CN107098699A - The leadless piezoelectric structured ceramics and preparation method of width sintering warm area and wide composition regulation - Google Patents

The leadless piezoelectric structured ceramics and preparation method of width sintering warm area and wide composition regulation Download PDF

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CN107098699A
CN107098699A CN201710191985.4A CN201710191985A CN107098699A CN 107098699 A CN107098699 A CN 107098699A CN 201710191985 A CN201710191985 A CN 201710191985A CN 107098699 A CN107098699 A CN 107098699A
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wide
warm area
template
leadless piezoelectric
piezoelectric
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翟继卫
刘百慧
沈波
李朋
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Tongji University
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Abstract

The present invention relates to wide sintering warm area and the leadless piezoelectric structured ceramics and preparation method of wide composition regulation, its chemical analysis meets chemical general formula 0.99K0.49Na0.49Li0.02Nb0.97‑xSb0.03TaxO3‑0.01CaZrO3, wherein 0.15≤x≤0.25.Its preparation comprises the following steps:1) corresponding base-material and template are prepared；2) by template, dispensing is placed in ball grinder by a certain percentage with base-material, is added solvent back roller and is ground to obtain slurry；Stream of slurry is delayed into acquisition diaphragm；It is lamination after diaphragm is cut, hot-forming；The sample heat treatment pressed is taken out, the good leadless piezoelectric structured ceramic material of orientation is obtained.The leadless piezoelectric structured ceramic material degree of orientation that the preparation method is obtained is high, and sintering temperature is low, and sintering warm area is wide, and Curie temperature is high, piezoelectric constant d33It is all higher than 300pC/N and can stablizes in a wider compositional range, piezoelectric property is superior, is adapted to factory's large-scale production, in terms of can be widely used for piezoelectric transducer, piezoelectric motors and high precision position shift controller.

Description

The leadless piezoelectric structured ceramics and preparation method of width sintering warm area and wide composition regulation
Technical field
The invention belongs to leadless piezoelectric material material field, more particularly, to a kind of the unleaded of wide sintering warm area and width composition regulation Piezoelectric structured ceramics and preparation method.
Background technology
Piezoelectric is a kind of inorganic material, be it is a kind of realize the electronic information material that mechanical energy and electric energy are mutually changed, Play the role of in the function elements such as electricity, magnetic, power, heat very important.With the fast development of modern society, the preparation of material Technology, research method and means of testing have obtained significantly developing so that the performance of piezoelectric is greatly improved, and enters One step promotes development and application value of the function element in high-tech sector based on piezoelectric.Current lead base piezoelectricity Material, such as lead zirconate titanate (Pb (Ti, Zr) O3, PZT), turn into the material being most widely used with excellent piezoelectric property Material, but lead is easy to volatilization in high temperature environments, can cause serious environmental pollution, lead and its compound enter can after body Multiple systems such as nerve, hematopoiesis, digestion, kidney, angiocarpy and endocrine are caused harm.Therefore based on preserving the ecological environment The healthy active demand with the mankind is needed, environmentally friendly leadless piezoelectric material material substitution lead base piezoelectric has been researched and developed It is that one urgent and the having important practical significance of the task.
At present, researchers have been achieved for certain achievement in the aspect of performance for improving leadless piezoelectric material material, but always For, there is not yet can replace the leadless piezoelectric material material of plumbum-based material completely at present, therefore also need to do in-depth study and Explore, further promote the practical development of leadless piezoelectric material material.Japanese Satio in 2004 et al. is sent out on Natue magazines Potassium-sodium niobate (KNN) base piezoelectric ceramic for the doped modification that table is prepared using texture method, its piezoelectric coefficient d33Reach 416pC/N, can be compared favourably with lead base piezoelectric, hereafter, and KNN bases ceramics are ground because its Curie temperature is high, piezoelectric property is good Study carefully as new focus.But K, Na are readily volatilized at high temperature, so that KNN bases ceramics have, compactness is bad, sinter temperature The narrow shortcoming in area, and due to KNbO3Fusing point it is relatively low, more than 1140 DEG C sintering easily form liquid phase in ceramics, greatly Limit the application of KNN bases ceramics.It is well known that the monocrystalline of perovskite structure compared with the polycrystalline ceramics with component have it is excellent Piezoelectric property because monocrystalline has anisotropy, its piezoelectric property has extreme value along specific direction, and polycrystalline ceramics is brilliant There is interaction between grain, piezoelectric response is cancelled out each other, average piezoelectric response is finally shown.But monocrystalline has The significant shortcomings such as component control hardly possible, production cost costliness and cycle length, more applies in expensive medical treatment and sonar spy In terms of survey, it is unfavorable for large-scale industrialization application.Accordingly it is desirable to make polycrystalline ceramics by certain technological means Crystal grain can grow in a certain direction as monocrystalline, and textured ceramics arise at the historic moment.The preparations of textured ceramics it is main by Casting technique, casting technology can be such that anisometric template is uniformly arranged among base-material, when carrying out heat treatment process, mould Plate has bigger surface free energy compared with base-material, therefore crystal grain can be made to be grown along template surface, is made with necessarily taking To textured ceramic.The characteristics of textured ceramic is provided with the advantage and low ceramic material cost of monocrystalline simultaneously, thus by scholar Extensive concern, but from after Satio delivers high performance KNN bases textured ceramic on Nature magazines, KNN bases texture pottery The research of porcelain could not be made a breakthrough again, and most work is all adulterated around pure KNN textured ceramics and single-element KNN bases textured ceramic expansion.For example, Chang Yunfei et al. systematic researches edge<001>(the K of direction texture0.5Na0.5)0.98Li0.02NbO3、(K0.5Na0.5)(Nb0.85Ta0.15)O3、(K0.5Na0.5)Nb0.97Sb0.03O3Adulterated with CuO (K0.476Na0.524)NbO3Piezoelectric ceramics ((1) Y.Chang, S.F.Poterala, Z.Yang, S.T.McKinstry, G.L.Messing,Appl.Phys.Lett.95(2009)232905.(2)Y.Chang,S.F.Poterala,Z.Yang, S.T.McKinstry, G.L.Messing, J.Mater.Res.25 (2011) 687-694.), but the d of these systems33Concentrate In 150-250pC/N, much commercial Application can not can not be more realized with lead base ceramic phase ratio.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of wide sintering warm area and The leadless piezoelectric structured ceramics and preparation method of wide composition regulation.
The purpose of the present invention can be achieved through the following technical solutions：
The leadless piezoelectric structured ceramics of width sintering warm area and wide composition regulation, its chemical analysis meets chemical general formula 0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3, wherein x represents potassium niobate sodium base leadless piezoelectricity shared by Ta The atomic percent of textured ceramic, and 0.15≤x≤0.25.
Preferably, x therein is 0.25.
The leadless piezoelectric structured ceramic preparation method of width sintering warm area and wide composition regulation, using following steps：
(1) base-material is prepared：According to 0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3Middle Na, K, Li, The stoichiometric proportion of Nb, Sb, Ta, Ca and Zr element weighs Na2CO3、K2CO3、Li2CO3、Nb2O5、Sb2O3、Ta2O5、CaCO3With ZrO2, sequentially pass through dispensing, batch mixing, precompressed and burn in step and prepare 0.99K0.49Na0.49Li0.02Nb0.97- xSb0.03TaxO3-0.01CaZrO3Powder base；
(2) template is prepared：NaNbO is prepared with two step molten-salt growth methods3Flaky powder template；
(2-1) uses Bi2O3、Na2CO3、Nb2O5It is raw material with NaCl, according to Bi2.5Na3.5Nb5O18Flaky powder template Stoichiometric proportion, weighs Bi2O3、Na2CO3And Nb2O5, NaCl mass is Bi2O3、Na2CO3And Nb2O51.1 times of gross mass；It is logical Cross fused salt legal system and obtain Bi2.5Na3.5Nb5O18Flaky powder template
(2-2) is with the Bi of acquisition2.5Na3.5Nb5O18Flaky powder template, NaCl and Na2CO3For raw material, control Bi2.5Na3.5Nb5O18Flaky powder template and Na2CO3The ratio of the amount of material is 1：1.75, NaCl quality is Bi2.5Na3.5Nb5O18Flaky powder template and Na2CO31.1 times of gross mass, NaNbO is made by molten-salt growth method3Flaky powder mould Plate；
(3) by the template of acquisition, dispensing is placed in ball grinder according to a certain percentage with base-material, is added solvent and is used every point The rotating speed roller of 60 turns of clock is ground 10-15 hours, is added binding agent and is ground 3-6 hours with 40 turns per minute of rotating speed roller, slurry is made； Solvent is the mixed solution of absolute ethyl alcohol and toluene；The addition of the solvent for per 10g base-materials and needed for template gross weight Correspondence adds 4-6g absolute ethyl alcohols and 5-9g toluene；
(4) obtained slurry is taken out, is cast on a glass using curtain coating scraper, curtain coating speed is 3cm/s- 10cm/s；Standing is kept flat after curtain coating, is scraped from glass plate diaphragm with blade；Lamination is hot-forming after diaphragm is cut, heat Molded temperature is 60-100 DEG C, and pressure is 15MPa-40MPa；Taking out the sample pressed, the row of progress is viscous successively, be heat-treated, and obtains It is wide sintering warm area, the leadless piezoelectric structured ceramics of wide composition regulation to the good leadless piezoelectric structured ceramic material of orientation.
Template quality accounts for the 1-6% of base-material gross mass, preferably 3% described in step (3)；The addition of solvent is every 10g base-materials addition 5g absolute ethyl alcohols corresponding with the gross weight of required template and 6.5g toluene；Middle addition solvent carries out roller mill, rotating speed For 60 turns per minute, roller time consuming is 10 hours；Add binding agent and carry out roller mill, rotating speed is 40 turns per minute, roller time consuming For 4 hours.
In step (4), the lamination, the hot-forming film for referring to scrape after curtain coating is stood are cut into 1.15cm × 1.15cm Piece, these a number of pieces are added to certain height, are then placed in mould, and on die coat one can With the heater of regulating and controlling temperature, then this is placed under single shaft tablet press machine added with the mould of heater, 60- is heated to 100 DEG C, 4 pressurizations are repeated, pressure size is 15MPa-40MPa, and the total time of heat-insulation pressure keeping is 1 hour, can make lamination Even compact is bonded together as a fine and close sheet green compact.
Highly preferred 200 μm of the preferred 6cm/s of speed of curtain coating in step (4), curtain coating scraper and glass plate；Put down after curtain coating Put standing 3 hours；Hot-forming temperature is preferably 70 DEG C；Hot-forming pressure is preferably 20MPa；Heat treatment is used Two-step sintering mode, the first step is that 1170-1185 DEG C is warming up to 6-8h from room temperature, is incubated 0-20min；Second step is with 8-15 DEG C/min rate of temperature fall is quickly cooled to 1060-1085 DEG C, is incubated 6-12h；Heat treatment is carried out in silicon carbide rod furnace.
Preferably, the heat treatment in step (4) is to use two-step sintering mode, and a step is to be warming up to from room temperature with 7h 1180 DEG C, 5min is incubated, second step is quickly cooled to 1065 DEG C with 10 DEG C/min rate of temperature fall, is incubated 10h.
The leadless piezoelectric structured ceramic applications prepared are in piezoelectric transducer, piezoelectric motors and high precision displacement control In system.
Compared with prior art, invention uses the anisometric NaNbO of sheet3Template is done, with casting technology 0.99K is realized with reference to two-step sintering0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3The texturing of ceramics, letter It is single feasible, a kind of wide sintering warm area, the leadless piezoelectric structured ceramic material of wide composition regulation can be prepared, so as to overcome biography Commons material random growth, the sciences problems of limited performance, with advantages below：
1st, casting technology is ripe wide variety of technology in ceramic industry, and preparation cost is low, technique is simple, it is large quantities of to be adapted to The industrialized production of amount.
2nd, compared with the technology that tradition prepares ceramics using prilling, prepared using casting technology 0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3Textured lead-free piezoceramic material is shown well The degree of orientation.The shearing force of scraper makes anisometric NN templates be uniformly arranged in along curtain coating direction in base-material in casting processes, Template has higher surface free energy compared with base-material, when heat treatment process provides enough activation energy (surface free energy difference) When, base-material will carry out hetero-epitaxy forming core in the minimum energy face of template ({ 100 } face), forms the crystal grain of oriented growth, takes Further grow up and form to crystal grain<001>The class monocrystalline textured ceramic of orientation, has the characteristic of ceramics and monocrystalline concurrently.
3、0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3Textured lead-free piezoceramic material With the ceramic phase ratio of other KNN bases, holding temperature is low (1065 DEG C), and sintering warm area is wide (1060-1085 DEG C can be into porcelain), component Scope is wide, and (ceramic piezoelectric property may remain in higher level, d in this interval range of 0.15≤x≤0.2533It is all higher than 300pC/N).Tantalum and niobium belong to same family, and chemical property is quite similar, niobium minerals and tantalum ore symbiosis, Masato etc. in nature The research of people shows that addition tantalum element can improve the mechanical coupling coefficient and mechanical quality factor of material in pure KNN ceramics (M.Matsubara,T.Yamaguchi,W.Sakamoto,K.Kikuta,T.Yogo,S-I.Hirano,Processing and Piezoelectric Properties of Lead-Free(K,Na)(Nb,Ta)O3 Ceramics.Journal of the American Ceramic Society 2005,88(5),1190-1196.).Ta atom is found after systematic research Percentage is when more than or equal to 0.15, and material is readily available higher piezoelectric property, in conjunction with casting technique, prepares edge< 001>The KNN base piezoelectric ceramics of direction texture, obtain good piezoelectric property.
4th, with the ceramic phase ratio of other systems, 0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3Knit The lead-free piezoceramic material Curie temperature of structure is high, and the Curie temperature of material remains unchanged up to 223 DEG C during x=0.25, it is ensured that Material can not lose piezoelectric property because ferroelectric phase is changed into paraelectric phase under the hot environment spent 100 more.Pure KNN ceramics tools There is higher Curie temperature, but piezoelectric property is not high；The elements such as doping Ta, Sb, Ca, Zr can improve the piezoelectric property of material, but The Curie temperature of material can be reduced；The doping of Li elements can improve the Curie temperature of material.In order to obtain high tension performance, be in In temperature piezoelectric ceramics, introduce 2at% Li elements can prevent a large amount of doping of Ta elements and cause material Curie temperature big Amplitude declines.
5、0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3Textured lead-free piezoceramic material With the ceramic phase ratio of current KNN bases, with higher piezoelectric modulus, the ceramic pressure in the interval range of 0.15≤x≤0.25 Electrostrictive coefficient is all higher than 300pC/N, is almost compared favourably with lead base ceramics, and this lays the foundation for the commercial Application of material.
6th, 0.99K of the invention0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3Leadless piezoelectric structured ceramics Material can be widely used in piezoelectric transducer, piezoelectric motors and high precision displacement control.
Brief description of the drawings
Fig. 1 is the piezoelectric modulus (d of the ceramic material prepared in embodiment 1,2 and 333) tendency chart；
Fig. 2 is in embodiment 1<001>The XRD spectrum of direction leadless piezoelectric ceramics；
Fig. 3 is in embodiment 1<001>The high temperature temperature spectrum of direction leadless piezoelectric ceramics.
Fig. 4 is in embodiment 3<001>The XRD spectrum of direction leadless piezoelectric ceramics；
Fig. 5 is actually applied in example 3<001>The high temperature temperature spectrum of direction leadless piezoelectric ceramics.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.Following examples will be helpful to this area Technical staff further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the general of this area For logical technical staff, without departing from the inventive concept of the premise, various modifications and improvements can be made.These are belonged to Protection scope of the present invention.
Embodiment 1：
0.99K0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3-0.01CaZrO3The preparation of base-material：Using Na2CO3、 K2CO3、Li2CO3、Nb2O5、Sb2O3、Ta2O5、CaCO3And ZrO2For raw material, first according to 0.99K0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3-0.01CaZrO3The change of middle Na, K, Li, Nb, Sb, Ta, Ca and Zr element Learn metering ratio and weigh Na2CO3、K2CO3、Li2CO3、Nb2O5、Sb2O3、Ta2O5、CaCO3And ZrO2, sequentially pass through dispensing, batch mixing, pre- Pressure and burn in step prepare 0.99K0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3-0.01CaZrO3Base-material；Heat treatment temperature Spend for 850 DEG C, soaking time is 6h.
Weigh the 0.99K of the above-mentioned preparations of 10.0g0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3-0.01CaZrO3Base-material, so After weigh 0.3g NaNbO3Template, adds 6.5g toluene and 5.0g absolute ethyl alcohols roller mill after 12 hours, adds 5.5g binding agents Roller is ground 4 hours, and slurry is made；The slurry made is taken out, is cast on a glass using curtain coating scraper, curtain coating speed is 6cm/s, scraper is highly 200 μm；Standing is kept flat after curtain coating 3 hours, diaphragm can be scraped from glass plate；Diaphragm is cut into Lamination after 11.5mm × 11.5mm square piece, hot-forming at 70 DEG C, hot pressing pressure is 20Mpa, heat-insulation pressure keeping 1 hour；Will be into Base substrate after type is viscous in 550 DEG C of rows, is finally heat-treated in silicon carbide rod furnace, heat treatment uses two-step sintering mode, The first step is raised to 1180 DEG C from room temperature, and the heating-up time is 7h, and soaking time is 5min；Second step is with 10 DEG C/min cooling rate 1065 DEG C are quickly cooled to, 10h is incubated；Prepare the good leadless piezoelectric structured ceramic material of the degree of orientation.
Fig. 1 is the d of the textured ceramic prepared in embodiment 1,2 and 333Tendency chart, from figure we can see that 0.99K0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3-0.01CaZrO3The d of textured ceramic33Up to 315pC/N, than most of Other KNN bases ceramics performance will be superior.
Fig. 2 is edge<001>The 0.99K of direction texture0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3-0.01CaZrO3It is unleaded The XRD spectrum of piezoelectric ceramics.It can be seen that from figure<00l>The more random oriented material of relative intensity of diffraction maximum has significantly Enhancing, shows that material introduces NaNbO3Orientation is generated after template.By the calculating to material XRD spectrum, its Lotgering ' s Factor (f)=80.9%.
Fig. 3 is edge<001>The 0.99K of direction texture0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3-0.01CaZrO3Nothing The high temperature temperature spectrum of lead piezoelectric ceramics, it will be seen that 0.99K from figure0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3- 0.01CaZrO3The Curie temperature of textured ceramic is 263 DEG C, it is meant that the temperature that material is changed into paraelectric phase from ferroelectric phase is higher, Material can be applied in high-temperature field.
Embodiment 2：
Weigh the 0.99K of the above-mentioned preparations of 10.0g0.49Na0.49Li0.02Nb0.77Sb0.03Ta0.20O3-0.01CaZrO3Base-material, so After weigh 0.3g NaNbO3Template, is added after 6.5g toluene and 5.0g absolute ethyl alcohols roller grind 12 hours, add 5.5g binding agents after Continuous roller is ground 4 hours, and slurry is made；The slurry made is taken out, is cast on a glass using curtain coating scraper, curtain coating speed is 6cm/s, scraper is highly 200 μm；Standing is kept flat after curtain coating 3 hours, diaphragm can be scraped from glass plate；Diaphragm is cut into Lamination after 11.5mm × 11.5mm square piece, hot-forming at 70 DEG C, hot pressing pressure is 20Mpa, heat-insulation pressure keeping 1 hour；Will be into Base substrate after type is viscous in 550 DEG C of rows, is finally heat-treated in silicon carbide rod furnace, heat treatment uses two-step sintering mode, The first step is raised to 1180 DEG C from room temperature, and the heating-up time is 7h, and soaking time is 5min；Second step is with 10 DEG C/min cooling rate 1065 DEG C are quickly cooled to, 10h is incubated；Prepare the good leadless piezoelectric structured ceramic material of the degree of orientation.
Fig. 1 is the d of the textured ceramic prepared in embodiment 1,2 and 333Tendency chart, from figure we can see that 0.99K0.49Na0.49Li0.02Nb0.77Sb0.03Ta0.20O3-0.01CaZrO3The d of textured ceramic33Up to 357pC/N, than 0.99K0.49Na0.49Li0.02Nb0.82Sb0.03Ta0.15O3-0.01CaZrO3The piezoelectric modulus of ceramics is high, illustrates to add Ta elements The piezoelectric property of material can be improved.
Embodiment 3：
Weigh the 0.99K of the above-mentioned preparations of 10.0g0.49Na0.49Li0.02Nb0.72Sb0.03Ta0.25O3-0.01CaZrO3Base-material, so After weigh 0.3g NaNbO3Template, is added after 6.5g toluene and 5.0g absolute ethyl alcohols roller grind 12 hours, add 5.5g binding agents after Continuous roller is ground 4 hours, and slurry is made；The slurry made is taken out, is cast on a glass using curtain coating scraper, curtain coating speed is 6cm/s, scraper is highly 200 μm；Standing is kept flat after curtain coating 3 hours, diaphragm can be scraped from glass plate；Diaphragm is cut into Lamination after 11.5mm × 11.5mm square piece, hot-forming at 70 DEG C, hot pressing pressure is 20Mpa, heat-insulation pressure keeping 1 hour；Will be into Base substrate after type is viscous in 550 DEG C of rows, is finally heat-treated in silicon carbide rod furnace, heat treatment uses two-step sintering mode, The first step is raised to 1180 DEG C from room temperature, and the heating-up time is 7h, and soaking time is 5min；Second step is with 10 DEG C/min cooling rate 1065 DEG C are quickly cooled to, 10h is incubated；Prepare the good leadless piezoelectric structured ceramic material of the degree of orientation.
Fig. 1 is the d of the textured ceramic prepared in embodiment 1,2 and 333Tendency chart, from figure we can see that 0.99K0.49Na0.49Li0.02Nb0.72Sb0.03Ta0.25O3-0.01CaZrO3The d of textured ceramic33Up to 372pC/N, than most of Other KNN bases ceramics performance will be superior, can be compared favourably with lead base piezoelectric ceramics.
Fig. 4 is edge<001>The 0.99K of direction texture0.49Na0.49Li0.02Nb0.72Sb0.03Ta0.25O3-0.01CaZrO3It is unleaded The XRD spectrum of piezoelectric ceramics.It can be seen that from figure<00l>The more random oriented material of relative intensity of diffraction maximum has significantly Enhancing, shows that material introduces NaNbO3Orientation is generated after template.By the calculating to material XRD spectrum, its Lotgering ' s Factor (f)=82.1%.
Fig. 5 is edge<001>The 0.99K of direction texture0.49Na0.49Li0.02Nb0.72Sb0.03Ta0.25O3-0.01CaZrO3It is unleaded The high temperature temperature spectrum of piezoelectric ceramics, 0.99K0.49Na0.49Li0.02Nb0.72Sb0.03Ta0.25O3-0.01CaZrO3The Curie of textured ceramic Temperature is 223 DEG C, illustrates that Ta doping reduces the Curie temperature of material, but Curie temperature value declines and little, and material exists Still there is higher Curie temperature in the case of high Ta dopings, can apply in high-temperature field.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring the substantive content of the present invention.

Claims (10)

1. the leadless piezoelectric structured ceramics of width sintering warm area and wide composition regulation, it is characterised in that the ceramic chemical analysis symbol Close chemical general formula 0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3, wherein x represents potassium-sodium niobate shared by Ta The atomic percent of base leadless piezoelectricity textured ceramic, and 0.15≤x≤0.25.
2. the leadless piezoelectric structured ceramics of wide sintering warm area according to claim 1 and wide composition regulation, it is characterised in that X therein preferably 0.25.
3. the leadless piezoelectric structured ceramic preparation method of wide sintering warm area as claimed in claim 1 and wide composition regulation, its It is characterised by, this method uses following steps：
(1) base-material is prepared：According to 0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3-0.01CaZrO3Middle Na, K, Li, Nb, The stoichiometric proportion of Sb, Ta, Ca and Zr element weighs Na2CO3、K2CO3、Li2CO3、Nb2O5、Sb2O3、Ta2O5、CaCO3And ZrO2, Sequentially pass through dispensing, batch mixing, precompressed and burn in step and prepare 0.99K0.49Na0.49Li0.02Nb0.97-xSb0.03TaxO3- 0.01CaZrO3Powder base；
(2) template is prepared：NaNbO is prepared with two step molten-salt growth methods3Flaky powder template；
(2-1) uses Bi2O3、Na2CO3、Nb2O5It is raw material with NaCl, according to Bi2.5Na3.5Nb5O18The chemistry of flaky powder template Metering ratio, weighs Bi2O3、Na2CO3And Nb2O5, NaCl mass is Bi2O3、Na2CO3And Nb2O51.1 times of gross mass；By molten Salt legal system obtains Bi2.5Na3.5Nb5O18Flaky powder template
(2-2) is with the Bi of acquisition2.5Na3.5Nb5O18Flaky powder template, NaCl and Na2CO3For raw material, control Bi2.5Na3.5Nb5O18Flaky powder template and Na2CO3The ratio of the amount of material is 1：1.75, NaCl quality is Bi2.5Na3.5Nb5O18Flaky powder template and Na2CO31.1 times of gross mass, NaNbO is made by molten-salt growth method3Flaky powder mould Plate；
(3) by the template of acquisition, dispensing is placed in ball grinder according to a certain percentage with base-material, is added solvent and is used per minute 60 The rotating speed roller turned is ground 10-15 hours, is added binding agent and is ground 3-6 hours with 40 turns per minute of rotating speed roller, slurry is made；Solvent For absolute ethyl alcohol and the mixed solution of toluene；The addition of the solvent is corresponding per 10g base-materials gross weight of template with needed for Add 4-6g absolute ethyl alcohols and 5-9g toluene；
(4) obtained slurry is taken out, is cast on a glass using curtain coating scraper, curtain coating speed is 3cm/s-10cm/s； Standing is kept flat after curtain coating, is scraped from glass plate diaphragm with blade；Lamination is hot-forming after diaphragm is cut, hot-forming Temperature is 60-100 DEG C, and pressure is 15MPa-40MPa；Taking out the sample pressed, the row of progress is viscous successively, be heat-treated, and obtains orientation good Good leadless piezoelectric structured ceramic material, is wide sintering warm area, the leadless piezoelectric structured ceramics of wide composition regulation.
4. the leadless piezoelectric structured ceramic preparation method of wide sintering warm area according to claim 3 and wide composition regulation, Characterized in that, template quality accounts for the 1-6% of base-material gross mass, preferably 3% described in step (3).
5. the leadless piezoelectric structured ceramic preparation method of wide sintering warm area according to claim 3 and wide composition regulation, Characterized in that, the addition of solvent is per the anhydrous second of the corresponding addition 5g of 10g base-materials gross weight of template with needed in step (3) Alcohol and 6.5g toluene.
6. the leadless piezoelectric structured ceramic preparation method of wide sintering warm area according to claim 3 and wide composition regulation, Characterized in that, solvent is added in step (3) carries out roller mill, rotating speed is 60 turns per minute, and roller time consuming is 10 hours；Add Binding agent carries out roller mill, and rotating speed is 40 turns per minute, and roller time consuming is 4 hours.
7. the leadless piezoelectric structured ceramic preparation method of wide sintering warm area according to claim 3 and wide composition regulation, Characterized in that, highly preferred 200 μm of the preferred 6cm/s of speed being cast in step (4), curtain coating scraper and glass plate；Curtain coating After keep flat standing 3 hours；Hot-forming temperature is preferably 70 DEG C；Hot-forming pressure is preferably 20MPa.
8. the leadless piezoelectric structured ceramic preparation method of wide sintering warm area according to claim 3 and wide composition regulation, Characterized in that, the heat treatment described in step (4) uses two-step sintering mode, the first step is to be warming up to from room temperature with 6-8h 1170-1185 DEG C, it is incubated 0-20min；Second step is to be quickly cooled to 1060-1085 DEG C with 8-15 DEG C/min rate of temperature fall, It is incubated 6-12h；Heat treatment is carried out in silicon carbide rod furnace.
9. the leadless piezoelectric structured ceramic preparation method of wide sintering warm area according to claim 8 and wide composition regulation, Characterized in that, the heat treatment described in step (4) uses two-step sintering mode, the first step is to be warming up to from room temperature with 7h 1180 DEG C, 5min is incubated, second step is quickly cooled to 1065 DEG C with 10 DEG C/min rate of temperature fall, is incubated 10h.
10. the leadless piezoelectric structured ceramic preparation method of wide sintering warm area according to claim 3 and wide composition regulation, Characterized in that, the leadless piezoelectric structured ceramic applications prepared are in piezoelectric transducer, piezoelectric motors and high precision position Move in control.
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