CN112898020A - Preparation method of potassium sodium niobate-based nano fine-grained ceramic with average grain size of 160nm - Google Patents
Preparation method of potassium sodium niobate-based nano fine-grained ceramic with average grain size of 160nm Download PDFInfo
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Abstract
The invention relates to a preparation method of potassium sodium niobate-based nano fine crystalline ceramics with the average grain size of 160nm, which can reduce oxygen vacancy generated by volatilization of alkali metal elements and simultaneously obstruct the growth of grains by adding 0.5 mol percent of lanthanum oxide into raw materials, thereby achieving the purpose of refining the grains. Calcining the dried powder after ball milling for 12-18h at the temperature of 800-900 ℃, secondary ball milling for 12-18h, calcining again at the temperature of 800-900 ℃ after drying for 2-4h, then carrying out ball milling for 12-18h for three times and drying, and carrying out ball milling and calcining for many times to fully react and refine the raw materials, so that the sintering temperature and the heat preservation time can be reduced, and the purpose of refining grains due to insufficient grain growth is achieved. The scanning electron microscope image and the particle size distribution diagram of the finally obtained potassium sodium niobate-based ceramic are shown in figure 2 by the doping modification and the improved traditional solid phase method of the rare earth element lanthanum, the average grain size is 160nm, and the grain size distribution is uniform and very fine.
Description
Technical Field
The invention belongs to the field of functional materials, and relates to a preparation method of potassium sodium niobate-based nano fine-grained ceramic with the average grain size of 160 nm.
Background
The properties of a material depend not only on the composition of the material but also on the microstructure of the material. In the past research, the inventor also found that the internal stress, the tetragonal degree, the grain boundary, the phase transition temperature and the like of the material are influenced by changing the grain size of the ceramic material, and further the piezoelectric property, the optical property, the energy storage property, the dielectric property and the like of the material are influenced. The breakdown field strength of the material can be greatly improved by thinning the crystal grains of the ceramic, so that the material has higher energy storage density and stability. In addition, because the grain boundary acts as a barrier to hinder the oxygen vacancy relaxation, the oxygen vacancy of the fine crystalline ceramic is less, and the relaxation activation energy is higher. The fine-grained ceramics can be sintered and formed at a lower temperature, so that the requirement on equipment can be reduced, and the cost is reduced.
In recent years, potassium sodium niobate-based ceramics gradually come into the visual field of people due to the remarkable characteristics of submicron-sized crystal grains, rich phase transition, high dielectric constant, low dielectric loss, large piezoelectric activity and the like. However, the density of the potassium-sodium niobate ceramic prepared by the traditional process is not high, the sintering temperature zone is also narrow, and the performance is greatly limited. Therefore, the method adopts a substituted modification or optimized sintering process to regulate and control the microstructure parameters of the material and improve the performance of the material, and has important research value and practical significance.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation method of potassium sodium niobate-based nano fine-grained ceramic with the average grain size of 160nm, which regulates and controls the microstructure of the material by doping and optimizing a sintering process, further refines the grains of the potassium sodium niobate-based ceramic and ensures that the potassium sodium niobate-based ceramic has good sintering performance.
Technical scheme
A method for preparing potassium sodium niobate-based nano fine crystalline ceramics with the average grain size of 160nm is characterized by comprising the following steps: doping rare earth element lanthanum and adopting an improved solid phase method, and comprises the following steps:
step 1: 3.433g K is weighed according to the proportion of 0.5 mol percent of lanthanum doping amount2CO3、2.637g Na2CO3、13.234g Nb2O5、0.163g La2O3
Step 2: putting the raw material powder into a polytetrafluoroethylene ball milling tank filled with zirconia balls, and carrying out ball milling by taking ethanol as a ball milling auxiliary agent at the rotating speed of 350r/min for 12-18 h;
and step 3: sieving the dried powder, pressing into blocks, placing on a corundum ceramic plate, and calcining for 2-4h at the temperature of 800-; performing secondary ball milling for 12-18 h; calcining for 2-4h at the temperature of 800-900 ℃ after drying and sieving, and then carrying out ball milling for three times, drying and sieving, wherein the ball milling time is 12-18 h;
and 4, step 4: prepressing the powder into small wafers, and molding by using a cold isostatic press at the molding pressure of 200-300 MPa;
and 5: placing the small round piece on a ceramic plate scattered with powder with the same components, covering a layer of powder on the surface of the ceramic plate, covering the ceramic plate with a corundum crucible, and putting the ceramic plate into a furnace for sintering; the sintering temperature is 1180-.
And 3, pressing the mixture into blocks with the size of 15mm in diameter and 28-32mm in height.
And 4, pressing the small round piece into a round piece with the diameter of 10mm and the thickness of 0.9-1.1 mm.
Advantageous effects
According to the preparation method of the potassium sodium niobate-based nano fine crystalline ceramic with the average grain size of 160nm, provided by the invention, 0.5 mol% of lanthanum oxide is added into the raw materials, so that oxygen vacancies generated due to volatilization of alkali metal elements can be reduced, the growth of grains is hindered, and the purpose of refining the grains is achieved. Calcining the dried powder after ball milling for 12-18h at the temperature of 800-900 ℃, secondary ball milling for 12-18h, calcining again at the temperature of 800-900 ℃ after drying for 2-4h, then carrying out ball milling for 12-18h for three times and drying, and carrying out ball milling and calcining for many times to fully react and refine the raw materials, so that the sintering temperature and the heat preservation time can be reduced, and the purpose of refining grains due to insufficient grain growth is achieved. The scanning electron microscope image and the particle size distribution diagram of the finally obtained potassium sodium niobate-based ceramic are shown in figure 2 by the doping modification and the improved traditional solid phase method of the rare earth element lanthanum, the average grain size is 160nm, and the grain size distribution is uniform and very fine.
Drawings
FIG. 1 is a schematic view showing a process for producing a potassium sodium niobate-based nano-fine crystalline ceramic of example 1 of the present invention;
fig. 2 is a scanning electron microscope image and a particle size distribution diagram of the potassium sodium niobate-based nano fine-grained ceramic of example 1 of the present invention.
FIG. 3 is a scanning electron micrograph and a particle size distribution of a potassium-sodium niobate ceramic of example 2 of the present invention.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
3.433g K is weighed according to the mixture ratio of the raw materials2CO3、2.637g Na2CO3、13.234g Nb2O5、0.163g La2O3。
Putting the weighed raw material powder into a polytetrafluoroethylene ball milling tank filled with zirconia balls, and carrying out ball milling by taking ethanol as a ball milling auxiliary agent at the rotating speed of 350r/min for 12-18 h.
The dried powder is pressed into a large block with the diameter of 15mm and the height of 28-32mm after being screened, and the large block is placed on a corundum ceramic plate and calcined for 2-4h at the temperature of 800-. And carrying out secondary ball milling on the sample subjected to primary calcination, wherein the ball milling time is 12-18 h. Calcining for 2-4h at the temperature of 800-900 ℃ after drying and sieving, and then carrying out ball milling for three times, drying and sieving, wherein the ball milling time is 12-18 h.
Prepressing the powder into small wafers with the diameter of 10mm and the thickness of 0.9-1.1mm, and molding by adopting a cold isostatic press at the molding pressure of 200-300 MPa.
The blank body is placed on a ceramic plate which is scattered with powder with the same components, the surface of the ceramic plate is also covered with a layer of powder, and then the ceramic plate is covered with a corundum crucible and placed into a furnace for sintering. The sintering temperature is 1180-.
The scanning electron microscope image and the particle size distribution diagram of the potassium sodium niobate-based nano fine-grained ceramic obtained by sintering are shown in figure 2, and the average grain size is 160 nm.
Example 2:
3.45g K2CO3, 2.65g of Na2CO3 and 13.3g of Nb2O5 are weighed according to the proportion of the raw materials not doped with lanthanum oxide.
Putting the weighed raw material powder into a polytetrafluoroethylene ball milling tank filled with zirconia balls, and carrying out ball milling by taking ethanol as a ball milling auxiliary agent at the rotating speed of 350r/min for 12-18 h.
The dried powder is pressed into a large block with the diameter of 15mm and the height of 28-32mm after being screened, and the large block is placed on a corundum ceramic plate and calcined for 2-4h at the temperature of 800-. And carrying out secondary ball milling on the sample subjected to primary calcination, wherein the ball milling time is 12-18 h. Calcining for 2-4h at the temperature of 800-900 ℃ after drying and sieving, and then carrying out ball milling for three times, drying and sieving, wherein the ball milling time is 12-18 h.
Prepressing the powder into small wafers with the diameter of 10mm and the thickness of 0.9-1.1mm, and molding by adopting a cold isostatic press at the molding pressure of 200-300 MPa.
The blank body is placed on a ceramic plate which is scattered with powder with the same components, the surface of the ceramic plate is also covered with a layer of powder, and then the ceramic plate is covered with a corundum crucible and placed into a furnace for sintering. The sintering temperature is 1130-.
The scanning electron microscope image and the particle size distribution diagram of the potassium sodium niobate-based nano fine-grained ceramic obtained by sintering are shown in figure 3, and the average grain size is 920 nm.
Example 3:
3.433g K2 g of CO 23, 2.637g of Na2CO3, 13.234g of Nb2O5 and 0.163g of La2O3 are weighed according to the raw material proportion of 0.5 mol percent of doped lanthanum.
Putting the weighed raw material powder into a polytetrafluoroethylene ball milling tank filled with zirconia balls, and carrying out ball milling by taking ethanol as a ball milling auxiliary agent at the rotating speed of 350r/min for 12-18 h.
The dried powder is pressed into a large block with the diameter of 15mm and the height of 28-32mm after being screened, and the large block is placed on a corundum ceramic plate and calcined for 2-4h at the temperature of 800-. Then carrying out secondary ball milling for 12-18h, and then drying and sieving.
Prepressing the powder into small wafers with the diameter of 10mm and the thickness of 0.9-1.1mm, and molding by adopting a cold isostatic press at the molding pressure of 200-300 MPa.
The blank body is placed on a ceramic plate which is scattered with powder with the same components, the surface of the ceramic plate is also covered with a layer of powder, and then the ceramic plate is covered with a corundum crucible and placed into a furnace for sintering. When the sintering temperature is searched, the heating rate and the heat preservation time are kept unchanged, and the proper sintering temperature is not found in the large temperature range of 1100-1300 ℃. The reason may be that the reaction for forming perovskite is insufficient in the calcination process, and the raw material powder is not completely reacted, so that the high-melting-point component niobium pentoxide cannot be liquefied in the sintering process, thereby affecting the sintering behavior of the material.
Claims (3)
1. A method for preparing potassium sodium niobate-based nano fine crystalline ceramics with the average grain size of 160nm is characterized by comprising the following steps: doping rare earth element lanthanum and adopting an improved solid phase method, and comprises the following steps:
step 1: 3.433g K is weighed according to the proportion of 0.5 mol percent of lanthanum doping amount2CO3、2.637g Na2CO3、13.234g Nb2O5、0.163g La2O3
Step 2: putting the raw material powder into a polytetrafluoroethylene ball milling tank filled with zirconia balls, and carrying out ball milling by taking ethanol as a ball milling auxiliary agent at the rotating speed of 350r/min for 12-18 h;
and step 3: sieving the dried powder, pressing into blocks, placing on a corundum ceramic plate, and calcining for 2-4h at the temperature of 800-; performing secondary ball milling for 12-18 h; calcining for 2-4h at the temperature of 800-900 ℃ after drying and sieving, and then carrying out ball milling for three times, drying and sieving, wherein the ball milling time is 12-18 h;
and 4, step 4: prepressing the powder into small wafers, and molding by using a cold isostatic press at the molding pressure of 200-300 MPa;
and 5: placing the small round piece on a ceramic plate scattered with powder with the same components, covering a layer of powder on the surface of the ceramic plate, covering the ceramic plate with a corundum crucible, and putting the ceramic plate into a furnace for sintering; the sintering temperature is 1180-.
2. The method for producing a potassium sodium niobate-based nano-fine crystalline ceramic having an average crystal grain size of 160nm as claimed in claim 1, wherein: and 3, pressing the mixture into blocks with the size of 15mm in diameter and 28-32mm in height.
3. The method for producing a potassium sodium niobate-based nano-fine crystalline ceramic having an average crystal grain size of 160nm as claimed in claim 1, wherein: and 4, pressing the small round piece into a round piece with the diameter of 10mm and the thickness of 0.9-1.1 mm.
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| CN112876248A (en) * | 2021-02-02 | 2021-06-01 | 西北工业大学 | Preparation method of 1.28% large electrostrictive strain lead-free potassium sodium niobate-based piezoelectric ceramic |
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| CN112876248A (en) * | 2021-02-02 | 2021-06-01 | 西北工业大学 | Preparation method of 1.28% large electrostrictive strain lead-free potassium sodium niobate-based piezoelectric ceramic |
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Application publication date: 20210604 |