CN101913868B - Method for preparing potassium-sodium niobate textured ceramic and potassium-sodium niobate single crystal - Google Patents
Method for preparing potassium-sodium niobate textured ceramic and potassium-sodium niobate single crystal Download PDFInfo
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- CN101913868B CN101913868B CN2010102474748A CN201010247474A CN101913868B CN 101913868 B CN101913868 B CN 101913868B CN 2010102474748 A CN2010102474748 A CN 2010102474748A CN 201010247474 A CN201010247474 A CN 201010247474A CN 101913868 B CN101913868 B CN 101913868B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 31
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000013078 crystal Substances 0.000 title abstract description 16
- 238000000034 method Methods 0.000 title abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 235000015895 biscuits Nutrition 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 238000001238 wet grinding Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims description 22
- 238000009413 insulation Methods 0.000 claims description 16
- 238000005469 granulation Methods 0.000 claims description 12
- 230000003179 granulation Effects 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 8
- 229910052573 porcelain Inorganic materials 0.000 claims description 8
- 238000000748 compression moulding Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 6
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 5
- 239000008187 granular material Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
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Abstract
The invention aims to provide a method for preparing potassium-sodium niobate textured ceramic and potassium-sodium niobate single crystal. K0.5Na0.5NbO3 is used as a main material and LiBiO3 or BiNiO3 is used as a doping raw material; and the method comprises the following steps of: performing wet-milling on the materials by using anhydrous alcohol as a medium and drying the materials to synthesize a ceramic material; performing secondary ball milling on the ceramic material, drying the ceramic material and adding an adhesive into the ceramic material to granulate; pressing the mixture under the pressure of 110MPa to prepare a biscuit sample; horizontally placing the biscuit sample into a high temperature electric furnace for sintering; and cooling the sintered biscuit sample along with the furnace to the room temperature so as to prepare KNN-based ceramic, wherein the single crystal with size of over 2mm can also be obtained by controlling the sintering temperature and the sintering time. By using the conventional ceramic preparation process, the KNN ceramic with superior preferred orientation is prepared under normal conditions; and the single crystal with size of over 2mm can also be obtained by controlling the sintering temperature and the sintering time.
Description
Technical field
The present invention relates to lead-free piezoceramic material, specifically is the preparation method of potassium-sodium niobate textured ceramic and potassium-sodium niobate monocrystalline.
Background technology
With the PbZrO that forms by ferroelectric and antiferroelectric
3-PbTiO
3(PZT) system solid solution is that the lead base piezoelectric ceramic of representative is widely used in fields such as transducer, driver resonator.Because at PZT is that lead oxide content poisonous in the pottery surpasses more than 60% of raw material gross mass, has brought serious harm to environment for human survival, the unleaded of piezoelectric ceramic is the urgent hope of human development.Compare potassium-sodium niobate (K with other system leadless piezoelectric ceramics of current research
0.5Na
0.5NbO
3, KNN) series piezoelectric ceramic because of have that dielectric constant is little, piezoelectric property is high, frequency constant is big, density is little, Curie temperature is high and component to characteristics such as human body close friends, be considered to one of leadless piezoelectric material material of very promising alternative PZT.
Generally, by the crystal habit of pottery, pottery can be divided into polycrystalline and monocrystalline two big classes.Single-crystal ceramic is not because receive the influence of grain size, grain orientation, crystal boundary and the porosity etc., thereby has excellent more performance than polycrystalline ceramics, as has dielectric, piezoelectricity and the optical property etc. of excellence more.Concerning PZT system pottery, the piezoelectric constant of monocrystalline will exceed an one magnitude than polycrystalline, and the PZN-PT monocrystalline that people such as S.E.Park studied in 1996 is in non-pole axis direction<001>Last d
33Reach 2500pC/N, electromechanical coupling factor k
33Greater than 90% (list of references: Park S E; Shrout T R.Ultrahigh strain and piezoelectricbehavior in relaxor based ferroelectric single crystals.J Appl Phys; 1997,82 (4): 1804-1811.).But with regard to current technology; Like top seed crystal solution growth (TSSG) method etc., still exist aspect preparation high-quality, the large-sized monocrystalline piezoelectric pottery rate of crystalline growth slowly, crystalline component skewness, crystal structure defects control difficulty cause material property fluctuation and preparation cost to cross high a series of problem.
At present, the texturing preparation method of KNN pottery mainly contains template grain growth (TGG) method and reaction template grain growth (RTGG) method, floating region (FZ) growth method and electric field, induced by magnetic field method etc.2004, the Satio of Academia Sinica of Japanese Toyota etc.
[11]Adopt Bi
2.5Na
3.5Nb
5O
18Flaky crystalline grain is that feedstock production obtains the NN flaky crystalline grain as template, is aided with NN, KN, KTaO again
3, LS crystal grain mixes, it is ceramic to make the higher LF4T of the degree of orientation through curtain coating lamination and sintering, d
33Reached 416pC/N, made the research of leadless piezoelectric ceramics obtain important breakthrough, this also is the best report (list of references: Saito Y of piezoelectric property up to now; Takao H, Tani T, et al.Lead-free piezoceramics.Nature; 2004,432 (4): 84-87.).This report has started the upsurge of the ceramic leadless piezoelectric material material of research KNN base; It is " dawn that occurs in the very long dark " (list of references: Cross E.Lead-free at last.Nature that doctor Cross writes articles this event description on Nature specially; 2004,432 (4): 24-25.).Prepare the piezoelectric property that textured piezoelectric ceramic can improve pottery significantly though generally believe template grain growth at present; But this method still exists many difficult problems to be solved fully as yet, mainly contains: (1) lets an amount of template be arranged in the sample comparatively difficult uniformly and equidistantly by specific direction; (2) be difficult to make the unified degree of orientation and the even distribution situation of template in base substrate precisely controlled; (3) be difficult to control the slewing growth of matrix granule on template; (4) introducing of the young crystal grain of a large amount of templates; The particularly introducing of heterogeneous template will form big crystal grain composite diphase material, can produce the mismatch of lattice, elastic performance and hot property; Thereby cause piezoelectric property descend (list of references: Sui Wanmei. the preparation method of polycrystal texture ceramic material. China; Patent of invention, publication number: CN1850725A, 2006.10.25.).
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of potassium-sodium niobate textured ceramic and potassium-sodium niobate monocrystalline.This method is an amount of oxide or the composite oxides that mix bismuth-containing (Bi) element in KNN base pottery, adopt traditional ceramic preparation technology, just can under normal condition, prepare the KNN base pottery and the monocrystalline of preferred orientation.
The preparation method of a kind of potassium-sodium niobate textured ceramic of the present invention comprises the steps:
(1) batching: at K
0.5Na
0.5NbO
3The middle LiBiO that adds
3, can use general formula (1-x) (K
0.5Na
0.5) NbO
3-xLiBiO
3Represent that x representes molar content in the ceramic systems in the formula, wherein 0.003≤x≤0.005; Or at K
0.5Na
0.5NbO
3The middle BiNiO that adds
3, with general formula (1-x) (K
0.5Na
0.5) NbO
3-xBiNiO
3Represent that x representes molar content in the ceramic systems in the formula, wherein 0.005≤x≤0.07;
(2) preparation technology with traditional ceramics prepares; Comprise wet-milling, dry, burn till, secondary ball milling, granulation, compression moulding, sintering; Different with prior art is: be medium wet-milling 12 hours with the absolute ethyl alcohol, the oven dry back is at 6 hours in advance synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, and the adding additives granulation of oven dry back is shaped to φ 18 * 2mm in the pressure pressed of 110MPa
2The biscuit sample.The biscuit sample is placed horizontally in the high-temperature electric resistance furnace; Programming rate with 120 ℃/h when sintering is warmed up to 500 ℃ of insulation 2h; Programming rate with 120 ℃/h was warmed up to 1080～1130 ℃ of heat preservation sinterings 2 to 24 hours again; Behind the sintering, cool to room temperature with the furnace, promptly make KNN base pottery with good preferred orientation.
The preparation method of a kind of potassium-sodium niobate monocrystalline of the present invention comprises batching, wet-milling, dries, burns till, secondary ball milling, granulation, compression moulding, sintering, it is characterized in that:
(1) batching: at K
0.5Na
0.5NbO
3The middle LiBiO that adds
3, can use general formula (1-x) (K
0.5Na
0.5) NbO
3-xLiBiO
3Represent that x representes molar content in the ceramic systems in the formula, wherein 0.003≤x≤0.005;
(2) with the absolute ethyl alcohol be medium wet-milling 12 hours, the oven dry back is at 6 hours in advance synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, and the adding additives granulation of oven dry back is shaped to φ 18 * 2mm in the pressure pressed of 110MPa
2The biscuit sample; The biscuit sample is placed horizontally in the high-temperature electric resistance furnace; Programming rate with 120 ℃/h when sintering is warmed up to 500 ℃ of insulation 2h, and the programming rate with 120 ℃/h was warmed up to 1115-1125 ℃ of heat preservation sintering 12 to 24 hours again, behind the sintering; Cool to room temperature with the furnace, can obtain size and reach the above monocrystalline of 2mm.
Advantage of the present invention is: adopt traditional ceramic preparation technology, prepare the KNN pottery with good preferred orientation in normal condition, reach the above monocrystalline of 2mm if control sintering temperature and time can also obtain size.
Description of drawings
The natural surface SEM photo of the sample of preparation among Fig. 1 embodiment 1;
The XRD figure of the cross section of the sample of preparation spectrum among Fig. 2 embodiment 1;
The monocrystalline SEM photo of preparation among Fig. 3 embodiment 2;
The XRD figure of the cross section of the sample of preparation spectrum among Fig. 4 embodiment 4.
Embodiment
Embodiment 1:
With Na
2CO
3, K
2CO
3, Nb
2O
5, Li
2CO
3And Bi
2O
3Be raw material, according to chemical formula:
0.996(K
0.5Na
0.5)NbO
3-0.004LiBiO
3
Preparing burden, is medium wet-milling 12 hours with the absolute ethyl alcohol, and the oven dry back is at 6 hours in advance synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, and the adding additives granulation of oven dry back is shaped to φ 18 * 2mm in the pressure pressed of 110MPa
2The biscuit sample.
The biscuit sample is placed horizontally in the high-temperature electric resistance furnace,, obtained the sintered body pottery in 3 hours at 1125 ℃ of sintering at last at 2 hours binder removals of 500 ℃ of insulations.Microstructure analysis shows that pottery has tangible oriented growth characteristic, and crystalline form is complete, and texture is clear.The XRD figure spectrum that is respectively the natural surface SEM photo and the cross section of the sample of preparation among the embodiment 1 illustrated in figures 1 and 2.
Embodiment 2:
With Na
2CO
3, K
2CO
3, Nb
2O
5, Li
2CO
3And Bi
2O
3Be raw material, according to chemical formula:
0.996(K
0.5Na
0.5)NbO
3-0.005LiBiO
3
Preparing burden, is medium wet-milling 12 hours with the absolute ethyl alcohol, and the oven dry back is at 6 hours in advance synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, and the adding additives granulation of oven dry back is shaped to φ 18 * 2mm in the pressure pressed of 110MPa
2The biscuit sample.
The biscuit sample is placed horizontally in the high-temperature electric resistance furnace, at 2 hours binder removals of 500 ℃ of insulations, obtains the sintered body pottery in 12 hours at 1125 ℃ of sintering at last.Microstructure analysis shows, grows bigger single crystal grain in the pottery, the about 2mm of size.Shown in Figure 3 is the monocrystalline SEM photo of preparation among the embodiment 2.
Embodiment 3:
With Na
2CO
3, K
2CO
3, Nb
2O
5, Li
2CO
3And Bi
2O
3Be raw material, according to chemical formula:
0.996(K
0.5Na
0.5)NbO
3-0.005LiBiO
3
Preparing burden, is medium wet-milling 12 hours with the absolute ethyl alcohol, and the oven dry back is at 6 hours in advance synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, and the adding additives granulation of oven dry back is shaped to φ 18 * 2mm in the pressure pressed of 110MPa
2The biscuit sample.
The biscuit sample is placed horizontally in the high-temperature electric resistance furnace, at 2 hours binder removals of 500 ℃ of insulations, obtains the sintered body pottery in 10 hours at 1115 ℃ of sintering at last.Microstructure analysis shows that pottery has oriented growth characteristic significantly, and ceramic dense, the about 1-2mm of single crystal grain size.
Embodiment 4:
With Na
2CO
3, K
2CO
3, Nb
2O
5, NiO and Bi
2O
3Be raw material, according to chemical formula: 0.994 (K
0.5Na
0.5) NbO
3-0.006BiNiO
3
Preparing burden, is medium wet-milling 12 hours with the absolute ethyl alcohol, and the oven dry back is at 6 hours in advance synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, and the adding additives granulation of oven dry back is shaped to φ 18 * 2mm in the pressure pressed of 110MPa
2The biscuit sample.
The biscuit sample is placed horizontally in the high-temperature electric resistance furnace, at 3 hours binder removals of 600 ℃ of insulations, obtains the sintered body pottery in 2 hours at 1090 ℃ of sintering at last.Microstructure analysis shows that pottery has oriented growth characteristic significantly, and ceramic dense, the about 1mm of single crystal grain size.Shown in Figure 4 is the XRD figure spectrum of the cross section of the sample of preparation among the embodiment 4.
Claims (2)
1. the preparation method of a potassium-sodium niobate textured ceramic comprises batching, wet-milling, dries, burns till, secondary ball milling, granulation, compression moulding, sintering, it is characterized in that:
(1) batching: at K
0.5Na
0.5NbO
3The middle LiBiO that adds
3, can use general formula (1-x) (K
0.5Na
0.5) NbO
3-xLiBiO
3Represent that x representes molar content in the ceramic systems in the formula, wherein 0.003≤x≤0.005; Or at K
0.5Na
0.5NbO
3The middle BiNiO that adds
3, with general formula (1-x) (K
0.5Na
0.5) NbO
3-xBiNiO
3Represent that x representes molar content in the ceramic systems in the formula, wherein 0.005≤x≤0.07;
(2) with the absolute ethyl alcohol be medium wet-milling 12 hours, the oven dry back is at 6 hours in advance synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, and the adding additives granulation of oven dry back is shaped to φ 18 * 2mm in the pressure pressed of 110MPa
2The biscuit sample; The biscuit sample is placed horizontally in the high-temperature electric resistance furnace; Programming rate with 120 ℃/h when sintering is warmed up to 500 ℃ of insulation 2h, and the programming rate with 120 ℃/h was warmed up to 1080～1130 ℃ of heat preservation sinterings 2 to 24 hours again, behind the sintering; Cool to room temperature with the furnace, promptly make KNN base pottery.
2. the preparation method of a potassium-sodium niobate monocrystalline comprises batching, wet-milling, dries, burns till, secondary ball milling, granulation, compression moulding, sintering, it is characterized in that:
(1) batching: at K
0.5Na
0.5NbO
3The middle LiBiO that adds
3, can use general formula (1-x) (K
0.5Na
0.5) NbO
3-xLiBiO
3Represent that x representes molar content in the ceramic systems in the formula, wherein 0.003≤x≤0.005;
(2) with the absolute ethyl alcohol be medium wet-milling 12 hours, the oven dry back is at 6 hours in advance synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, and the adding additives granulation of oven dry back is shaped to φ 18 * 2mm in the pressure pressed of 110MPa
2The biscuit sample; The biscuit sample is placed horizontally in the high-temperature electric resistance furnace; Programming rate with 120 ℃/h when sintering is warmed up to 500 ℃ of insulation 2h, and the programming rate with 120 ℃/h was warmed up to 1115-1125 ℃ of heat preservation sintering 12 to 24 hours again, behind the sintering; Cool to room temperature with the furnace, can obtain size and reach the above monocrystalline of 2mm.
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| CN101913868B true CN101913868B (en) | 2012-09-26 |
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|---|---|---|---|---|
| DK2726438T3 (en) | 2011-07-01 | 2018-09-03 | Ceram Gmbh | Process for preparing a piezoceramic lead-free material |
| CN103601493B (en) * | 2013-10-15 | 2015-09-30 | 陕西科技大学 | A kind of KNN-LS leadless piezoelectric ceramics and preparation method thereof |
| CN103613383A (en) * | 2013-11-14 | 2014-03-05 | 常州大学 | Preparation method of Er<3+> and Yb<3+> co-doped LiBiO3 modified KNN-based transparent up-conversion ceramic |
| CN105271409A (en) * | 2014-07-25 | 2016-01-27 | 同济大学 | Preparation method of sheet shaped potassium-sodium niobate powder |
| CN106270523B (en) * | 2016-09-30 | 2018-02-13 | 中国人民大学 | A kind of large-area ultrathin monocrystalline and its method for fast growing and application |
| CN106087058A (en) * | 2016-06-22 | 2016-11-09 | 桂林电子科技大学 | A kind of K0.5na0.5nbO3base ferroelectric piezoelectric single crystal and preparation method thereof |
| CN106521627B (en) * | 2016-11-10 | 2019-01-08 | 桂林电子科技大学 | A kind of potassium-sodium niobate-based piezoelectric monocrystal and preparation method thereof |
| CN106757302B (en) * | 2016-11-24 | 2019-03-15 | 桂林电子科技大学 | A kind of potassium-sodium niobate monocrystalline and preparation method thereof |
| CN107032784A (en) * | 2017-05-02 | 2017-08-11 | 桂林电子科技大学 | A kind of big Piezoelectric Anisotropy lead-free piezoceramic material and preparation method thereof |
| CN107445618A (en) * | 2017-07-26 | 2017-12-08 | 江苏大学 | A kind of microwave dielectric material and preparation method thereof |
| CN109402737B (en) * | 2018-03-05 | 2021-02-19 | 苏州科技大学 | Method for preparing lead zirconate titanate single crystal at low temperature |
| CN109208066B (en) * | 2018-03-05 | 2021-03-12 | 苏州科技大学 | Single crystal preparation method of ferroelectric ceramic compound |
| CN109553413B (en) * | 2019-01-17 | 2021-07-16 | 南方科技大学 | Textured piezoelectric ceramic and preparation method and application thereof |
| CN115784741B (en) * | 2022-10-20 | 2024-02-02 | 济南大学 | Potassium sodium niobate-based dielectric ceramic material with ultra-wide temperature stability and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644562A (en) * | 2004-07-15 | 2005-07-27 | 清华大学 | Lead free piezoelectric ceramics of potassium sodium niobate and preparation thereof |
| CN1937274A (en) * | 2005-09-23 | 2007-03-28 | 清华大学 | Ferroelectric domain array structure, and its preparing method and ferroelectric film having same |
| CN101621112A (en) * | 2008-06-30 | 2010-01-06 | 日立金属株式会社 | Ceramic sintered compact and piezoelectric element |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644562A (en) * | 2004-07-15 | 2005-07-27 | 清华大学 | Lead free piezoelectric ceramics of potassium sodium niobate and preparation thereof |
| CN1937274A (en) * | 2005-09-23 | 2007-03-28 | 清华大学 | Ferroelectric domain array structure, and its preparing method and ferroelectric film having same |
| CN101621112A (en) * | 2008-06-30 | 2010-01-06 | 日立金属株式会社 | Ceramic sintered compact and piezoelectric element |
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