CN100497257C - Method for preparing polycrystal texture ceramic material - Google Patents
Method for preparing polycrystal texture ceramic material Download PDFInfo
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- CN100497257C CN100497257C CNB2006100442286A CN200610044228A CN100497257C CN 100497257 C CN100497257 C CN 100497257C CN B2006100442286 A CNB2006100442286 A CN B2006100442286A CN 200610044228 A CN200610044228 A CN 200610044228A CN 100497257 C CN100497257 C CN 100497257C
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Abstract
This invention relates to polycrystal texture ceramic material preparation method, it includes preparation technique principle and corresponding technique method. Diffusion route of ion and polar particle in high temperature field can be affected by electrostatic field, the characteristic is used to induct crystal nucleus growth process and reinforce anisotropy growth to form texture polycrystal material. Different strength orientation electric field is applied, and the strength is related to material system different component, core forming and crystal growth speed, anisotropy radius-thickness ratio expected, and electric breakdown strength of environment and materials. The anisotropy growth of polusrystal texture made is appreciable, polyspinal deformity is uniform, breaking tenacity and fracture toughness of material on wishful direction can be improved. Directed dielectric property can be great improved, and material piezoelectric constant and electromechanical conpling factor can be improved, dielectric loss can be reduced.
Description
Technical field:
The invention belongs to material science, relate to and a kind ofly prepare the processing method of polycrystal texture ceramic material, be called electric field and intervene method polycrystal texture ceramic material preparation method with the auxiliary principle of electrical forces effect.
Technical background:
In the ceramic material Technology, all to relate to the raw material dispersion mostly and mix moulding, main technique steps such as sintering.Wherein, sintering is to allow porous forming of green body body form set chemical composition and wish microstructural most critical technological step.In this process, mainly rely on the sintering process motivating force that high temperature provides a kind of material densification and forms set microstructure.High temperature source can be fuel heat, electric power energy, micro-wave energy etc.For the carrying out that promote correlated response and the acceleration of densification process, also relate to some other ancillary technique measure, mainly contain exert pressure, chemical additive, measures such as ambiance, different householder methods has different technique influences to the structure of stupalith with performance.
In the function ceramics field, ferroelectric material can be divided into ferroelectric single crystal and ferroelectric polycrystalline ceramics two big classes.Ferroelectric single crystal material is not owing to be subjected to the influence of grain size, grain orientation, crystal boundary and void content, thereby has the performance more excellent more than ferroelectric polycrystalline ceramic.In recent years, the research of relaxation sections electricity single crystal and relaxation sections electroceramics is respectively the focus that people pay close attention to, and finds that the relaxation ferroelectric ceramic(s) has good piezoelectricity, dielectric properties [Science Bulletin, 1999,44 (20): 2157 near accurate homotype phase boundary; Journal of Inorganic Materials, 2000,15 (1) 109; Journal of Inorganic Materials, 2002,17 (3) 387].But the two is compared, and monocrystal material tends to show excellent more performance.Exceeded an order of magnitude as the PMN-PT of developments such as Thomas Shront in 1997 and the piezoelectric constant of PZN-PT ferro-electricity single crystal than ferroelectric ceramic(s).At present, the piezoelectric constant of relaxation ferroelectric single crystal and piezoelectric coupling coefficient are one of performance is the highest in the existing piezoelectric material [J.Appl.Phys., 1997,82 (4): 1804].But the problem that exists is, though this processing method has improved material property, still used environmentally harmful lead element, belongs to the non-ambient coordinating material, do not meet environmental requirement.
The ceramic science theory is pointed out, polycrystalline ceramics and the difference of monocrystalline crystalline microstructure mainly are to exist in the ceramic body crystal grain and crystal boundary, and crystal grain is that random orientation is arranged, thereby makes the performances such as dielectric, piezoelectricity and optics of polycrystalline ceramics compare greatly inferior with single crystal.As the piezo-electric modulus of the back polycrystalline piezoelectric ceramics that polarizes is far away from corresponding single crystal.But in the process of producing high quality large size single crystal body, run at present crystalline growth velocity slowly, crystalline component skewness and crystal structure defects control difficulty cause a series of problems such as material property fluctuation and preparation cost height.Though and the polycrystalline ferroelectric ceramic material have preparation technology comparatively simple, be easy to advantage such as controlling quality, but at present a large amount of use and better performances material remain based on lead-containing materials, the performance that piezoelectricity, ferroelectric ceramic material are coordinated in the non-lead ring border of developing still is difficult to compare with traditional lead-containing materials at present.
Thereby, the focus of attention that becomes the investigator in conjunction with the material preparation process advantage and the material structure performance characteristics of monocrystalline and polycrystalline material how.An impressive progress that wherein obtains is taked proper process measures exactly in ceramic preparation process, change the state of grain orientation random alignment in the polycrystalline ceramic, allow in the pottery grain orientation growth and arrange by same direction, both can improve the strength and toughness on the structural ceramic material specific orientation, also can improve the polarization efficiency and the dielectric properties of ferroelectric function ceramics greatly.Here it is so-called texture ceramic material.
In recent years, exploitation microstructure and material property become a kind of important techniques method between the texture ferroelectric ceramic material between the two.Especially because ferroelectric, the piezoelectric property of functional materials is closely related with the orientation of crystal, crystal grain, make consistent orientation of crystal grain height of pottery by effective texturing technology, can increase substantially ceramic ferroelectric, piezoelectric property.At present, the highest 60-80%[J.Am.Ceram.Society that can reach monocrystal material of the piezo-electric modulus of textured ceramic, 2001,82 (11): 2507], material property is brought up near the monocrystalline level, and its preparation technology also has general ceramic material time weak point, low cost and other advantages.
Control grain orientation growth and aligning in material preparation process is the key problem in technology of the height-oriented textured ceramic of preparation.At present, the main preparation methods of texture ferroelectric ceramic(s) has, and uses TGG (the Templated Grain Growth) Process [103 of growing single-crystal
RdAm.Ceram.Socie.Annual Meeting, April 22-25,2001], and RTGG (ReactiveTemplated Grain Growth) Process.The difference of two kinds of technologies is to react between the raw material in the heat treatment process of RTGG and generates the product crystalline phase, and is arranged in oriented growth on the seed crystal face, has promptly finished two steps of building-up reactions and grain orientation growth simultaneously, forms textured ceramic.And the TGG rule is that template is aligned in the thin brilliant base substrate identical with the product crystalline phase, allows base substrate close grain oriented growth on seed crystal face, forms textured ceramic.Template is young brilliant to align main curtain coating or the extruding forming method of having adopted in molding biscuit.Other also has heat to forge and contains technology [Ferroelectrics, 2000,24:43 such as lamination liquid phase sintering after the moulding of seed crystal slip casting method, hot pressed sintering; 14].Its fundamental principle also is to create a kind of environment that helps crystal grain along a certain direction preferential growth, and crystal grain can be aligned.It also is a kind of feasible method that the control crystal grain orienting is arranged that (eutectic solidification) technology is solidified in eutectic.
Though think that at present it is one of main technique methods of improving significantly the ferroelectric ceramic(s) performance that template prepares ferroelectric textured ceramic.But the many difficult problems in its fabricating technology are solved as yet fully.The subject matter that exists has: 1) the young brilliant size of the template of current use is bigger, allows an amount of template be arranged in the sample base substrate comparatively difficult uniformly and equidistantly by specific direction.2) in forming method, main at present curtain coating lay-up method, extrusion moulding and the uniaxial pressure method of forming etc. of adopting.These methods all make the sheet seed crystal be orientated on certain orientation with the orientation force that macroscopical moulding process forms.Obviously, it is all precisely controlled that such forming method is difficult to make unified orientation degree and the uniform distribution situation of template in base substrate.3) how to control the slewing growth of matrix granule on template on request.As regulate and control matrix granule granularity and distribution situation, with the accumulation situation etc. that contacts of seed crystal, main at present employing improves measure solutions such as biscuit density.
Simultaneously, aspect the dependency of the microstructure-performance of textured ceramic, lack systematic study.As in template technology, increase with young crystal template add-on usually, the orientation degree that crystal grain orienting is arranged improves.But a large amount of introducings of the introducing, particularly heterogeneous template of the young crystalline substance of a large amount of templates will form big crystal grain composite diphase material structure, thereby can cause decline ferroelectric, piezoelectric property; Simultaneously, the existence of a large amount of heterogeneous laths can produce the mismatch of elastic performance and thermal characteristics and causes problems such as mechanical fatigue destruction.In addition, the general directed grain-size of the textured ceramic of template prepared can reach ten several microns～size more than 50 microns, and this belongs to the super large grain-size in the ceramic structure theory, be unfavorable for the raising of mechanics and dielectric properties.As according to BaTiO
3Specific inductivity and particle diameter relation under the pottery room temperature, specific inductivity maximum when its median size is one micron left and right sides [day disclosure special permission communique, the spy opens 2000-154054] usually should be several microns sizes.
From the traditional ceramics sintering theory, know, the formation and the grain growth of the generation of chemical reaction, the forming core of poly grains, cell configuration, its motivating force is mainly derived from heat energy and drives particle and move and finish, and can also apply outer mechanical pressure such as technical measures such as atmosphere pressures, hot axial pressing and hot isostatic pressing simultaneously.Other means that have been applied to the high temperature densification also have the microwave in the microwave sintering method to turn to drive etc., and utilize the dispatch from foreign news agency field force to influence the sintering of polycrystalline ceramic and the know-why and the processing method of grain orientation growth process still do not have relevant report.
Can think that ferroelectric ceramic(s) texturing technology is the effective technical way that comprehensively solves the ferroelectric single crystal material performance.Especially functional materials ferroelectric, piezoelectric property is relevant with the close state of the orientations of crystal, crystal grain, makes the grain orientation growth and highly consistent orientation of pottery by texturing technology, can increase substantially ceramic ferroelectric, piezoelectric property.But realize the breakthrough of the particularly ferroelectric ceramic material performance of texture ceramic material, need seek the practice of new know-why support and technological method, control from the mesoscopic structure of material, the assembling of crystal grain and the evolution growth course of crystalline form, and then reach the purpose of regulation and control polarization performance and original domain structure, finally form the ferroelectric ceramic material of the class single crystal structure that grain-size is tiny evenly, degree of grain alignment is big.The present invention is exactly about the electrical forces effect being introduced the formation of textured ceramic preparation technology with the growth and development process and the material orientation texture tissue of effective regulation and control polycrystalline ceramics crystal grain, be called electric field by the technological principle feature and intervene method technology, technology of the present invention can combine the strong technique means that forms the preparation texture ceramic material with other processing methodes such as template, doctor-blade casting processes.
Summary of the invention:
The present invention is intended to overcome the shortcoming that exists in the prior art, seeks to design a kind of ultimate principle and processing method for preparing texture ceramic material, develops a kind of textured ceramic based on external electric field stress effect regulation and control grain orientation growth and prepares new principle and novel process.Particularly relate to the performances such as polarizability, dielectric coefficient and piezoelectric constant that improve or effectively regulate and control ferroelectric texture ceramic material greatly, and then can improve the performance and the efficient of functional devices such as piezoelectricity, pyroelectricity, electric light greatly.
Technical characterictic main points of the present invention are in inorganic materials high temperature preparation process, press the crystalline structure of crystal grain and the difference of nucleus growth habit, sintered compact is applied simultaneously the electrical forces of proper orientation, the electrostatic potential that provides with extra electric field is as the supplementary means of regulation and control crystal grain anisotropic growth, adopt field-effect to intervene anisotropic growth rates at the crystal grain assembling process, induce, strengthen and control the anisotropy oriented growth of crystal grain, the final polycrystal texture ceramic material that forms with certain texture characteristic, propose original electricdomain notion and electrical forces and regulate and control the technological thought of original domain structure and orientation, with the technological approaches of the electrical texture ceramic material of expansion preparation high pressure.
The present invention proposes following technological thought: the high temperature base substrate is applied electrical forces, utilize the high penetrating power of electrostatic field and the energy of position that has, form many kinetics, thermodynamic driving force, strengthen and quicken the anisotropic growth speed of crystal grain, regulate and control initial domain structure ferroelectric, piezoceramic material, be beneficial to form the regulatable texture ceramic material of the height-oriented and original electricdomain of crystal grain.
Apply field force and realize the preparation of anisotropy fine ceramics texture, mainly consider polycrystalline ceramic in nucleation and nuclei growth process, the motion particle mostly is charged particle greatly, and it moves, assembling process is subjected to the influence that electromotive force drives energy.Electrical effect in the sintered compact can be regulated and control synthesizing and process of growth of stupalith at least aspect three.The one, influence the movement path of ion or charged group; The 2nd, cause the poly-partially of localized particle; The 3rd, the activation energy of change crystal grain nucleation and growth process.Particularly, the sintered compact that is in the high temperature densification process is applied electrical forces, regulating and controlling effect will take place to the formation of the initial electricdomain of ferroelectric ceramic material and the orientation of electricdomain, suitably that the forming core, growth orientation etc. of electricdomain will be suffered restraints will be regular for the electrical effect of orientation, even reach the poling effect.We know that the high voltage polarization of piezoelectric is the indispensable step of piezoelectric ceramics, but the high voltage polarization of material preparation after finishing belongs to physical process, and domain wall motion suffers restraints, and are difficult to realize that the high orientation of electricdomain arranges.The present invention proposes a material after-polarization process and moves to the high temperature preparatory phase, follows the growing up course of crystal grain and carries out simultaneously.Improve the degree of orientation even the poling on original farmland, finish sintering densification process after-polarization problem of difficult to solve some ferroelectric ceramic material.
For achieving the above object, the present invention proposes electric field to intervene the craft technical feature of method as follows:
Choose ceramic earlier, add weight percent and be 0～10% sintering aid or young crystalline flour end, add weight percent again and be the crystalline template thing of sheet that 0～15% molten-salt growth method is made, mixing aftershaping is the base substrate sample; Put into the high-temperature electric resistance furnace workspace after the base substrate samples dried, settle high temperature electrode along the sample peripheral direction; In base substrate sample sintering process, apply electric field, get product after finishing to sintering.
Pending biscuit of ceramics body is placed the high-temperature zone, arrange electrode around base substrate, each all is the point symmetry center arrangement with the sample to positive-negative electrode plate.Apply the difference of the arrangement of electrodes orientation of electric field according to the ceramic sintered bodies crystal formation, can be respectively same horizontal distribution single electrode in opposite directions to, two electrodes to or three electrode pairs; Be in conplane each to positive and negative electrode all around the sintered compact single electrode to arranging by 180 degree in opposite directions.Two electrodes to the time arrange by intersecting 90 degree, arrange by adjacent friendship 60 degree of each counter electrode during three electrode pairs.
Apply electric field according to ceramic sintered bodies crystal formation and molding biscuit shape difference, by with the vertical direction of plane electrode, settling pair of electrodes to control the crystalline growth velocity on this direction on the sintered compact; The time that applies electric field can carry out with interruption or successive mode stage by stage, time period comprises from the high temperature sintering body and tangible solid phase, solid-liquid occur mutually and the liquid liquid phase reaction, perhaps significantly migration appears in the particle particle in the high temperature sintering body, perhaps occurs nucleus forming core and grain growth phenomenon in the high temperature sintering body and begins till above-mentioned dynamic process stops; The electric field that applies can be respectively a DC electric field according to the difference of expectation electrical effect, or alternating-electric field, or DC electric field and alternating-electric field alternately apply and carry out.
The crystal formation of arranging the quantity of electrode pair how much to depend on to prepare material and the material grains texture characteristics of expectation.High symmetry crystal formation material can adopt single electrode to or the plane two electrodes to structural arrangement; The low-symmetry crystal formation adopt two electrodes to or three electrode pair structural arrangement; When forming lengthy motion picture crystalline substance texture, expectation adopt single electrode to structural arrangement; When forming common platelet texture, expectation adopt plane two electrodes or plane three-electrode structure to arrange; Expectation can increase the electrode pair of vertical orientations and arrange when further controlling third dimension grain growing speed.
Apply among the present invention electric field the electromotive force size can from 0.1KV/mm until the sintering high temperature environment and the material bodies not disruption potential that can bear itself be 5000V/mm.
The present invention combines with template technology, and the formed body that will contain homogeneity or heterogeneous template places the electric field system of this invention proposition to carry out the high temperature electric field treatment, with the formation of cooperative reinforcing texture structure; Combine with doctor-blade casting process technology, extrusion molding moulding process, lamination compression moulding technology etc., with directed pre-arrangement of particle or template crystal grain in the reinforcement biscuit; The polycrystalline ceramic that the preparation that combines with flux method has fine directed crystal grain texture.Among the preparation technology of the diphase ceramic material that can be widely used in structural ceramic materials such as aluminum oxide, mullite, zirconium white, silicon nitride, silicon carbide, match dragon and form between them; Also can be applicable among the preparation technology of ceramic materials such as ferroelectric, piezoelectricity, electric light.
The present invention compares with art methods that to have principle reliable, and technology is easy, and condition is controlled strong, and the quality of materials of preparation is reliable, stable performance.
Embodiment:
Embodiment 1: aluminum oxide texture ceramic material electrical effect aid preparation technology.
Choose median size and be light-burned γ-alumina powder of 1～10 micron, the silicon oxide such as mole such as grade, the magnesium oxide eutectic mixture powder that add 2wt%, add the crystalline α-alumina powder of sheet that the molten-salt growth method of 3wt% is made again, wet-mixed was dried after 4 hours in ball milling, and utilizing the bidirection press method of forming is the biscuit sample of 10 * 10 * 4mm at the 100Mpa forming under the pressure.
The base substrate sample puts it into the hot operation district horizontal positioned of high-temperature electric resistance furnace after 120 ℃ of following dryings, arrange a pair of high temperature electrode in the sample both sides along sample rectangular edges length direction.In the sample sintering temperature-rise period, temperature begins to utilize electrode to apply the DC electric field of 400V/mm to sample when reaching 800 ℃, until 1550 ℃ down 6 hours sintering processes of insulation finish.The microstructure analysis of the final sample that obtains shows, grain growing along direction of an electric field has significant oriented growth feature, the slenderness ratio of its crystal grain and intensity, toughness properties improve 20%～200% than the sample under the same preparation process condition that does not apply electric field.
Embodiment 2: barium titanate texture ceramic material electrical effect aid preparation technology.
Choose median size and be 1～10 micron barium titanate micro mist, add the crystalline strontium titanate micro mist of sheet that the molten-salt growth method of 4wt% is made again, wet-mixed was dried after 4 hours in ball milling, utilize the extrusion molding moulding, along extruding direction is sheet sample length and width directions, and processing cuts the biscuit sample that is of a size of 15 * 15 * 5mm.
The base substrate sample puts it into the hot operation district horizontal positioned of high-temperature electric resistance furnace after 120 ℃ of following dryings, respectively arrange a pair of high temperature electrode in the sample side direction along the parallel edges length direction, and two electrodes is to arranging by intersecting 90 degree.In the sample sintering temperature-rise period, temperature begins to utilize electrode to apply the DC electric field of 800V/mm to sample when reaching 600 ℃, until 1360 ℃ down 4 hours sintering processes of insulation finish.The microstructure analysis of the final sample that obtains shows, has significant oriented growth feature along the grain growing of direction of an electric field, and the slenderness ratio of its crystal grain and dielectric properties improve 30%～180% than the sample under the same preparation process condition that does not apply electric field.
Claims (2)
1. the preparation method of a polycrystal texture ceramic material, it is characterized in that choosing earlier ceramic, the adding weight percent is 0～10% sintering aid or young crystalline flour end, add weight percent again greater than 0 and be no more than the crystalline template thing of sheet that 15% molten-salt growth method is made, mixing aftershaping is the base substrate sample; Put into the high-temperature electric resistance furnace workspace after the base substrate samples dried, settle high temperature electrode along the sample peripheral direction; In base substrate sample sintering process, apply electric field, get product after finishing to sintering;
Wherein, base substrate places the high-temperature zone, arranges electrode around base substrate, and each all is the point symmetry center arrangement with the sample to positive-negative electrode plate; The arrangement of electrodes orientation that applies electric field be respectively same horizontal distribution single electrode in opposite directions to or two electrodes right, single electrode is to arranging by 180 degree in opposite directions, two electrodes to the time arrange by intersecting 90 degree; The electric field that applies is a DC electric field;
Wherein, the time that applies electric field carries out in a continuous manner, and the temperature that occurs tangible solid phase or solid-liquid phase reaction from the high temperature sintering body begins to stop until dynamic process.
2. the preparation method of polycrystal texture ceramic material according to claim 1 is characterized in that applying the electromotive force size of electric field from 0.1KV/mm to 5000V/mm.
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| JP5800408B2 (en) * | 2008-02-05 | 2015-10-28 | 株式会社村田製作所 | Multilayer ceramic capacitor |
| US20130240786A1 (en) * | 2010-12-02 | 2013-09-19 | Koninklijke Philips Electronics N.V. | Ceramic non-cubic fluoride material for lasers |
| CN104197714B (en) * | 2014-08-27 | 2015-12-09 | 中国石油大学(华东) | There is the piezoelectric ceramics sintering furnace of function of polarization and the method for sintering polarization thereof |
| CN104844195A (en) * | 2015-04-28 | 2015-08-19 | 苏州大学 | Method for preparing copper titanate bismuth sodium ceramic |
| CN107344386A (en) * | 2017-07-04 | 2017-11-14 | 陕西科技大学 | A kind of piezoelectric structured ceramic injection forming machine |
| CN107586136B (en) * | 2017-10-17 | 2020-10-23 | 广东工业大学 | 3D printing method of silicon nitride ceramic |
| CN110451990B (en) * | 2019-09-06 | 2022-06-28 | 西北工业大学 | Method for preparing metal oxide textured ceramic material by rapid sintering at normal temperature |
| CN111960820B (en) * | 2020-07-31 | 2022-07-26 | 东莞东阳光科研发有限公司 | Piezoelectric crystal material and preparation method thereof |
| CN113501710A (en) * | 2021-06-25 | 2021-10-15 | 淮阴工学院 | Preparation method of sodium bismuth titanate textured ceramic |
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