CN104119078A - Method for preparing KNN (K, Na, Nb) series low-loss leadless piezoelectric ceramic - Google Patents
Method for preparing KNN (K, Na, Nb) series low-loss leadless piezoelectric ceramic Download PDFInfo
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Abstract
The invention belongs to the technical field of piezoelectric ceramic preparation, and in particular relates to a method for preparing KNN (K, Na, Nb) series low-loss leadless piezoelectric ceramic. The method comprises the following steps: by respectively taking potassium hydroxide and sodium hydroxide as a potassium source and a sodium source, and taking the superfluous components as precursors, respectively adding niobium pentoxide into solutions, so as to prepare powder of KNbO3 and NaNbO3; precisely weighing certain grams of the powder of KNbO3 and NaNbO3, performing hydrothermal reaction twice, after the reaction is completed, sufficiently drying an obtained mixed liquid so as to obtain powder, and calcining the powder, thereby preparing the ceramic. According to the method, a two-step hydrothermal method is adopted, the preparation process is good in process repeatability, the material components are accurately distributed, and the prepared KNN series low-loss leadless piezoelectric ceramic is high in purity.
Description
Technical field
The invention belongs to piezoelectric ceramics preparing technical field, be specifically related to a kind of KNN series lead-free piezoelectric ceramic preparation method.
Background technology
Piezoelectric is to realize the class critical function material that mechanical energy and electric energy are changed mutually, aspect the various electronic devices and components such as sensor, driving mechanism, ultrasonic transducer, resonator, wave filter, hummer and ignition, is having a wide range of applications.A large amount of piezoelectric ceramics that use are mainly leaded systems at present, as Pb (Mg
1/3nb
2/3) O
3-PbTiO
3(being called for short PMN-PT) or Pb (Zr, Ti) O
3(being called for short PZT) etc.(or the Pb of PbO in these stupaliths
3o
4) content account for 60% left and right.Plumbous toxicity make lead base piezoelectric ceramics produce, use and discarded after treating processes in cause serious harm to the mankind and ecotope, the Sustainable development of this and human society is runed counter to; Simultaneous oxidation lead is volatile, needs sealed sintering in preparation process, has not only increased product cost, has also caused the consistency of performance of product poor.Therefore researching and developing leadless piezoelectric ceramics is a problem that has great social effect and economic implications.
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 day by day.Than lead base piezoelectric ceramics such as PZT, KNN series lead-free piezoelectric ceramic everyway has more excellent performance, and 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.
The performance optimization of potassium-sodium niobate, normally by the method such as solid solution, doping, changes the structure of its intracell; And this case is to optimize by the deep to preparation technology, improve its purity; Thereby reduction dielectric loss, improves performance.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, often (K, Na) NbO
3the not out existence of K of fundamental presentation in powder, this is that traditional hydrothermal method existence cannot be avoided problem; If simple employing divides one-step hydrothermal, by NaNbO
3, KNbO
3separately synthetic remix, closes NaNbO if carry out wet mixing with the state of solution in washing process
3, KNbO
3can mix fully, but synthetic (K, Na) NbO
3in potassium, sodium ratio can not accurately control; Again or will prepare dry NaNbO
3, KNbO
3powder is dry blending after accurate weighing, although can also ensure accurate potassium, the accuracy of sodium ratio, but after facing mixing, uniformity coefficient cannot ensure.
Summary of the invention
The object of the invention is to the defect and the deficiency that exist for prior art, provide a kind of preparation technology reproducible, material composition proportion speed, the KNN that purity is high is low-loss leadless piezoelectric ceramics preparation method.
For achieving the above object, the present invention by the following technical solutions: comprise the following steps,
Step 1, gets respectively potassium hydroxide solution A and sodium hydroxide solution B that concentration is 4～10mol/L;
Step 2 adds Niobium Pentxoxide respectively in A, B, the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide is (8～20): 1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are carried out respectively to hydro-thermal reaction, and the temperature of hydro-thermal reaction is 180～220 DEG C, and the time is 6～10h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B, and with deionized water rinsing, to neutral, then drying and processing obtains powder A, powder B;
Step 4, to powder A, powder B milled processed, gets xmol powder A respectively, and ymol powder B mixes in deionized water, stirs and obtains mixing precursor liquid C; Mixing precursor liquid C is incubated to 4～6h at 180～220 DEG C and carries out Hydrothermal Synthesis; Wherein the mol ratio of powder A, powder B is x:y=(1:9)～(9:1);
Step 5, is used deionized water rinsing to neutral mixing precursor liquid C after Hydrothermal Synthesis, dries and obtains powder C, obtains KNN series lead-free piezoelectric ceramic 1200～1300 DEG C of calcinings.
Further, described in step 2, in A, B, add separately the amount of Niobium Pentxoxide to be 0.01mol.
Further, precursor liquid is put into hydrothermal reaction kettle, and compactedness is 80%, after sealing, puts into thermostat container and carry out hydro-thermal reaction.
Further, stir and use magnetic stirring apparatus described in step 4, the time is 30～60min.
Further, after stirring described in step 4, use microwave concussion to process, the time is 60min.
Further, in microwave sintering retort furnace, in 1h, evenly rise to 900 DEG C by room temperature, insulation 10min; Then in 30min, evenly rise to 1200～1300 DEG C by 900 DEG C, insulation 5min; Cool to room temperature with the furnace.
Further, the condition of drying and processing is 60～80 DEG C described in step 3,5,12～24h.
Compared with prior art, the present invention is by first using potassium hydroxide and sodium hydroxide to carry out hydro-thermal reaction with Niobium Pentxoxide respectively, prepare powder A, powder B, re-use powder A, B preparation mixing precursor liquid and carry out hydro-thermal reaction, by two step hydro-thermal reactions, ensure the accurate control to potassium, sodium ratio, made (K, Na) NbO of preparation
3uniformity coefficient is higher; And preparation technology is simple, reproducible, contrast by the piezoelectric ceramics of preparing with existing one step hydro thermal method, dielectric loss is obviously lower, and the KNN of preparation is that low-loss leadless piezoelectric ceramics purity is high.
Brief description of the drawings
Fig. 1 is that KNN prepared by the embodiment of the present invention 2 supplying methods is low-loss leadless piezo-electric ceramic K
0.65na
0.35nbO
3with the K through two step hydrothermal treatment consists not
0.65na
0.35nbO
3pottery X-ray diffraction comparison diagram;
Fig. 2 is that KNN prepared by the embodiment of the present invention 2 supplying methods is low-loss leadless piezo-electric ceramic K
0.65na
0.35nbO
3with the K through two step hydrothermal treatment consists not
0.65na
0.35nbO
3the temperature variant contrast collection of illustrative plates of dielectric loss of pottery.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail.
A kind of KNN provided by the invention is low-loss leadless piezoelectric ceramics preparation method, comprises the following steps,
Step 1, gets respectively potassium hydroxide solution A and sodium hydroxide solution B that concentration is 4～10mol/L;
Step 2 adds separately 0.01mol Niobium Pentxoxide respectively in A, B, the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide is (8～20): 1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are put into respectively to hydrothermal reaction kettle and carry out hydro-thermal reaction, and to control compactedness be 80%, the temperature of hydro-thermal reaction is 180～220 DEG C, and the time is 6～10h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B,, then at 60～80 DEG C, dries 12～24h and obtains powder A, powder B to neutral with deionized water rinsing;
Step 4, to powder A, powder B milled processed, gets powder A, x=0.1～0.9mol respectively, powder B, 1-xmol mixes in deionized water, use magnetic stirring apparatus, stir the mixing precursor liquid C that 30～60min obtains stirring, re-use microwave concussion and process 60min; Then mixing precursor liquid C is incubated to 4～6h at 180～220 DEG C and carries out Hydrothermal Synthesis.
Step 5, is used deionized water rinsing to neutral mixing precursor liquid C after Hydrothermal Synthesis, dries 12～24h and obtain powder C at 60～80 DEG C, in microwave sintering retort furnace, in 1h, evenly rises to 900 DEG C by room temperature, insulation 10min; Then in 30min, evenly rise to 1200～1300 DEG C by 900 DEG C, insulation 5min; Cool to room temperature with the furnace, obtain (K, Na) NbO
3(KNN) series lead-free piezoelectric ceramic.
Embodiment 1
Step 1, getting concentration is the potassium hydroxide solution A of 4mol/L and the sodium hydroxide homogeneous solution B that concentration is 4mol/L;
Step 2 adds separately 0.01mol Niobium Pentxoxide respectively in potassium hydroxide solution A, sodium hydroxide solution B, makes the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 8:1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are put into respectively to hydrothermal reaction kettle and carry out hydro-thermal reaction, and to control compactedness be 80%, the temperature of hydro-thermal reaction is 200 DEG C, and the time is 8h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B,, then at 60 DEG C, dries 24h and obtains powder A, powder B to neutral with deionized water rinsing;
Step 4, to powder A, powder B milled processed, gets 0.1mol powder A respectively, and 0.9mol powder B mixes in deionized water, uses magnetic stirring apparatus, stirs the mixing precursor liquid C that 60min obtains stirring, and re-uses microwave concussion and processes 60min; Then mixing precursor liquid C is incubated to 4h at 200 DEG C and carries out Hydrothermal Synthesis.
Step 5, is used deionized water rinsing to neutral mixing precursor liquid C after Hydrothermal Synthesis, dries 24h and obtain powder C at 60 DEG C, in microwave sintering retort furnace, in 1h, evenly rises to 900 DEG C by room temperature, insulation 10min; 30min evenly rises to 1255 DEG C by 900 DEG C, and insulation 5min, obtains K
0.1na
0.9nbO
3series lead-free piezoelectric ceramic.
Embodiment 2
Step 1, getting concentration is the potassium hydroxide solution A of 6mol/L and the sodium hydroxide homogeneous solution B that concentration is 6mol/L;
Step 2 adds separately 0.01mol Niobium Pentxoxide respectively in potassium hydroxide solution A, sodium hydroxide solution B, makes the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 12:1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are put into respectively to hydrothermal reaction kettle and carry out hydro-thermal reaction, and to control compactedness be 80%, the temperature of hydro-thermal reaction is 180 DEG C, and the time is 10h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B,, then at 60 DEG C, dries 20h and obtains powder A, powder B to neutral with deionized water rinsing;
Step 4, to powder A, powder B milled processed, gets 0.65mol powder A respectively, and 0.35mol powder B mixes in deionized water, uses magnetic stirring apparatus, stirs the mixing precursor liquid C that 60min obtains stirring, and re-uses microwave concussion and processes 60min; Then mixing precursor liquid C is divided into D, E two portions, D convection drying; E pours in hydrothermal reaction kettle and sealing; Put into and in thermostat container, at 200 DEG C, be incubated 4h and carry out Hydrothermal Synthesis.
Step 5, is used deionized water rinsing to neutral mixing precursor liquid E after Hydrothermal Synthesis, dries 24h and obtain powder C at 60 DEG C, in microwave sintering retort furnace, in 1h, evenly rises to 900 DEG C by room temperature, insulation 10min; 30min evenly rises to 1200 DEG C by 900 DEG C, and insulation 5min, obtains K
0.65na
0.35nbO
3series lead-free piezoelectric ceramic.
Referring to Fig. 1, Fig. 2, the K being prepared by mixing precursor liquid E in the present embodiment
0.65na
0.35nbO
3the performance of pottery is obviously better than the K preparing by mixing precursor liquid D convection drying
0.65na
0.35nbO
3pottery.
Embodiment 3
Step 1, getting concentration is the potassium hydroxide solution A of 8mol/L and the sodium hydroxide homogeneous solution B that concentration is 8mol/L;
Step 2 adds separately 0.01mol Niobium Pentxoxide respectively in potassium hydroxide solution A, sodium hydroxide solution B, makes the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 10:1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are put into respectively to hydrothermal reaction kettle and carry out hydro-thermal reaction, and to control compactedness be 80%, the temperature of hydro-thermal reaction is 220 DEG C, and the time is 6h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B,, then at 80 DEG C, dries 12h and obtains powder A, powder B to neutral with deionized water rinsing;
Step 4, to powder A, powder B milled processed, gets 0.5mol powder A respectively, and 0.5mol powder B mixes in deionized water, uses magnetic stirring apparatus, stirs the mixing precursor liquid C that 30min obtains stirring, and re-uses microwave concussion and processes 60min; Then mixing precursor liquid C is incubated to 4h at 220 DEG C and carries out Hydrothermal Synthesis.
Step 5, is used deionized water rinsing to neutral mixing precursor liquid C after Hydrothermal Synthesis, dries 24h and obtain powder C at 60 DEG C, in microwave sintering retort furnace, in 1h, evenly rises to 900 DEG C by room temperature, insulation 10min; 30min evenly rises to 1300 DEG C by 900 DEG C, and insulation 5min, obtains K
0.5na
0.5nbO
3series lead-free piezoelectric ceramic.
Embodiment 4
Step 1, getting concentration is the potassium hydroxide solution A of 10mol/L and the sodium hydroxide homogeneous solution B that concentration is 10mol/L;
Step 2 adds separately 0.01mol Niobium Pentxoxide respectively in potassium hydroxide solution A, sodium hydroxide solution B, makes the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 16:1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are put into respectively to hydrothermal reaction kettle and carry out hydro-thermal reaction, and to control compactedness be 80%, the temperature of hydro-thermal reaction is 190 DEG C, and the time is 9h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B,, then at 70 DEG C, dries 20h and obtains powder A, powder B to neutral with deionized water rinsing;
Step 4, to powder A, powder B milled processed, gets 0.35mol powder A respectively, and 0.65mol powder B mixes in deionized water, uses magnetic stirring apparatus, stirs the mixing precursor liquid C that 50min obtains stirring, and re-uses microwave concussion and processes 60min; Then mixing precursor liquid C is incubated to 5h at 190 DEG C and carries out Hydrothermal Synthesis.
Step 5, is used deionized water rinsing to neutral mixing precursor liquid C after Hydrothermal Synthesis, dries 24h and obtain powder C at 65 DEG C, in microwave sintering retort furnace, in 1h, evenly rises to 900 DEG C by room temperature, insulation 10min; 30min evenly rises to 1200 DEG C by 900 DEG C, and insulation 5min, obtains K
0.35na
0.65nbO
3series lead-free piezoelectric ceramic.
Embodiment 5
Step 1, getting concentration is the potassium hydroxide solution A of 4mol/L and the sodium hydroxide homogeneous solution B that concentration is 4mol/L;
Step 2 adds separately 0.01mol Niobium Pentxoxide respectively in potassium hydroxide solution A, sodium hydroxide solution B, makes the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 20:1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are put into respectively to hydrothermal reaction kettle and carry out hydro-thermal reaction, and to control compactedness be 80%, the temperature of hydro-thermal reaction is 180 DEG C, and the time is 9h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B,, then at 70 DEG C, dries 18h and obtains powder A, powder B to neutral with deionized water rinsing;
Step 4, to powder A, powder B milled processed, gets 0.9mol powder A respectively, and 0.1mol powder B mixes in deionized water, uses magnetic stirring apparatus, stirs the mixing precursor liquid C that 40min obtains stirring, and re-uses microwave concussion and processes 60min; Then mixing precursor liquid C is incubated to 4h at 200 DEG C and carries out Hydrothermal Synthesis.
Step 5, is used deionized water rinsing to neutral mixing precursor liquid C after Hydrothermal Synthesis, dries 24h and obtain powder C at 60 DEG C, in microwave sintering retort furnace, in 1h, evenly rises to 900 DEG C by room temperature, insulation 10min; 30min evenly rises to 1250 DEG C by 900 DEG C, and insulation 5min, obtains K
0.9na
0.1nbO
3series lead-free piezoelectric ceramic.
Embodiment 6
Step 1, getting concentration is the potassium hydroxide solution A of 5mol/L and the sodium hydroxide homogeneous solution B that concentration is 5mol/L;
Step 2 adds separately 0.01mol Niobium Pentxoxide respectively in potassium hydroxide solution A, sodium hydroxide solution B, makes the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide be 17:1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are put into respectively to hydrothermal reaction kettle and carry out hydro-thermal reaction, and to control compactedness be 80%, the temperature of hydro-thermal reaction is 190 DEG C, and the time is 8h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B,, then at 80 DEG C, dries 16h and obtains powder A, powder B to neutral with deionized water rinsing;
Step 4, to powder A, powder B milled processed, gets 0.2mol powder A respectively, and 0.8mol powder B mixes in deionized water, uses magnetic stirring apparatus, stirs the mixing precursor liquid C that 50min obtains stirring, and re-uses microwave concussion and processes 60min; Then mixing precursor liquid C is incubated to 4h at 210 DEG C and carries out Hydrothermal Synthesis.
Step 5, is used deionized water rinsing to neutral mixing precursor liquid C after Hydrothermal Synthesis, dries 20h and obtain powder C at 70 DEG C, in microwave sintering retort furnace, in 1h, evenly rises to 900 DEG C by room temperature, insulation 10min; 30min evenly rises to 1230 DEG C by 900 DEG C, and insulation 5min, obtains K
0.2na
0.8nbO
3series lead-free piezoelectric ceramic.
Consult Fig. 1, by prepared K
0.65na
0.35nbO
3rigaku D/max2000PC x-ray diffractometer analytic sample for pottery, finds that product is the K that JCPDS is numbered 77-0038
0.65na
0.35nbO
3.Fig. 1 (a) is for dividing an one-step hydrothermal to prepare KNbO
3, NaNbO
3after powder through stirring, concussion etc. fully after physical mixed, K prepared by sintering
0.65na
0.35nbO
3pottery, wherein has miscellaneous K
3nbO
4, NbO
2.46, this is the inhomogeneous presentation directly perceived of physical mixed; Fig. 1 (b) is for dividing an one-step hydrothermal to prepare KNbO
3, NaNbO
3after powder through the fully physical mixed such as stirring, concussion, after two one-step hydrothermals, K prepared by sintering
0.65na
0.35nbO
3pottery, XRD characterizes pure phase.
Consult Fig. 2, Fig. 1 (a) is for dividing an one-step hydrothermal to prepare KNbO
3, NaNbO
3after powder through stirring, concussion etc. fully after physical mixed, K prepared by sintering
0.65na
0.35nbO
3pottery; Fig. 1 (b) is for dividing an one-step hydrothermal to prepare KNbO
3, NaNbO
3after powder through the fully physical mixed such as stirring, concussion, after two one-step hydrothermals, K prepared by sintering
0.65na
0.35nbO
3pottery.The K that the inventive method prepares can be described thus
0.65na
0.35nbO
3leadless piezoelectric ceramics dielectric loss decreases.
The present invention adopts two one-step hydrothermals to prepare K
0.65na
0.35nbO
3pottery, improves the unavoidable technological difficulties of traditional hydrothermal method: 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, often (K, Na) NbO
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 can not control accurately than at all; If by the NaNbO preparing
3, KNbO
3powder metage mixes, although can also ensure accurate potassium, sodium ratio, but after facing mixing, uniformity coefficient cannot ensure.Adopt in the present invention two one-step hydrothermals, preparation technology is reproducible, material composition proportion speed, and purity is high, the preparation method of low-loss KNN leadless piezoelectric ceramics.
Claims (7)
1. a KNN series lead-free piezoelectric ceramic preparation method, is characterized in that: comprises the following steps,
Step 1, gets respectively potassium hydroxide solution A and sodium hydroxide solution B that concentration is 4～10mol/L;
Step 2 adds Niobium Pentxoxide respectively in A, B, the mol ratio of potassium hydroxide and Niobium Pentxoxide, sodium hydroxide and Niobium Pentxoxide is (8～20): 1; Stir, form precursor liquid A, precursor liquid B; Precursor liquid A, precursor liquid B are carried out respectively to hydro-thermal reaction, and the temperature of hydro-thermal reaction is 180～220 DEG C, and the time is 6～10h;
Step 3, is cooled to respectively room temperature by the precursor liquid A after hydro-thermal reaction, precursor liquid B, and with deionized water rinsing, to neutral, then drying and processing obtains powder A, powder B;
Step 4, to powder A, powder B milled processed, gets xmol powder A respectively, and ymol powder B mixes in deionized water, stirs and obtains mixing precursor liquid C; Mixing precursor liquid C is incubated to 4～6h at 180～220 DEG C and carries out Hydrothermal Synthesis; Wherein the mol ratio of powder A, powder B is x:y=(1:9)～(9:1);
Step 5, is used deionized water rinsing to neutral mixing precursor liquid C after Hydrothermal Synthesis, dries and obtains powder C, obtains KNN series lead-free piezoelectric ceramic 1200～1300 DEG C of calcinings.
2. according to the inner a kind of KNN series lead-free piezoelectric ceramic preparation method who requires described in 1, it is characterized in that: described in step 2, in A, B, add separately the amount of Niobium Pentxoxide to be 0.01mol.
3. according to the inner a kind of KNN series lead-free piezoelectric ceramic preparation method who requires described in 1, it is characterized in that: described in step 2, the concrete operations of hydro-thermal reaction are: precursor liquid is put into hydrothermal reaction kettle, and compactedness is 80%, after sealing, puts into thermostat container and carry out hydro-thermal reaction.
4. according to the inner a kind of KNN series lead-free piezoelectric ceramic preparation method who requires described in 1, it is characterized in that: described in step 4, stir and use magnetic stirring apparatus, the time is 30～60min.
5. according to the inner a kind of KNN series lead-free piezoelectric ceramic preparation method who requires described in 1 or 4, it is characterized in that: after stirring described in step 4, use microwave concussion to process, the time is 60min.
6. according to the inner a kind of KNN series lead-free piezoelectric ceramic preparation method who requires described in 1, it is characterized in that: described in step 5, the concrete operations of calcining are: in microwave sintering retort furnace, in 1h, evenly rise to 900 DEG C by room temperature, insulation 10min; Then in 30min, evenly rise to 1200～1300 DEG C by 900 DEG C, insulation 5min; Cool to room temperature with the furnace.
7. according to the inner a kind of KNN series lead-free piezoelectric ceramic preparation method who requires described in 1 or 6, it is characterized in that: described in step 3,5, the condition of drying and processing is 60～80 DEG C, 12～24h.
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