CN104098334A - Method for synthetizing leadless piezoelectric ceramic K0.65Na0.35NbO3 powder adopting two-step hydrothermal method - Google Patents

Method for synthetizing leadless piezoelectric ceramic K0.65Na0.35NbO3 powder adopting two-step hydrothermal method Download PDF

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CN104098334A
CN104098334A CN201410333443.2A CN201410333443A CN104098334A CN 104098334 A CN104098334 A CN 104098334A CN 201410333443 A CN201410333443 A CN 201410333443A CN 104098334 A CN104098334 A CN 104098334A
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CN104098334B (en
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蒲永平
刘雨雯
靳乾
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Shaanxi University of Science and Technology
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Abstract

The invention provides a method for synthetizing leadless piezoelectric ceramic K0.65Na0.35NbO3 powder adopting a two-step hydrothermal method. Excess potassium hydroxide and excess sodium hydroxide are taken as a potassium source and a sodium source respectively and dissolved in deionized water; then niobium pentoxide is added into the solution respectively, and precursor solutions of KNbO3 and NaNbO3 can be synthesized respectively after even stirring; the precursor solutions are sealed in a hydrothermal kettle respectively, the hydrothermal kettle is placed in a thermostat for hydrothermal synthesis at a certain temperature, cooling to the room temperature is performed after the reaction, and powder obtained through the reaction is washed with deionized water for several times and dried finally. After a grinding process, KNbO3 powder and NaNbO3 powder are accurately weighed and mixed in the deionized water; microwave oscillation is performed after stirring; the mixture is poured into a hydrothermal reaction kettle and sealed for hydrothermal synthesis, cooling to the room temperature is performed after the reaction, and a mixed liquid obtained through the reaction is fully dried to obtain the powder. According to the method, the two-step hydrothermal method is adopted to synthetize the K0.65Na0.35NbO3 powder, the preparation technology is good in repeatability, the material component proportion is accurate, the powder is good in uniformity and high in purity, and crystal grains are complete in development and even in distribution.

Description

A kind of two one-step hydrothermals synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder
Technical field
The present invention relates to piezoelectric ceramic powder preparation field, especially a kind of two one-step hydrothermals synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder.
Background technology
The piezoceramic material using is at present with Pb-based lanthanumdoped zirconate titanates, and wherein in lead base piezoelectric ceramics, plumbous oxide accounts for 70% of starting material gross weight.Because plumbous oxide is a kind of volatile toxic substance, cause serious harm in the treating processes after using and discarding the mankind and ecotope; In preparation process, need sealed sintering, not only increased product cost, also caused the consistency of performance of product poor simultaneously.Along with the enhancing of social sustainable development implementation and people's environmental consciousness, the research of lead-free piezoceramic material and application cause people's concern more day by day.Than lead base piezoelectric ceramics such as PZT, for many years for valued base metal niobate pottery (KNbO 3, NaNbO 3, LiNbO 3) everyway has more excellent performance, specific inductivity is little, frequency constant is large, piezoelectricity is high and density is little etc.In addition, again because the metal ions such as Nb, Na, K all belong to non-toxic substance concerning human body and physical environment, and NaNbO 3-KNbO 3system is after improving conventional sintering technique, and properties can be better than the leadless piezoelectric ceramics of other system greatly; And with respect to PZT pottery, (K, Na) NbO 3pottery also has specific inductivity preferably, lower mechanical Qm value, low density and the high advantages such as acoustic propagation velocity, thereby also obtained application in high-frequency transducer field.Most important, (K, Na) NbO 3the Curie temperature of pottery up to 400 ℃, is expected to realize the application of the high performance device under hot conditions.The electrical property of the KNN base orientation leadless piezoelectric ceramics that the people such as SaitoY successfully develop can compare favourably with PZT, and then creates the researching value of KNN base piezoelectric ceramic.Certainly, NaNbO 3-KNbO 3system pottery becomes again the research object getting most of the attention.
The performance of potassium-sodium niobate is with its purity, particle shape, particle size and distribute relevant.Therefore, wish to obtain high purity, as far as possible little particle size and the particle of high-compactness.For this purpose, in succession adopted chemical precipitation method, sol-gel method, above method or complicated operation, or be exactly complex process, the cycle is long, poor repeatability.By contrast, hydrothermal method has the some superiority of synthetic potassium-sodium niobate, so be the method that most of researcher adopts, but traditional hydrothermal method cannot be avoided problem: because the binding ability of K, two kinds of ions of Na and Nb differs too large, if synthetic by traditional one step hydro thermal method, (K, Na) NbO often 3the not out existence of K of fundamental presentation in powder; But adopt NaNbO 3, KNbO 3separately synthetic remix, if mix in washing process, (K, Na) NbO 3potassium, sodium than at all, can not control accurately; If by the NaNbO preparing 3, KNbO 3powder metage mixes, although can also guarantee accurate potassium, sodium ratio, but after facing mixing, uniformity coefficient cannot ensure.
Summary of the invention
The object of the invention is to solve problems of the prior art, provide a kind of material composition proportion speed, grain-size is little and the synthetic leadless piezo-electric ceramic K of even, purity is high two one-step hydrothermals 0.65na 0.35nbO 3the method of powder.
Technical scheme of the present invention is:
Comprise the following steps:
The first step: add Niobium Pentxoxide respectively in potassium hydroxide solution and sodium hydroxide solution, wherein the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide is (2～24): 1, stir and form uniform KNbO 3precursor liquid and NaNbO 3precursor liquid, by KNbO 3precursor liquid and NaNbO 3precursor liquid seals respectively and carries out Hydrothermal Synthesis, after having reacted, obtains powder, finally powder is washed respectively, dries and obtain KNbO 3powder and NaNbO 3powder;
Second step: through grinding technics, get KNbO by the required stoichiometric ratio of preparing powder 3, NaNbO 3powder mixes and seals and carries out Hydrothermal Synthesis in water, after having reacted, obtains mixing solutions, is dried and both obtains leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
The concentration of described potassium hydroxide solution and sodium hydroxide solution is 3～12mol/L.
In the described the first step, stir is to use magnetic stirring apparatus to stir 30～70min.
Hydrothermal synthesis reaction in the described the first step is by KNbO 3precursor liquid and NaNbO 3precursor liquid is sealed in respectively in hydrothermal reaction kettle, at the temperature of 180～220 ℃, is incubated 6～10h, has reacted cool to room temperature.
The compactedness of described hydrothermal reaction kettle is 65～90%.
KNbO in described second step 3, NaNbO 3powder mixes and refers in water, uses magnetic stirrer 30～80min, re-uses microwave concussion 30～80min.
Described second step hydrothermal synthesis reaction is by KNbO 3, NaNbO 3powder is sealed in hydrothermal reaction kettle after mixing in water, at the temperature of 180～220 ℃, is incubated 2～6h, has reacted cool to room temperature.
The leadless piezo-electric ceramic K that described second step obtains 0.65na 0.35nbO 3powder is through washing and oven dry.
Described washing, for using deionized water rinsing to neutral, is dried as being incubated 20～26h at 70～110 ℃.
In described hydrothermal synthesis reaction, hydrothermal reaction kettle is placed in to thermostat container.
Compared with prior art, the present invention has following useful technique effect:
Leadless piezo-electric ceramic K prepared by the present invention 0.65na 0.35nbO 3powder, by usining excessive potassium hydroxide solution and sodium hydroxide solution as potassium source, sodium source, forms precursor liquid with Niobium Pentxoxide respectively, through hydrothermal synthesis reaction, obtains KNbO 3powder and NaNbO 3powder, effectively avoids K, two kinds of ions of Na inaccurate from the different composition proportion that cause of binding ability of Nb; And through washing and dry, make powder purity high, inclusion-free impact; According to required material, can adjust got KNbO again 3, NaNbO 3powder mol ratio, gets two kinds and is dissolved in distilled water through the powder grinding, and can accurately control the mol ratio of powder, and through grinding, diameter of particle is less, is convenient to mix in liquor, makes it carry out hydrothermal synthesis reaction and obtains leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder, the present invention at least has the following advantages: have preparation technology reproducible; Material composition proportion speed; Through grinding physically, and intermediate water thermal response makes mixed powder effectively ensure uniformity coefficient, and prepared powder has very high purity, grain-size is little and even; Not containing hazardous compounds such as Pb, meet the requirement that environment-friendly electronic material is manufactured.
Further, in second step, use magnetic agitation and microwave oscillation that powder is mixed more fully in water, make the leadless piezo-electric ceramic K obtaining 0.65na 0.35nbO 3powder is more even.
Accompanying drawing explanation
Fig. 1 is the leadless piezo-electric ceramic K of being prepared by the embodiment of the present invention 3 0.65na 0.35nbO 3the X-ray diffraction of powder (XRD) figure;
Fig. 2 is the leadless piezo-electric ceramic K of being prepared by the embodiment of the present invention 3 0.65na 0.35nbO 3the SEM figure of powder.
Embodiment
The present invention includes following steps:
The first step, KNbO 3, NaNbO 3synthesizing of powder
(1) get the potassium hydroxide solution that 20mL concentration is 3～12mol/L, get the sodium hydroxide solution that 20mL concentration is 3～12mol/L;
(2) in potassium hydroxide solution, sodium hydroxide solution, add separately 0.01～0.03mol Niobium Pentxoxide, the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide is (2～24): 1; Use magnetic stirring apparatus, stir 30～70min, form uniform KNbO 3precursor liquid, NaNbO 3precursor liquid; By KNbO 3precursor liquid, NaNbO 3precursor liquid is poured into respectively in different hydrothermal reaction kettles, and controlling compactedness is 65～90%, puts into thermostat container and at 180～220 ℃, be incubated 6～10h and carry out Hydrothermal Synthesis after sealing;
(3) question response completes and is cooled to room temperature, and the material in taking-up hydrothermal reaction kettle, is dried at 70～110 ℃ of insulation 20～26h with deionized water rinsing to neutrality, obtains KNbO 3, NaNbO 3two kinds of powders.
Second step: leadless piezo-electric ceramic K 0.65na 0.35nbO 3synthesizing of powder
(1) by KNbO 3, NaNbO 3two kinds of powders, through grinding technics, weigh KNbO for 0.65:0.35 in molar ratio accurately 3, NaNbO 3powder mixes in deionized water; Use magnetic stirrer 30～80min; Re-use the precursor liquid that microwave concussion 30～80min obtains mixing, the uniform precursor liquid of physical mixed is poured in hydrothermal reaction kettle and sealing; Put into and in thermostat container, at 180～220 ℃, be incubated 2～6h and carry out Hydrothermal Synthesis;
(2) question response completes and is cooled to room temperature, after the dry materials in taking-up hydrothermal reaction kettle, obtains powder, with deionized water rinsing, to neutrality, at 70～110 ℃ of insulation 20～26h, dries, and obtains leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
In the present invention, can, according to required material, adjust the KNbO getting 3, NaNbO 3powder mol ratio, is converted to grams by mol ratio, can accurate weighing; This experiment need to make K 0.65na 0.35nbO 3powder, so get KNbO 3, NaNbO 3mol ratio is 0.65:0.35.
Embodiment 1
The first step, KNbO 3, NaNbO 3synthesizing of powder
(1) get the potassium hydroxide solution that 20mL concentration is 3mol/L, get the sodium hydroxide solution that 20mL concentration is 3mol/L;
(2) in potassium hydroxide solution, sodium hydroxide solution, add separately 0.03mol Niobium Pentxoxide, make the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 2:1; Use magnetic stirring apparatus, stir 30min, form uniform KNbO 3precursor liquid, NaNbO 3precursor liquid; By KNbO 3precursor liquid, NaNbO 3precursor liquid is poured into respectively in different hydrothermal reaction kettles, and controlling compactedness is 90%, puts into thermostat container and at 180 ℃, be incubated 10h and carry out Hydrothermal Synthesis after sealing;
(3) be cooled to room temperature, the material in taking-up hydrothermal reaction kettle, is dried at 70 ℃ of insulation 26h with deionized water rinsing to neutrality, obtains KNbO 3, NaNbO 3two kinds of powders.
Second step: leadless piezo-electric ceramic K 0.65na 0.35nbO 3synthesizing of powder
(1) by KNbO 3, NaNbO 3two kinds of powders, through grinding technics, weigh KNbO for 0.65:0.35 in molar ratio accurately 3, NaNbO 3powder mixes in deionized water; Use magnetic stirrer 50min; Re-use the precursor liquid that microwave concussion 50min obtains mixing, the uniform precursor liquid of physical mixed is poured in hydrothermal reaction kettle and sealing; Put into and in thermostat container, at 185 ℃, be incubated 4.5h and carry out Hydrothermal Synthesis;
(2) be cooled to room temperature, after the dry materials in taking-up hydrothermal reaction kettle, obtain powder, with deionized water rinsing, to neutrality, at 100 ℃ of insulation 23h, dry, obtain leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
Embodiment 2
The first step, KNbO 3, NaNbO 3synthesizing of powder
(1) get the potassium hydroxide solution that 20mL concentration is 4mol/L, get the sodium hydroxide solution that 20mL concentration is 4mol/L;
(2) in potassium hydroxide solution, sodium hydroxide solution, add separately 0.02mol Niobium Pentxoxide, make the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 4:1; Use magnetic stirring apparatus, stir 40min, form uniform KNbO 3precursor liquid, NaNbO 3precursor liquid; By KNbO 3precursor liquid, NaNbO 3precursor liquid is poured into respectively in different hydrothermal reaction kettles, and controlling compactedness is 65%, puts into thermostat container and at 220 ℃, be incubated 8h and carry out Hydrothermal Synthesis after sealing;
(3) be cooled to room temperature, the material in taking-up hydrothermal reaction kettle, is dried at 80 ℃ of insulation 25h with deionized water rinsing to neutrality, obtains KNbO 3, NaNbO 3two kinds of powders.
Second step: leadless piezo-electric ceramic K 0.65na 0.35nbO 3synthesizing of powder
(1) by KNbO 3, NaNbO 3two kinds of powders, through grinding technics, weigh KNbO for 0.65:0.35 in molar ratio accurately 3, NaNbO 3powder mixes in deionized water; Use magnetic stirrer 60min; Re-use the precursor liquid that microwave concussion 60min obtains mixing, the uniform precursor liquid of physical mixed is poured in hydrothermal reaction kettle and sealing; Put into and in thermostat container, at 190 ℃, be incubated 6h and carry out Hydrothermal Synthesis;
(2) be cooled to room temperature, after the dry materials in taking-up hydrothermal reaction kettle, obtain powder, with deionized water rinsing, to neutrality, at 110 ℃ of insulation 22h, dry, obtain leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
Embodiment 3
The first step, KNbO 3, NaNbO 3synthesizing of powder
(1) get the potassium hydroxide solution that 20mL concentration is 6mol/L, get the sodium hydroxide solution that 20mL concentration is 6mol/L;
(2) in potassium hydroxide solution, sodium hydroxide solution, add separately 0.01mol Niobium Pentxoxide, make the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 12:1; Use magnetic stirring apparatus, stir 50min, form uniform KNbO 3precursor liquid, NaNbO 3precursor liquid; By KNbO 3precursor liquid, NaNbO 3precursor liquid is poured into respectively in different hydrothermal reaction kettles, and controlling compactedness is 70%, puts into thermostat container and at 210 ℃, be incubated 6h and carry out Hydrothermal Synthesis after sealing;
(3) be cooled to room temperature, the material in taking-up hydrothermal reaction kettle, is dried at 90 ℃ of insulation 24h with deionized water rinsing to neutrality, obtains KNbO 3, NaNbO 3two kinds of powders.
Second step: leadless piezo-electric ceramic K 0.65na 0.35nbO 3synthesizing of powder
(1) by KNbO 3, NaNbO 3two kinds of powders, through grinding technics, weigh KNbO for 0.65:0.35 in molar ratio accurately 3, NaNbO 3powder mixes in deionized water; Use magnetic stirrer 70min; Re-use the precursor liquid that microwave concussion 30min obtains mixing, the uniform precursor liquid of physical mixed is poured in hydrothermal reaction kettle and sealing; Put into and in thermostat container, at 180 ℃, be incubated 5h and carry out Hydrothermal Synthesis;
(2) be cooled to room temperature, after the dry materials in taking-up hydrothermal reaction kettle, obtain powder, with deionized water rinsing, to neutrality, at 95 ℃ of insulation 20h, dry, obtain leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
Embodiment 4
The first step, KNbO 3, NaNbO 3synthesizing of powder
(1) get the potassium hydroxide solution that 20mL concentration is 10mol/L, get the sodium hydroxide solution that 20mL concentration is 10mol/L;
(2) in potassium hydroxide solution, sodium hydroxide solution, add separately 0.01mol Niobium Pentxoxide, make the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 20:1; Use magnetic stirring apparatus, stir 60min, form uniform KNbO 3precursor liquid, NaNbO 3precursor liquid; By KNbO 3precursor liquid, NaNbO 3precursor liquid is poured into respectively in different hydrothermal reaction kettles, and controlling compactedness is 80%, puts into thermostat container and at 200 ℃, be incubated 7h and carry out Hydrothermal Synthesis after sealing;
(3) be cooled to room temperature, the material in taking-up hydrothermal reaction kettle, is dried at 100 ℃ of insulation 23h with deionized water rinsing to neutrality, obtains KNbO 3, NaNbO 3two kinds of powders.
Second step: leadless piezo-electric ceramic K 0.65na 0.35nbO 3synthesizing of powder
(1) by KNbO 3, NaNbO 3two kinds of powders, through grinding technics, weigh KNbO for 0.65:0.35 in molar ratio accurately 3, NaNbO 3powder mixes in deionized water; Use magnetic stirrer 80min; Re-use the precursor liquid that microwave concussion 40min obtains mixing, the uniform precursor liquid of physical mixed is poured in hydrothermal reaction kettle and sealing; Put into and in thermostat container, at 220 ℃, be incubated 3h and carry out Hydrothermal Synthesis;
(2) be cooled to room temperature, after the dry materials in taking-up hydrothermal reaction kettle, obtain powder, with deionized water rinsing, to neutrality, at 70 ℃ of insulation 26h, dry, obtain leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
Embodiment 5
The first step, KNbO 3, NaNbO 3synthesizing of powder
(1) get the potassium hydroxide solution that 20mL concentration is 12mol/L, get the sodium hydroxide solution that 20mL concentration is 12mol/L;
(2) in potassium hydroxide solution, sodium hydroxide solution, add separately 0.01mol Niobium Pentxoxide, make the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 24:1; Use magnetic stirring apparatus, stir 70min, form uniform KNbO 3precursor liquid, NaNbO 3precursor liquid; By KNbO 3precursor liquid, NaNbO 3precursor liquid is poured into respectively in different hydrothermal reaction kettles, and controlling compactedness is 85%, puts into thermostat container and at 190 ℃, be incubated 9h and carry out Hydrothermal Synthesis after sealing;
(3) be cooled to room temperature, the material in taking-up hydrothermal reaction kettle, is dried at 110 ℃ of insulation 22h with deionized water rinsing to neutrality, obtains KNbO 3, NaNbO 3two kinds of powders.
Second step: leadless piezo-electric ceramic K 0.65na 0.35nbO 3synthesizing of powder
(1) by KNbO 3, NaNbO 3two kinds of powders, through grinding technics, weigh KNbO for 0.65:0.35 in molar ratio accurately 3, NaNbO 3powder mixes in deionized water; Use magnetic stirrer 30min; Re-use the precursor liquid that microwave concussion 70min obtains mixing, the uniform precursor liquid of physical mixed is poured in hydrothermal reaction kettle and sealing; Put into and in thermostat container, at 210 ℃, be incubated 2h and carry out Hydrothermal Synthesis;
(2) be cooled to room temperature, after the dry materials in taking-up hydrothermal reaction kettle, obtain powder, with deionized water rinsing, to neutrality, at 80 ℃ of insulation 25h, dry, obtain leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
Embodiment 6
The first step, KNbO 3, NaNbO 3synthesizing of powder
(1) get the potassium hydroxide solution that 20mL concentration is 8mol/L, get the sodium hydroxide solution that 20mL concentration is 6mol/L;
(2) in potassium hydroxide solution, sodium hydroxide solution, add separately 0.02mol Niobium Pentxoxide, make the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 6:1; Use magnetic stirring apparatus, stir 60min, form uniform KNbO 3precursor liquid, NaNbO 3precursor liquid; By KNbO 3precursor liquid, NaNbO 3precursor liquid is poured into respectively in different hydrothermal reaction kettles, and controlling compactedness is 75%, puts into thermostat container and at 195 ℃, be incubated 9h and carry out Hydrothermal Synthesis after sealing;
(3) be cooled to room temperature, the material in taking-up hydrothermal reaction kettle, is dried at 95 ℃ of insulation 20h with deionized water rinsing to neutrality, obtains KNbO 3, NaNbO 3two kinds of powders.
Second step: leadless piezo-electric ceramic K 0.65na 0.35nbO 3synthesizing of powder
(1) by KNbO 3, NaNbO 3two kinds of powders, through grinding technics, weigh KNbO for 0.65:0.35 in molar ratio accurately 3, NaNbO 3powder mixes in deionized water; Use magnetic stirrer 40min; Re-use the precursor liquid that microwave concussion 80min obtains mixing, the uniform precursor liquid of physical mixed is poured in hydrothermal reaction kettle and sealing; Put into and in thermostat container, at 200 ℃, be incubated 4h and carry out Hydrothermal Synthesis;
(2) be cooled to room temperature, after the dry materials in taking-up hydrothermal reaction kettle, obtain powder, with deionized water rinsing, to neutrality, at 90 ℃ of insulation 24h, dry, obtain leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
Refer to shown in Fig. 1, by prepared K 0.65na 0.5nbO 3rigaku D/max2000PCX-x ray diffractometer x analytic sample for powder, finds that product is the K that JCPDS is numbered 77-0038 0.65na 0.35nbO 3.
Refer to shown in Fig. 2 the cube K being prepared by the inventive method 0.65na 0.35nbO 3powder, particle surface rule, particle is grown complete, and component is even.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of any equivalence that the logical technician in this area takes technical solution of the present invention by reading specification sheets of the present invention, is claim of the present invention and contains.

Claims (10)

1. an one-step hydrothermal synthesizes leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder, is characterized in that: comprise the following steps:
The first step: add Niobium Pentxoxide respectively in potassium hydroxide solution and sodium hydroxide solution, wherein the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide is (2～24): 1, stir and form uniform KNbO 3precursor liquid and NaNbO 3precursor liquid, by KNbO 3precursor liquid and NaNbO 3precursor liquid seals respectively and carries out Hydrothermal Synthesis, after having reacted, obtains powder, finally powder is washed respectively, dries and obtain KNbO 3powder and NaNbO 3powder;
Second step: through grinding technics, get KNbO by the required stoichiometric ratio of preparing powder 3, NaNbO 3powder mixes and seals and carries out Hydrothermal Synthesis in water, after having reacted, obtains mixing solutions, is dried and both obtains leadless piezo-electric ceramic K 0.65na 0.35nbO 3powder.
2. two one-step hydrothermals according to claim 1 synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder, is characterized in that: the concentration of described potassium hydroxide solution and sodium hydroxide solution is 3～12mol/L.
3. two one-step hydrothermals according to claim 1 synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder, is characterized in that: in the described the first step, stirring is to use magnetic stirring apparatus to stir 30～70min.
4. according to the synthetic leadless piezo-electric ceramic K of two one-step hydrothermals described in claim 1-3 any one 0.65na 0.35nbO 3the method of powder, is characterized in that: the hydrothermal synthesis reaction in the described the first step is by KNbO 3precursor liquid and NaNbO 3precursor liquid is sealed in respectively in hydrothermal reaction kettle, at the temperature of 180～220 ℃, is incubated 6～10h, has reacted cool to room temperature.
5. two one-step hydrothermals according to claim 4 synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder, is characterized in that: the compactedness of described hydrothermal reaction kettle is 65～90%.
6. two one-step hydrothermals according to claim 1 synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder, is characterized in that: the KNbO in described second step 3, NaNbO 3powder mixes and refers in water, uses magnetic stirrer 30～80min, re-uses microwave concussion 30～80min.
7. according to the synthetic leadless piezo-electric ceramic K of two one-step hydrothermals described in claim 1 or 6 0.65na 0.35nbO 3the method of powder, is characterized in that: described second step hydrothermal synthesis reaction is by KNbO 3, NaNbO 3powder is sealed in hydrothermal reaction kettle after mixing in water, at the temperature of 180～220 ℃, is incubated 2～6h, has reacted cool to room temperature.
8. two one-step hydrothermals according to claim 7 synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder, is characterized in that: the leadless piezo-electric ceramic K that described second step obtains 0.65na 0.35nbO 3powder is through washing and oven dry.
9. two one-step hydrothermals according to claim 8 synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder, is characterized in that: described washing, for using deionized water rinsing to neutral, is dried as being incubated 20～26h at 70～110 ℃.
10. two one-step hydrothermals according to claim 9 synthesize leadless piezo-electric ceramic K 0.65na 0.35nbO 3the method of powder, is characterized in that: in described hydrothermal synthesis reaction, hydrothermal reaction kettle is placed in to thermostat container.
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CN110217821A (en) * 2019-07-02 2019-09-10 华南理工大学 A kind of method that solid phase-hydro-thermal method prepares cubic potassium-sodium niobate nano particle
CN115924970A (en) * 2022-09-19 2023-04-07 济南大学 Potassium niobate nanowire and preparation method thereof

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