CN101913868A - 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 PDF

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CN101913868A
CN101913868A CN2010102474748A CN201010247474A CN101913868A CN 101913868 A CN101913868 A CN 101913868A CN 2010102474748 A CN2010102474748 A CN 2010102474748A CN 201010247474 A CN201010247474 A CN 201010247474A CN 101913868 A CN101913868 A CN 101913868A
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江民红
邓满姣
刘心宇
陈国华
徐华蕊
刘超英
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Guilin University of Electronic Technology
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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

The preparation method of potassium-sodium niobate textured ceramic and potassium-sodium niobate monocrystalline
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 ferroelectrics and antiferroelectric 3-PbTiO 3(PZT) system solid solution is that the lead base piezoelectric ceramics of representative is widely used in fields such as transverter, driving mechanism resonator.Because at PZT is that deleterious plumbous oxide content surpasses more than 60% of raw material total mass in the pottery, has brought serious harm to environment for human survival, the unleaded of piezoelectric ceramics 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 specific inductivity 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 be subjected to the influence of grain size, grain orientation, crystal boundary and void content 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 order of 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% (reference: 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, as top seed crystal solution growth (TSSG) method etc., still exist aspect preparation high quality, the large-sized monocrystalline piezoelectric pottery crystalline growth velocity 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 growing (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, and makes the higher LF4T pottery of orientation degree, d through curtain coating lamination and sintering 33Reached 416pC/N, made the research of leadless piezoelectric ceramics obtain important breakthrough, this also is the best report (reference: 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 " (reference: 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) allows an amount of template be arranged in the sample comparatively difficult uniformly and equidistantly by specific direction; (2) be difficult to make unified orientation degree and the uniform 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, to form big crystal grain composite diphase material, can produce the mismatch of lattice, elastic performance and thermal characteristics, thereby cause piezoelectric property descend (reference: 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 compound or the composite oxides that mix bismuth-containing (Bi) element in KNN base pottery, adopt traditional ceramic preparation technology, just can prepare the KNN base pottery and the monocrystalline of preferred orientation under normal condition.
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 represents 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 represents molar content in the ceramic systems in the formula, wherein 0.005≤x≤0.07;
(2) preparation technology with traditional ceramics is prepared, comprise wet-milling, dry, burn till, secondary ball milling, granulation, compression moulding, sintering, unlike the prior art be: be medium wet-milling 12 hours with the dehydrated alcohol, oven dry back is at 6 hours pre-synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, the adding additives granulation of oven dry back, and compression moulding is φ 18 * 2mm under the pressure of 110MPa 2The biscuit sample.The biscuit sample is placed horizontally in the high-temperature electric resistance furnace, heat-up rate with 120 ℃/h when sintering is warmed up to 500 ℃ of insulation 2h, heat-up 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 represents molar content in the ceramic systems in the formula, wherein 0.003≤x≤0.005;
(2) with the dehydrated alcohol be medium wet-milling 12 hours, the oven dry back is at 6 hours pre-synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, the adding additives granulation of oven dry back, and compression moulding is φ 18 * 2mm under the pressure of 110MPa 2The biscuit sample, the biscuit sample is placed horizontally in the high-temperature electric resistance furnace, heat-up rate with 120 ℃/h when sintering is warmed up to 500 ℃ of insulation 2h, heat-up 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 dehydrated alcohol, and the oven dry back is at 6 hours pre-synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, the adding additives granulation of oven dry back, and compression moulding is φ 18 * 2mm under the pressure of 110MPa 2The biscuit sample.
The biscuit sample is placed horizontally in the high-temperature electric resistance furnace,, obtained the sintered compact 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 feature, 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 dehydrated alcohol, and the oven dry back is at 6 hours pre-synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, the adding additives granulation of oven dry back, and compression moulding is φ 18 * 2mm under the pressure 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 compact pottery in 12 hours at 1125 ℃ of sintering at last.Microstructure analysis shows, grows bigger single crystal particle in the pottery, the about 2mm of size.Figure 3 shows that 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 dehydrated alcohol, and the oven dry back is at 6 hours pre-synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, the adding additives granulation of oven dry back, and compression moulding is φ 18 * 2mm under the pressure 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 compact 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 particle 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 dehydrated alcohol, and the oven dry back is at 6 hours pre-synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, the adding additives granulation of oven dry back, and compression moulding is φ 18 * 2mm under the pressure 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 compact 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 particle size.Figure 4 shows that 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 represents 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 represents molar content in the ceramic systems in the formula, wherein 0.005≤x≤0.07;
(2) with the dehydrated alcohol be medium wet-milling 12 hours, the oven dry back is at 6 hours pre-synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, the adding additives granulation of oven dry back, and compression moulding is φ 18 * 2mm under the pressure of 110MPa 2The biscuit sample, the biscuit sample is placed horizontally in the high-temperature electric resistance furnace, heat-up rate with 120 ℃/h when sintering is warmed up to 500 ℃ of insulation 2h, heat-up 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 represents molar content in the ceramic systems in the formula, wherein 0.003≤x≤0.005;
(2) with the dehydrated alcohol be medium wet-milling 12 hours, the oven dry back is at 6 hours pre-synthetic porcelains of 880 ℃ of insulations; Porcelain is through secondary ball milling 6 hours, the adding additives granulation of oven dry back, and compression moulding is φ 18 * 2mm under the pressure of 110MPa 2The biscuit sample, the biscuit sample is placed horizontally in the high-temperature electric resistance furnace, heat-up rate with 120 ℃/h when sintering is warmed up to 500 ℃ of insulation 2h, heat-up 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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Cited By (14)

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WO2013004622A1 (en) * 2011-07-01 2013-01-10 Ceramtec Gmbh Piezoceramic lead-free material
CN103601493A (en) * 2013-10-15 2014-02-26 陕西科技大学 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
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
CN106521627A (en) * 2016-11-10 2017-03-22 桂林电子科技大学 Potassium-sodium niobate based piezoelectric single crystal and preparation method thereof
CN106757302A (en) * 2016-11-24 2017-05-31 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
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WO2018058872A1 (en) * 2016-09-30 2018-04-05 中国人民大学 Large-area ultrathin single crystal and rapid generation method therefor
CN109208066A (en) * 2018-03-05 2019-01-15 苏州科技大学 The method for preparing single crystal of ferroelectric ceramics class compound
CN109402737A (en) * 2018-03-05 2019-03-01 苏州科技大学 The method of low temperature preparation lead zirconate titanate monocrystalline
CN109553413A (en) * 2019-01-17 2019-04-02 南方科技大学 Textured piezoelectric ceramic and preparation method and application thereof
CN115784741A (en) * 2022-10-20 2023-03-14 济南大学 Potassium sodium niobate-based dielectric ceramic material with ultra-wide temperature stability and preparation method thereof

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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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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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WO2013004622A1 (en) * 2011-07-01 2013-01-10 Ceramtec Gmbh Piezoceramic lead-free material
US10008661B2 (en) 2011-07-01 2018-06-26 Ceramtec Gmbh Piezoceramic lead-free material
CN103601493A (en) * 2013-10-15 2014-02-26 陕西科技大学 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
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
WO2018058872A1 (en) * 2016-09-30 2018-04-05 中国人民大学 Large-area ultrathin single crystal and rapid generation method therefor
CN106521627A (en) * 2016-11-10 2017-03-22 桂林电子科技大学 Potassium-sodium niobate based 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
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CN106757302A (en) * 2016-11-24 2017-05-31 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
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CN109402737A (en) * 2018-03-05 2019-03-01 苏州科技大学 The method of low temperature preparation lead zirconate titanate monocrystalline
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
CN109553413A (en) * 2019-01-17 2019-04-02 南方科技大学 Textured piezoelectric ceramic and preparation method and application thereof
CN109553413B (en) * 2019-01-17 2021-07-16 南方科技大学 Textured piezoelectric ceramic and preparation method and application thereof
CN115784741A (en) * 2022-10-20 2023-03-14 济南大学 Potassium sodium niobate-based dielectric ceramic material with ultra-wide temperature stability and preparation method 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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