CN1286774C - Niobate leadless piezoelectric material material and preparation method thereof - Google Patents

Niobate leadless piezoelectric material material and preparation method thereof Download PDF

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CN1286774C
CN1286774C CN 200510018833 CN200510018833A CN1286774C CN 1286774 C CN1286774 C CN 1286774C CN 200510018833 CN200510018833 CN 200510018833 CN 200510018833 A CN200510018833 A CN 200510018833A CN 1286774 C CN1286774 C CN 1286774C
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CN1699280A (en
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曹明贺
刘韩星
王万强
罗大兵
郝华
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Wuhan University of Technology WUT
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Abstract

The present invention relates to a niobate leadless piezoelectric material and a preparation method thereof. The material is mainly composed of (K<0.44>Na<0.52>Li<0.04>) (Nb<0.84>Ta<0.10>Bb<0.06>) O<3> chemically, wherein 1 to 30 vol% of SrTiO3 powder lot is added. In the preparation method for the niobate leadless piezoelectric material, the powder lot of KHCO3, NaHCO3, Li2CO3, Nb2O5, Ta2O and Sb2O is first compounded according to a stoichiometric ratio, anhydrous alcohol is added, and the powder lot and the anhydrous alcohol are mixed and milled through balls for 12 h to 24 h; then, at the temperature of 70 DEG C to 150 DEG C, the mixture is baked; a cementing agent is added to the baked material, and the material is pressed into a block-shaped blank body; after pre-burned at the temperature of 700 DEG C to 790 DEG C in an alumina porcelain crucible, the blank body is pulverized and milled through balls; the SrTio3 powder lot is added to the material milled through balls; the material milled through balls is placed in a beaker, anhydrous alcohol is added, and the material milled through balls and the anhydrous alcohol are stirred for 12 h to 24 h; then, the material milled through balls and the anhydrous alcohol are baked at the temperature of 70 DEG C to 150 DEG C and are pressed into blank sheets with phi of 12mm and the thickness of 2mm with pressure of 4 to MPa; the material milled through balls and the anhydrous alcohol are buried, burned and thermally processed for 1 to 5 h at the temperature of 1100 DEG C to 1250 DEG C in air, and leadless piezoelectric ceramics are obtained. After the SrTio3 is added, the sintering character of niobate leadless piezoelectric ceramics in the KNNT system is improved, and the piezoelectric properties are also greatly improved.

Description

A kind of columbate leadless piezoelectric materials
Technical field
The present invention relates to a kind of columbate leadless piezoceramic material and preparation method thereof, be specifically related to a kind of with SrTiO 3Powder carries out the (K of doping vario-property 0.44Na 0.52Li 0.04) (Nb 0.84Ta 0.10Sb 0.06) O 3(KNNT) columbate leadless piezoceramic material and preparation method thereof.
Background technology
Piezoelectricity has widely in the detection of various information, dump, stores processor to be used, and uses very wide in many high and new technologies fields such as information, space flight, laser and biology; Yet up to now, exhausted most piezoelectric is still plumbiferous.Wherein plumbous oxide or tri-lead tetroxide account for starting material gross weight 70%, the production of these materials, use and the process of discarded aftertreatment in all can bring serious harm to human health and ecotope, the theory of this and human social is runed counter to, add because the global resources storage is limited, according to the estimation of internal authority department, the lead of estimating the whole world in 20 years is with approach exhaustion.Therefore, develop non-lead base environment compatibility piezoceramic material be one urgent and have a problem of great Practical significance.
ANbO 3(its A is Li, Na or K) type niobate is the important leadless piezoelectric material material system of a class, and it is the material that a class has perovskite-like structure.Compare with other lead-free ceramics system, this compounds has characteristics such as piezoelectric property is better, and specific inductivity is low, and frequency constant is big, and density is little, is one of material system that replaces the consideration of lead base piezoceramic material emphasis.But,, be difficult to realize densification sintering with ordinary method owing to Li, Na, K are easy to volatilization.
Summary of the invention
The purpose of this invention is to provide a kind of columbate leadless piezoceramic material, a kind of preparation method of this piezoceramic material is provided simultaneously.
The present invention adopts and introduce SrTiO in the niobate material 3Method, can prepare the high (K of density with traditional solid sintering technology 0.44Na 0.52Li 0.04) (Nb 0.81Ta 0.10Sb 0.06) O 3(KNNT) type columbate leadless piezoelectric ceramics; The piezoelectric property of the KNNT type columbate leadless piezoelectric ceramics of its preparation method preparation is also improved by a relatively large margin, is suitable for industrial production.
The present invention adopts the KHCO of commercial purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Be starting raw material, with commercial SrTiO 3Be the doping vario-property material, preparation meets the lead-free piezoceramic material of performance requriements.
Its technical scheme is:
A kind of columbate leadless piezoelectric materials, its main chemical constitution is (K 0.44Na 0.52Li 0.04) (Nb 0.84Ta 0.10Sb 0.06) O 3(KNNT), wherein mix the SrTiO of 1～30vol% 3Powder.
The preparation process of this columbate leadless piezoelectric materials is:
The first, elder generation is with the KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by the stoichiometric ratio batching, add dehydrated alcohol as dispersion medium, the volume ratio of dehydrated alcohol and powder is 5～1: 1, and mixing and ball milling 12～24h is dried under 70～150 ℃ of temperature then, material after the oven dry adds concentration and makes cakingagent for the 2wt% polyvinyl alcohol water solution, carry out granulation, the volume ratio of its cakingagent and powder is 0.1～0.15: 1, is pressed into block base substrate then, place alumina porcelain crucible pre-burning 3～5h, calcined temperature is 700～790 ℃;
The second, the blank of gained after step 1 pre-burning is pulverized ball milling, the material after the ball milling mixes the SrTiO of 1～30vol% 3Powder, insert in the beaker then, add the dehydrated alcohol dispersion medium, the volume ratio of ethanol and powder is 5～1: 1, stir 12～24h, under 70～150 ℃ of temperature, dry again, material after the oven dry is that the 2wt% polyvinyl alcohol water solution is as cakingagent with concentration, forming under the pressure at 4～6MPa is the thick 2mm round billet of a diameter 12mm sheet, the volume ratio of its cakingagent and powder is 0.1～0.15: 1, base substrate buries burning thermal treatment under 1100～1250 ℃ of temperature in air atmosphere, thermal treatment insulation 1～5h promptly makes columbate leadless piezoelectric materials.
One-tenth porcelain base substrate burning infiltration silver electrode after its thermal treatment polarizes in 120 ℃ silicone oil then, uses d 33The piezoelectric constant survey meter is measured d 33
The present invention is by control KNNT and SrTiO 3SrTiO in volume ratio=1: 0.01～0.30 3Incorporation, obtained a kind of density height, novel columbate leadless piezoelectric materials that piezoelectric property is good by control moulding process and sintering schedule.
Description of drawings
Fig. 1 is different SrTiO 3The piezoelectric constant d of the KNNT pottery of incorporation 33Comparison diagram;
Fig. 2 is different SrTiO 3The relative density distribution plan of the KNNT ceramics sample of incorporation:
A among Fig. 3, b, c, d are KNNT: SrTiO 3Volume ratio be respectively: 1: 0,1: 0.07, the SEM figure of the KNNT pottery of 1: 0.2 and 1: 0.3;
As can be seen from Figure 1, KNNT: SrTiO 3Volume ratio be 1: 0.05 o'clock, the d of goods 33Value is best;
As can be seen from Figure 2, along with SrTiO 3The increase of incorporation, the density of goods increases, and works as KNNT: SrTiO 3Volume ratio be approximately at 1: 0.2 o'clock, it is best that the goods density reaches;
As can be seen from Figure 3, at KNNT: SrTiO 3Volume ratio be respectively: 1: 0,1: 0.07, in 1: 0.2 and 1: 0.3 four sample, work as KNNT: SrTiO 3Volume ratio be approximately at 1: 0.2 o'clock, it is best that the void content minimum of goods, density reach, with the rule basically identical of Fig. 2 reflection.
Embodiment
The embodiment of the invention is with KNNT and SrTiO 3Volume ratio is that 1: 0.01～0.30 ratio prepares leadless piezoelectric ceramics, and the method for employing is traditional solid sintering technology.
Concrete enforcement is as follows: elder generation is with the KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder adds dehydrated alcohol as dispersion medium by the stoichiometric ratio batching, and the volume ratio of dehydrated alcohol and powder is 5～1: 1, and mixing and ball milling 12h is dried under 70～150 ℃ of temperature then; Material after the oven dry adds concentration and makes cakingagent for the 2wt% polyvinyl alcohol water solution, carries out granulation, and the volume ratio of its cakingagent and powder is 0.1～0.15: 1, is pressed into sheet then, places alumina porcelain crucible pre-burning 3～5h, and calcined temperature is 700～790 ℃; Carry out the crushing ball mill after pre-burning is finished, the material after the ball milling mixes 1～30vol%SrTiO 3Powder, insert in the wide-mouth beaker, magnetic agitation 12～24h, dispersion agent is a dehydrated alcohol, the volume ratio of dehydrated alcohol and powder is 5～1: 1, under 70～150 ℃ of temperature, dry then, material after the oven dry is that the 2wt% polyvinyl alcohol water solution is as cakingagent with concentration, forming under the pressure at 4～6MPa is the thick 2mm round billet of a diameter phi 12mm sheet, the volume ratio of its cakingagent and powder is 0.1～0.15: 1, base substrate buries burning thermal treatment under 1100～1250 ℃ of temperature in air atmosphere, the thermal treatment soaking time is 1～5h.One-tenth porcelain base substrate burning infiltration silver electrode after the thermal treatment polarizes in 120 ℃ silicone oil then.Use d 33The piezoelectric constant survey meter is measured d 33
The prescription and the following embodiment of condition of preparation KNNT based leadless piezoelectric ceramics.
Embodiment 1
Press KNNT and SrTiO 3Volume ratio is that 1: 0.01 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.KHCO with purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 700 ℃ of pre-burning 3h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1130 ℃ of sintering temperatures of air atmosphere, sintering time is 3h.
Embodiment 2
Press KNNT and SrTiO 3Volume ratio is that 1: 0.03 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 700 ℃ of pre-burning 5h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 5MPa, and in 1170 ℃ of sintering temperatures of air atmosphere, sintering time is 3h.
Embodiment 3
Press KNNT and SrTiO 3Volume ratio is that 1: 0.05 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 750 ℃ of pre-burning 3h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1185 ℃ of sintering temperatures of air atmosphere, sintering time is 2h.
Embodiment 4
Press KNNT and SrTiO 3Volume ratio is that 1: 0.07 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 780 ℃ of pre-burning 5h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1170 ℃ of sintering temperatures of air atmosphere, sintering time is 5h.B. among the SEM of product sample such as Fig. 3
Embodiment 5
Press KNNT and SrTiO 3Volume ratio is that 1: 0.10 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 770 ℃ of pre-burning 4h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1180 ℃ of sintering temperatures of air atmosphere, sintering time is 1h.
Embodiment 6
Press KNNT and SrTiO 3Volume ratio is that 1: 0.15 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 790 ℃ of pre-burning 4h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1185 ℃ of sintering temperatures of air atmosphere, sintering time is 3h.
Embodiment 7
Press KNNT and SrTiO 3Volume ratio is that 1: 0.20 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 760 ℃ of pre-burning 3.5h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1175 ℃ of sintering temperatures of air atmosphere, sintering time is 3h.The SEM of product sample is as c. in 3
Embodiment 8,
Press KNNT and SrTiO 3Volume ratio is that 1: 0.30 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 780 ℃ of pre-burning 4.5h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1200 ℃ of sintering temperatures of air atmosphere, sintering time is 3.5h.The SEM of product sample is as d. in 3
Embodiment 9,
Press KNNT and SrTiO 3Volume ratio is that 1: 0.30 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 780 ℃ of pre-burning 4h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1200 ℃ of sintering temperatures of air atmosphere, sintering time is 4h.
Embodiment 10,
Press KNNT and SrTiO 3Volume ratio is that 1: 0.20 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 790 ℃ of pre-burning 3h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1185 ℃ of sintering temperatures of air atmosphere, sintering time is 5h.
Embodiment 11,
Press KNNT and SrTiO 3Volume ratio is that 1: 0.15 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 770 ℃ of pre-burning 4h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1185 ℃ of sintering temperatures of air atmosphere, sintering time is 3.5h.
Embodiment 12,
Press KNNT and SrTiO 3Volume ratio is that 1: 0.33 ratio prepares leadless piezoelectric ceramics, adopts traditional solid sintering technology.The KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by after the stoichiometric ratio batching, mixing and ball milling, and at 700 ℃ of pre-burning 4.5h, the material after the pre-burning is pulverized ball milling, is the thick 2mm round billet of diameter phi 12mm sheet at the forming under the pressure of 4MPa, and in 1175 ℃ of sintering temperatures of air atmosphere, sintering time is 4h.

Claims (1)

1, a kind of columbate leadless piezoceramic material is characterized in that the main chemical constitution of this stupalith is (K 0.44Na 0.52Li 0.04) (Nb 0.84Ta 0.10Sb 0.06) O 3, wherein mix the SrTiO of volume 1～30% 3Powder, preparation as follows, its preparation process is:
The first, elder generation is with the KHCO of purity 99.5% 3, the NaHCO of purity 99.5% 3, the Li of purity 99.5% 2CO 3, the Nb of purity 99.5% 2O 5, the Ta of purity 99.0% 2O 5And the Sb of purity 99.0% 2O 5Powder is by the stoichiometric ratio batching, add dehydrated alcohol as dispersion medium, the volume ratio of dehydrated alcohol and powder is 5～1: 1, and mixing and ball milling 12～24 hours is dried under 70～150 ℃ of temperature then, it is that 2% polyvinyl alcohol water solution is made cakingagent that material after the oven dry adds mass concentration, carry out granulation, the volume ratio of its cakingagent and powder is 0.1～0.15: 1, is pressed into block base substrate then, place alumina porcelain crucible pre-burning 3～5 hours, calcined temperature is 700～790 ℃;
The second, the blank of gained after step 1 pre-burning is pulverized ball milling, the material after the ball milling mixes the SrTiO of volume 1～30% 3Powder, insert in the beaker then, add the dehydrated alcohol dispersion medium, the volume ratio of dehydrated alcohol and powder is 5～1: 1, stirred 12～24 hours, under 70～150 ℃ of temperature, dry again, material after the oven dry is that 2% polyvinyl alcohol water solution is a cakingagent with mass concentration, is 12 millimeters of diameters at the forming under the pressure of 4～6 MPas, thick 2 millimeters round billet sheet, the volume ratio of its cakingagent and powder is 0.1～0.15: 1, base substrate buries burning thermal treatment under 1100～1250 ℃ of temperature in air atmosphere, thermal treatment insulation 1～5 hour promptly makes the columbate leadless piezoceramic material.
CN 200510018833 2005-06-02 2005-06-02 Niobate leadless piezoelectric material material and preparation method thereof Expired - Fee Related CN1286774C (en)

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CN100518995C (en) * 2005-12-28 2009-07-29 中国科学院长春应用化学研究所 Composite crucible for preparing rare earth-magnesium intermediate alloy by molten salt electrolysis and preparation method thereof
US7779522B2 (en) * 2006-05-05 2010-08-24 Fujifilm Dimatix, Inc. Method for forming a MEMS
CN100424037C (en) * 2006-11-23 2008-10-08 陕西师范大学 Tantalum substitutional sodium potassium niobate based piezoelectric ceramics without plumbum, and preparation method
CN101885611B (en) * 2010-07-29 2013-04-17 西安理工大学 Method for preparing piezoelectric material for roads by spraying technology

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