CN109020499B - Preparation process of high-performance piezoelectric ceramic - Google Patents
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Abstract
The invention discloses a preparation process of high-performance piezoelectric ceramic, which comprises the following steps: 1) taking a piezoelectric ceramic raw material; 2) the piezoelectric ceramic raw materials are filled into a ball milling tank for full mixing and ball milling, and slurry obtained after ball milling is placed in a drying box for drying to obtain powder; 3) adding water into the powder, adding one or a combination of any of ammonia water, citric acid or oxalic acid, heating for hydrothermal treatment, and drying the powder after the hydrothermal treatment to obtain piezoelectric ceramic raw material powder; 4) and (3) treating the piezoelectric ceramic raw material powder prepared in the step 3) by adopting a traditional piezoelectric ceramic treatment process to obtain the high-performance piezoelectric ceramic. The invention has the characteristics of good performance of the prepared piezoelectric ceramic, less raw material consumption, low cost, less pollution, simpler process and good process stability.
Description
Technical Field
The invention relates to a processing method of a ceramic doping material, in particular to a preparation process of high-performance piezoelectric ceramic.
Background
The piezoelectric ceramic is an information functional ceramic material capable of converting mechanical energy and electric energy into each other. The piezoelectric ceramic is manufactured by utilizing the piezoelectric effect that the material causes the relative displacement of the positive and negative charge centers in the material under the action of mechanical stress to generate polarization, so that bound charges with opposite signs appear on the surfaces of two ends of the material, and has the characteristic of sensitivity.
The particle size of the piezoelectric ceramic raw material is approximately several micrometers to several tens micrometers. How to uniformly disperse elements of each component into the ceramic is a key factor for improving the performance of the pressure-sensitive ceramic.
At present, in the actual production process of piezoelectric ceramics, raw materials are usually treated by a ball milling method, but the ball milling method can only ball mill the raw materials to about 1 micron, and although the requirements of most applications are met, the performance of ceramics using the raw materials cannot meet the requirements of customers in some high-end application occasions. In recent years, chemical coprecipitation, solution-gel method, freeze-drying method and other methods are adopted to synthesize the superfine raw material oxide, so that the performance of the ceramic is improved. However, the desired effect is not obtained yet. The hydrothermal method is a new method aiming at the treatment of ceramic raw materials at present, and can further improve the treatment effect of the raw materials. However, the current hydrothermal method still has defects, which are mainly reflected in that: 1. at present, soluble salt (mainly nitrate) of raw materials is used as a raw material in a hydrothermal method and reacts with alkali to finally prepare an oxide, but the price of the soluble salt is much higher than that of the oxide, so that the raw material cost of the ceramic is increased; 2. the amount of the oxide finally prepared from the soluble salt of the raw material is only a small part of the amount of the soluble salt (taking the soluble nitrate of zirconium oxide-zirconium nitrate pentahydrate as an example, the zirconium dioxide is 29 percent after the treatment is finished, and the rest 71 percent is nitrate radical and crystal water), so that a large amount of soluble salt and alkali are needed for reaction when the oxide is prepared, the raw material cost of the ceramic is further increased, and meanwhile, a large amount of acid radicals are contained in the waste liquid, so that the environmental pollution is large; 3. the reaction system of soluble salt and alkali is more complex, the conditions are more rigorous, and the stability of the process in the treatment process is difficult to control.
Disclosure of Invention
The invention aims to provide a preparation process of high-performance piezoelectric ceramic. The invention has the characteristics of good performance of the prepared piezoelectric ceramic, less raw material consumption, low cost, less pollution, simpler process and good process stability.
The technical scheme of the invention is as follows: a preparation process of high-performance piezoelectric ceramic comprises the following steps:
1) taking Pb3O4、TiO2、ZrO2、Nb2O5Mixing with NiO to obtain a piezoelectric ceramic raw material;
2) putting a piezoelectric ceramic raw material into a ball milling tank, adding alcohol, fully mixing and ball milling the raw material, and putting slurry obtained after ball milling into a drying box for drying to obtain powder;
3) adding water into the powder, adding one or a combination of any of ammonia water, citric acid or oxalic acid, heating for hydrothermal treatment, and drying the powder after the hydrothermal treatment in a drying oven to obtain piezoelectric ceramic raw material powder;
4) and (3) treating the piezoelectric ceramic raw material powder prepared in the step 3) by adopting a traditional piezoelectric ceramic treatment process to obtain the high-performance piezoelectric ceramic.
In the preparation process of the high-performance piezoelectric ceramic, in the step 2), the slurry is dried in a drying oven at 60-120 ℃.
In the preparation process of the high-performance piezoelectric ceramic, the slurry is dried in a drying oven at 70 ℃.
In the preparation process of the high-performance piezoelectric ceramic, in step 3), in the reaction system of the hydrothermal treatment, the concentration of one or a combination of any of ammonia water, citric acid and oxalic acid is 0.5 to 2 mol/L.
In the preparation process of the high-performance piezoelectric ceramic, in the reaction system of the hydrothermal treatment, the concentration of one or a combination of any of ammonia water, citric acid and oxalic acid is 1 mol/L.
In the preparation process of the high-performance piezoelectric ceramic, in the step 3), the treatment temperature of the hydrothermal treatment is 200-400 ℃; the treatment time of the hydrothermal treatment is 5-25 h.
In the preparation process of the high-performance piezoelectric ceramic, the treatment temperature of the hydrothermal treatment is 300 ℃; the treatment time of the hydrothermal treatment is 15 h.
In the preparation process of the high-performance piezoelectric ceramic, in step 3), the powder after the hydrothermal treatment is dried in a drying oven at 60-80 ℃.
In the preparation process of the high-performance piezoelectric ceramic, the powder after the hydrothermal treatment is dried in a drying oven at 70 ℃.
The invention has the advantages of
1. According to the invention, raw material powder is treated by an improved hydrothermal treatment method, the prepared powder is more uniform in distribution, smaller in particle size, narrower in particle size distribution range, more in specific surface area and stronger in activity, and the prepared piezoelectric ceramic is better in performance.
2. According to the invention, by directly using the oxide as the raw material for treatment, compared with the method using soluble salt as the raw material, the raw material cost is greatly reduced; meanwhile, because the oxide is directly treated to obtain the oxide, almost no raw material loss exists, and the required amount of the oxide is only required to be treated by using more raw materials, so that the material consumption is greatly reduced, and the cost is further reduced; in addition, the treatment agent consumption is less in the treatment process, the generated waste liquid is less, and the pollution degree to the environment is greatly reduced; in addition, the method directly utilizes the oxide for treatment, so that the process is simpler and the process stability is better.
To further illustrate the beneficial effects of the present invention, the applicant designed the following experiments:
examples of the experiments
1. The experimental method comprises the following steps: in the experimental example, four sets of experiments were set, the first set was the piezoelectric ceramic sheet prepared by the conventional process, the second set was the piezoelectric ceramic sheet prepared in example 1 of the present invention, the third set was the piezoelectric ceramic sheet prepared in example 2 of the present invention, and the fourth set was the piezoelectric ceramic sheet prepared in example 3 of the present invention, and the piezoelectric constants, dielectric losses, electromechanical coupling coefficients, and curie temperatures of the four sets of ceramic sheets were measured, respectively.
The experimental results are as follows: table 1 is a comparison table of experimental data results of four ceramic sheets, and it can be seen from table 1 that: the piezoelectric constant of the piezoelectric ceramic piece processed by the method of the embodiment of the invention is improved by 10 percent, the dielectric constant is improved by 20 percent, the dielectric loss is slightly reduced, and the Curie temperature is increased to about 137 ℃. The performance of the piezoelectric ceramic prepared by the invention is greatly improved, the ceramic cost is greatly reduced, the environmental pollution is reduced, and the process stability is ensured.
Table 1: four-group ceramic wafer experimental data result comparison table
Drawings
FIG. 1 is a graph showing the cumulative distribution of particle sizes of piezoelectric ceramic powders prepared by a conventional solid phase method and a hydrothermal method according to the present invention;
FIG. 2 is a scanning electron microscope image of piezoelectric ceramic powder prepared by a conventional solid phase method;
FIG. 3 is a scanning electron microscope image of a piezoelectric ceramic powder prepared by a hydrothermal method of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Examples of the invention
Example 1: a preparation process of high-performance piezoelectric ceramic comprises the following steps:
1) taking Pb according to mass percentage3O465％、TiO210％、ZrO25％、Nb2O5Mixing 15% and NiO 5% to obtain a piezoelectric ceramic raw material;
2) putting a piezoelectric ceramic raw material into a ball milling tank, adding alcohol, fully mixing and ball milling the raw material, and placing slurry obtained after ball milling into a drying box at 70 ℃ for drying to obtain powder;
3) adding water into the powder, adding ammonia water, heating to perform hydrothermal treatment, wherein in a reaction system of the hydrothermal treatment, the concentration of the ammonia water is 1mol/L, the treatment temperature of the hydrothermal treatment is 300 ℃, the treatment time of the hydrothermal treatment is 15h, and drying the powder after the hydrothermal treatment in a drying oven at 70 ℃ to obtain piezoelectric ceramic raw material powder;
4) adding 300g of deionized water into 1kg of the piezoelectric ceramic raw material powder prepared in the step 3), adding 550g of polyvinyl alcohol with the concentration of 10%, 8g of dispersant and 4g of defoaming agent, carrying out ball milling and mixing for 2 hours, then carrying out tape casting, and carrying out lamination isostatic pressing, sheet punching, glue discharging, sintering, surface metallization and polarization treatment to obtain the high-performance piezoelectric ceramic.
Example 2: a preparation process of high-performance piezoelectric ceramic comprises the following steps:
1) taking Pb according to mass percentage3O465％、TiO210％、ZrO25％、Nb2O5Mixing 15% and NiO 5% to obtain a piezoelectric ceramic raw material;
2) putting a piezoelectric ceramic raw material into a ball milling tank, adding alcohol, fully mixing and ball milling the raw material, and placing slurry obtained after ball milling into a drying box at 60 ℃ for drying to obtain powder;
3) adding water into the powder, adding citric acid, heating for hydrothermal treatment, wherein the concentration of the citric acid in a reaction system of the hydrothermal treatment is 0.5mol/L, the treatment temperature of the hydrothermal treatment is 200 ℃, the treatment time of the hydrothermal treatment is 25 hours, and drying the powder after the hydrothermal treatment in a drying oven at 60 ℃ to obtain piezoelectric ceramic raw material powder;
4) adding 250g of deionized water into 1kg of the piezoelectric ceramic raw material powder prepared in the step 3), then adding 500g of polyvinyl alcohol with the concentration of 10%, 6g of dispersant and 2g of defoaming agent, carrying out ball milling and mixing for 1 hour, then carrying out tape casting, and carrying out lamination isostatic pressing, sheet punching, glue discharging, sintering, surface metallization and polarization treatment to obtain the high-performance piezoelectric ceramic.
Example 3: a preparation process of high-performance piezoelectric ceramic comprises the following steps:
1) taking Pb according to mass percentage3O465％、TiO210％、ZrO25％、Nb2O5Mixing 15% and NiO 5% to obtain a piezoelectric ceramic raw material;
2) putting a piezoelectric ceramic raw material into a ball milling tank, adding alcohol, fully mixing and ball milling the raw material, and placing slurry obtained after ball milling into a drying box at 120 ℃ for drying to obtain powder;
3) adding water into the powder, adding oxalic acid, heating for hydrothermal treatment, wherein in a reaction system of the hydrothermal treatment, the concentration of the oxalic acid is 2mol/L, the treatment temperature of the hydrothermal treatment is 400 ℃, the treatment time of the hydrothermal treatment is 5 hours, and drying the powder after the hydrothermal treatment in a drying oven at the temperature of 80 ℃ to obtain piezoelectric ceramic raw material powder;
4) adding 350g of deionized water into 1kg of the piezoelectric ceramic raw material powder prepared in the step 3), then adding 600g of polyvinyl alcohol with the concentration of 10%, 10g of dispersant and 6g of defoaming agent, carrying out ball milling and mixing for 3 hours, then carrying out tape casting, and carrying out lamination isostatic pressing, sheet punching, glue discharging, sintering, surface metallization and polarization treatment to obtain the high-performance piezoelectric ceramic.
Claims (6)
1. A preparation process of high-performance piezoelectric ceramic is characterized by comprising the following steps:
1) taking Pb3O4、TiO2、ZrO2、Nb2O5Mixing with NiO to obtain a piezoelectric ceramic raw material;
2) putting a piezoelectric ceramic raw material into a ball milling tank, adding alcohol, fully mixing and ball milling the raw material, and putting slurry obtained after ball milling into a drying box for drying to obtain powder;
3) adding water into the powder, adding one or a combination of any of ammonia water, citric acid or oxalic acid, heating for hydrothermal treatment, and drying the powder after the hydrothermal treatment in a drying oven to obtain piezoelectric ceramic raw material powder;
4) processing the piezoelectric ceramic raw material powder prepared in the step 3) by adopting a traditional piezoelectric ceramic processing technology to obtain high-performance piezoelectric ceramic;
in the step 2), the slurry is dried in a drying oven at the temperature of 60-120 ℃;
in the step 3), in the reaction system of the hydrothermal treatment, the concentration of one or a combination of any more of ammonia water, citric acid or oxalic acid is 0.5-2 mol/L;
in the step 3), the treatment temperature of the hydrothermal treatment is 200-400 ℃; the treatment time of the hydrothermal treatment is 5-25 h.
2. The process for preparing a high-performance piezoelectric ceramic according to claim 1, wherein: the slurry was dried in a drying oven at 70 ℃.
3. The process for preparing a high-performance piezoelectric ceramic according to claim 1, wherein: in the reaction system of the hydrothermal treatment, the concentration of one or the composition of any more of ammonia water, citric acid or oxalic acid is 1 mol/L.
4. The process for preparing a high-performance piezoelectric ceramic according to claim 1, wherein: the treatment temperature of the hydrothermal treatment is 300 ℃; the treatment time of the hydrothermal treatment is 15 h.
5. The process for preparing a high-performance piezoelectric ceramic according to claim 1, wherein: in the step 3), the powder after the hydrothermal treatment is dried in a drying oven at the temperature of 60-80 ℃.
6. The process for preparing a high-performance piezoelectric ceramic according to claim 1, wherein: and drying the powder subjected to the hydrothermal treatment in a drying oven at 70 ℃.
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| CN101607823A (en) * | 2009-07-09 | 2009-12-23 | 南京航空航天大学 | A kind of hydrothermal high-temperature mixed synthetic method of piezoelectric ceramic powder |
| US20150364674A1 (en) * | 2013-02-26 | 2015-12-17 | Fujifilm Corporation | Oxide particles, piezoelectric element, and method for producing oxide particles |
| JP6414818B2 (en) * | 2015-02-24 | 2018-10-31 | 神島化学工業株式会社 | Nano composite oxide and method for producing the same |
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| CN106631005B (en) * | 2017-01-10 | 2020-01-14 | 北京元六鸿远电子科技股份有限公司 | Medium-temperature sintered lead-free high-voltage capacitor dielectric ceramic material and preparation method thereof |
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| CN101607823A (en) * | 2009-07-09 | 2009-12-23 | 南京航空航天大学 | A kind of hydrothermal high-temperature mixed synthetic method of piezoelectric ceramic powder |
| US20150364674A1 (en) * | 2013-02-26 | 2015-12-17 | Fujifilm Corporation | Oxide particles, piezoelectric element, and method for producing oxide particles |
| JP6414818B2 (en) * | 2015-02-24 | 2018-10-31 | 神島化学工業株式会社 | Nano composite oxide and method for producing the same |
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| 水热合成锆钛酸铅微粉;梁焕珍等;《矿冶》;19950630;第4卷(第2期);第57-59页 * |
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