundred hours, make that preparation process complexity, cycle are long, energy consumption is bigger, and the short period of time sintering prepares the few of CCTO pottery.
The loss tangent of ceramic capacitor material is low more, helps production application more.But the CCTO material of preparation generally has bigger dielectric loss when having high permittivity.Room temperature lowest loss angle tangent value D is 0.05 (D.P.Cann under the 1kHz of bibliographical information at present, S.Aygun, X.Tan, Extended Abstracts of the 11th USJapan Seminar onDielectric and Piezoelectric Ceramics, Sapporo Japan, 2003:153-156) with 0.06 (Li Xuewei, the firm .CaCu of State of Zhao
3Ti
4O
12Microstructure of ceramics and dielectric properties [J]. Liaoning Project Technology University's journal, 2005,25).
Summary of the invention
The object of the present invention is to provide a kind of low-dielectric loss CaCu
3Ti
4O
12The preparation method of pottery.
Concrete steps of the present invention are:
1) earlier raw material lime carbonate, titanium dioxide and cupric oxide were mixed in 1: 4: 3 in molar ratio, wet ball grinding gets mixed powder.
2) with the mixed powder oven dry, with the mixed powder pre-burning, the temperature of pre-burning is 850～1000 ℃ after the oven dry.
3) mixed powder after the pre-burning carries out ball milling again, crosses 80 eye mesh screens, drying at least, adds polyvinyl alcohol (PVA), and grinding, granulation get the granulation powder.
4) the granulation dried bean noodles is molded, cold isostatic compaction gets base substrate again.
5) with blank sintering, furnace cooling gets target product then.
Before the test, target product is carried out surface finish, last silver electrode is done the dielectric properties test.
Wet ball grinding is crossed 80 eye mesh screens at least.Mixed powder after grinding is dried in baking oven.With powder pre-burning in the agate crucible, can be incubated 1～6h after the pre-burning then.The amount that adds polyvinyl alcohol is 7%～10% of a dry back mixed powder.The pressure that the granulation dried bean noodles is molded is preferably 100～250MPa; The pressure of cold isostatic compaction is preferably 100～250MPa.The agglomerating temperature is preferably 1020～1100 ℃, also insulation behind the sintering.
Adopt the prepared CaCu of the present invention
3Ti
4O
12Pottery, its base substrate densification, pore quantity is few, and shrinking percentage is low, can more sinter porcelain under the low temperature, and dielectric properties are improved significantly, and its loss tangent is minimum to be 0.024, is a kind of method of the effective CCTO of improvement dielectric properties.
Embodiment
Embodiment 1
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 80 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1: 1.2.Use planetary ball mill ball milling 4h, rotating speed 250 commentaries on classics/min, mixed powder after grinding is dried in baking oven.With mixed powder pre-burning in the agate crucible, 950 ℃ of pre-burnings also are incubated 2h then.Mixed powder after the pre-burning carries out ball milling, drying again.The PVA that adds 10% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 150MPa pressure, be diameter 9mm at the 200MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1020 ℃ of sintering and be incubated 2h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.Its D=0.024, ε r=3535.4.
Embodiment 2
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 100 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1.1: 1.1.Use planetary ball mill ball milling 4h, rotating speed 250 commentaries on classics/min, mixed powder after grinding is dried in baking oven.With mixed powder pre-burning in the agate crucible, 850 ℃ of pre-burnings also are incubated 6h then.Mixed powder after the pre-burning carries out ball milling, drying again.The PVA that adds 7% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 200MPa pressure, be diameter 9mm at the 150MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1050 ℃ of sintering and be incubated 2h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.Its D=0.024, ε r=3535.4.
Embodiment 3
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 120 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 0.9: 0.9.Use planetary ball mill ball milling 4h, rotating speed 250 commentaries on classics/min, mixed powder after grinding is dried in baking oven.With mixed powder pre-burning in the agate crucible, 900 ℃ of pre-burnings also are incubated 1h then.Mixed powder after the pre-burning carries out ball milling, drying again.The PVA that adds 8% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 100MPa pressure, be diameter 9mm at the 250MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1100 ℃ of sintering and be incubated 2h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 4
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 80 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1.2: 1.Use planetary ball mill ball milling 5h, rotating speed 200 commentaries on classics/min, mixed powder after grinding is dried in baking oven.With mixed powder pre-burning in the agate crucible, 1000 ℃ of pre-burnings also are incubated 3h then.Mixed powder after the pre-burning carries out ball milling, drying again.The PVA that adds 10% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 250MPa pressure, be diameter 9mm at the 100MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1060 ℃ of sintering and be incubated 2h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 5
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 120 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1: 1.2.Use planetary ball mill ball milling 4h, rotating speed 250 commentaries on classics/min, mixed powder after grinding is dried in baking oven.With mixed powder pre-burning in the agate crucible, 950 ℃ of pre-burnings also are incubated 5h then.Mixed powder after the pre-burning carries out ball milling, drying again.The PVA that adds 9% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 150MPa pressure, be diameter 9mm at the 150MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1030 ℃ of sintering and be incubated 2h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 6
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 100 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1.1: 1.3.Use planetary ball mill ball milling 6h, rotating speed 200 commentaries on classics/min.Mixed powder after grinding is dried in baking oven.Then with mixed powder pre-burning in the agate crucible, 850 ℃ of pre-burnings and be incubated the 6h. pre-burning after powder carry out ball milling, drying again.The PVA that adds 7% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 100MPa pressure, be diameter 8mm at the 250MPa cold isostatic compaction again, the disk of thickness 1.5mm.Base substrate in electric furnace in 1050 ℃ of sintering and be incubated 2h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.Its D=0.066, ε r=3554.9.
Embodiment 7
Raw material lime carbonate, titanium dioxide and cupric oxide were mixed in 1: 4: 3 in molar ratio, and wet ball grinding in agate jar is crossed 120 eye mesh screens, and ball-milling medium is a distilled water, presses mass ratio, raw material: agate ball: distilled water=1: 0.9: 1.2.Use planetary ball mill ball milling 5h, the powder behind the rotating speed 250 commentaries on classics/min. ball millings is dried in baking oven.Then with powder pre-burning in the agate crucible, 1000 ℃ of pre-burnings and be incubated the 1h. pre-burning after powder carry out ball milling, drying again.The PVA that adds 8% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 150MPa pressure, be diameter 9mm at the 200MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1020 ℃ of sintering and be incubated 2h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 8
Raw material lime carbonate, titanium dioxide and cupric oxide were mixed in 1: 4: 3 in molar ratio, and wet ball grinding in agate jar is crossed 100 eye mesh screens, and ball-milling medium is a distilled water, compares raw material by quality; Agate ball: distilled water=1: 1: 1.1.Use planetary ball mill ball milling 5h, the powder behind the rotating speed 280 commentaries on classics/min. ball millings is dried in baking oven.Then with powder pre-burning in the agate crucible, 1000 ℃ of pre-burnings and be incubated the 2h. pre-burning after powder carry out ball milling, drying again.The PVA that adds 8% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 200MPa pressure, be diameter 8mm at the 150MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1050 ℃ of sintering and be incubated 3h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 9
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 80 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1.1: 1.2.Use planetary ball mill ball milling 3h, the powder behind the rotating speed 300 commentaries on classics/min. ball millings is dried in baking oven.Then with powder pre-burning in the agate crucible, 1000 ℃ of pre-burnings and be incubated the 4h. pre-burning after powder carry out ball milling, drying again.The PVA that adds 10% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 180MPa pressure, be diameter 9mm at the 150MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1100 ℃ of sintering and be incubated 3h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 10
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 100 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1.1: 1.Use planetary ball mill ball milling 4h, the powder behind the rotating speed 250 commentaries on classics/min. ball millings is dried in baking oven.Then with powder pre-burning in the agate crucible, 950 ℃ of pre-burnings and be incubated the 5h. pre-burning after powder carry out ball milling, drying again.The PVA that adds 9% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 200MPa pressure, be diameter 9mm at the 180MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1050 ℃ of sintering and be incubated 3h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 11
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 120 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1.1: 1.Use planetary ball mill ball milling 3h, the powder behind the rotating speed 300 commentaries on classics/min. ball millings is dried in baking oven.Then with powder pre-burning in the agate crucible, 850 ℃ of pre-burnings and be incubated the 2h. pre-burning after powder carry out ball milling, drying again.The PVA that adds 10% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 150MPa pressure, be diameter 9mm at the 150MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1020 ℃ of sintering and be incubated 3h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 12
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 80 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1.1: 1.2.Use planetary ball mill ball milling 5h, the powder behind the rotating speed 250 commentaries on classics/min. ball millings is dried in baking oven.Then with powder pre-burning in the agate crucible, 960 ℃ of pre-burnings and be incubated the 5h. pre-burning after powder carry out ball milling, drying again.The PVA that adds 8% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 250MPa pressure, be diameter 9mm at the 150MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1100 ℃ of sintering and be incubated 4h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Embodiment 13
Raw material lime carbonate, titanium dioxide and cupric oxide 1: 4: 3 are in molar ratio mixed, and wet ball grinding in agate jar is crossed 100 eye mesh screens, and ball-milling medium is a distilled water, by quality than raw material: agate ball: distilled water=1: 1.1: 0.9.Use planetary ball mill ball milling 4h, the powder behind the rotating speed 300 commentaries on classics/min. ball millings is dried in baking oven.Then with powder pre-burning in the agate crucible, 950 ℃ of pre-burnings and be incubated the 6h. pre-burning after powder carry out ball milling, drying again.The PVA that adds 10% mass percent then, grinding, granulation in agate mortar.The granulation powder is dry-pressing formed under 150MPa pressure, be diameter 9mm at the 200MPa cold isostatic compaction again, the disk of thickness 2mm.Base substrate in electric furnace in 1020 ℃ of sintering and be incubated 4h, furnace cooling then.Surface finish, last silver electrode is carried out the dielectric properties test.
Claims (5)
1. low-dielectric loss CaCu
3Ti
4O
12The preparation method of pottery is characterized in that its concrete steps are:
1) earlier raw material lime carbonate, titanium dioxide and cupric oxide were mixed in 1: 4: 3 in molar ratio, wet ball grinding gets mixed powder, and wet ball grinding is crossed 80 eye mesh screens at least;
2) with the mixed powder oven dry, with the mixed powder pre-burning, the temperature of pre-burning is 850～1000 ℃ after the oven dry;
3) mixed powder after the pre-burning carries out ball milling again, crosses 80 eye mesh screens, drying at least, adds polyvinyl alcohol, and grinding, granulation get the granulation powder;
4) the granulation dried bean noodles is molded, cold isostatic compaction gets base substrate again, and the molded pressure of granulation dried bean noodles is 100～250MPa, and the pressure of cold isostatic compaction is 100～250MPa;
5) with blank sintering, furnace cooling gets target product then.
2. a kind of low-dielectric loss CaCu as claimed in claim 1
3Ti
4O
12The preparation method of pottery is characterized in that pre-burning insulation 1～6h.
3. a kind of low-dielectric loss CaCu as claimed in claim 1
3Ti
4O
12The preparation method of pottery is characterized in that the amount that adds polyvinyl alcohol is 7%～10% of dry back mixed powder.
4. a kind of low-dielectric loss CaCu as claimed in claim 1
3Ti
4O
12The preparation method of pottery is characterized in that the agglomerating temperature is 1020～1100 ℃.
5. a kind of low-dielectric loss CaCu as claimed in claim 1
3Ti
4O
12The preparation method of pottery is characterized in that being incubated 2h under sintering temperature.
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|---|---|---|---|
| CNB2007100091119A CN100494117C (en) | 2007-06-18 | 2007-06-18 | Low dielectric comsumption CaCu3Ti4O12 ceramic preparing method |
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|---|---|---|---|
| CNB2007100091119A CN100494117C (en) | 2007-06-18 | 2007-06-18 | Low dielectric comsumption CaCu3Ti4O12 ceramic preparing method |
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| CN100494117C true CN100494117C (en) | 2009-06-03 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391769B (en) * | 2008-10-24 | 2011-08-17 | 昆明理工大学 | Preparation of barium carbide dielectric block body material by reactive synthesis |
| CN101792308B (en) * | 2010-02-11 | 2012-06-27 | 哈尔滨工业大学 | Shell-core structure ceramic material CaCu3Ti4O12 and preparation method thereof |
| CN101798213B (en) * | 2010-03-12 | 2012-10-10 | 厦门大学 | Double-doped ceramic material with high dielectric constant and preparation method thereof |
| CN102173780B (en) * | 2011-01-11 | 2013-09-18 | 桂林理工大学 | Preparation method of rare earth modified pressure-sensitive material |
| CN102173781A (en) * | 2011-02-24 | 2011-09-07 | 西北工业大学 | Preparation method of CaCu3Ti4O12 ceramic |
| CN103382111A (en) * | 2013-07-11 | 2013-11-06 | 中国科学院福建物质结构研究所 | NaxCu3NbyTi3O12 based giant dielectric ceramic material and preparation method thereof |
| CN103951414B (en) * | 2014-04-25 | 2016-01-27 | 厦门大学 | There is the manufacture method of the huge specific inductivity of low-dielectric loss and pressure-sensitive character stupalith |
| CN109912305B (en) * | 2019-04-25 | 2022-03-04 | 重庆大学 | CaCu with high potential gradient and low dielectric loss3Ti4O12Pressure-sensitive ceramic and preparation method thereof |
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2007
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Non-Patent Citations (2)
| Title |
|---|
| CaCu3Ti4O12陶瓷显微结构及介电性能. 李学伟等.辽宁工程技术大学学报，第25卷第3期. 2006 |
| CaCu3Ti4O12陶瓷显微结构及介电性能. 李学伟等.辽宁工程技术大学学报，第25卷第3期. 2006 * |
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Assignee: Xiamen Ningly Electronics Co., Ltd. Assignor: Xiamen University Contract record no.: 2011350000251 Denomination of invention: Method for preparing low dielectric loss CaCu[sub]3[/sub]Ti[sub]4[/sub]O[sub]12[/sub] ceramic Granted publication date: 20090603 License type: Exclusive License Open date: 20071114 Record date: 20111031 |
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