CN113149644A - Low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic and preparation method thereof - Google Patents
Low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic and preparation method thereof Download PDFInfo
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Abstract
A low-dielectric-loss piezoelectric ceramic of lead antimonate manganese-lead zirconate titanate sintered at low temperature and a preparation method thereof. The invention belongs to the field of piezoelectric materials. The invention aims to solve the technical problems of high sintering temperature and lower piezoelectric property of the existing hard ceramic. The chemical general formula of the low-dielectric-loss piezoelectric ceramic of the invention is 0.05Pb (Mn)1/3Sb2/3)O3‑0.47PbZrO3‑0.48PbTiO3+x wt％Li2CO3Wherein 0 is<x is less than or equal to 1. The preparation method comprises the following steps: proportioning the raw materials according to the ceramic component ratio, then presintering, tabletting, binder removal, sintering at 950 ℃, and finally carrying outAnd (3) sintering silver and polarizing to obtain the low-dielectric-loss piezoelectric ceramic of lead antimonate manganese-lead zirconate titanate sintered at low temperature. The invention introduces Li with proper content2CO3The piezoelectric performance of the product is improved by 27-34%, and the sintering temperature of the ceramic is obviously reduced. The sintering temperature of about 950 ℃ greatly reduces the requirements on the sintering furnace and reduces the energy cost.
Description
Technical Field
The invention belongs to the field of piezoelectric materials, and particularly relates to low-dielectric-loss piezoelectric ceramic of lead antimonate manganese and lead zirconate titanate sintered at a low temperature and a preparation method thereof.
Background
With the continuous miniaturization of electronic products, electronic components are gradually developing in the direction of being small, light and thin. The multilayer ceramic capacitor (MLCC) is widely applied to the high and new technology fields such as medical treatment, navigation, communication and actuating systems as a chip component. For multilayer ceramics, the sintering temperature needs to be lowered to facilitate co-firing of the ceramics with internal electrodes (e.g., silver palladium alloy). In addition, the lower sintering temperature also reduces the energy consumption and the volatilization of lead oxide in the production process, and reduces the diffusion of metal ions into the ceramic. Therefore, the research and development of a new generation of piezoelectric materials with low sintering temperature and high electrical performance has great social significance and economic value.
PZT-based ceramics are widely used in various devices due to their characteristics of simple preparation process, low cost, excellent electrical properties, etc. However, the sintering temperature of the general PZT-based ceramic is over 1200 ℃, which severely limits the selection of electrodes in the preparation of multilayer ceramic. Generally, the inner electrode slurry which can be stabilized above 1200 ℃ to realize co-firing is a pure platinum electrode, which greatly increases the cost of multilayer preparation. When the sintering temperature is lower than 1000 ℃, the selection of the internal electrode slurry is greatly expanded, such as a nickel internal electrode, a copper internal electrode, a silver internal electrode and the like. The cost and the process difficulty are both obviously reduced. Therefore, lowering the sintering temperature of the material below 1000 ℃ is very critical for the preparation of multilayer piezoelectric ceramics.
Disclosure of Invention
The invention provides low-dielectric-loss lead antimonate manganese-lead zirconate titanate piezoelectric ceramic sintered at a low temperature and a preparation method thereof, aiming at solving the technical problems of high sintering temperature and low piezoelectric property of the existing hard ceramic.
The chemical general formula of the low-dielectric-loss piezoelectric ceramic of the invention is 0.05Pb (Mn)1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3Wherein 0 is<x≤1。
Further define theThe chemical formula of the low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic is 0.05Pb (Mn)1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+1wt％Li2CO3。
The preparation method of the low-dielectric-loss piezoelectric ceramic sintered at low temperature comprises the following steps of:
step one, batching: in MnO2、PbO、TiO2、ZrO2、Sb2O3、LiCO3Weighing raw materials according to the stoichiometric ratio of low-dielectric-loss piezoelectric ceramics sintered at low temperature, wherein the mass of PbO is excessive by 1.5 percent, and performing ball milling and drying;
step two, pre-burning: placing the dried powder in the first step into a crucible, and then presintering the powder in a muffle furnace;
step three, tabletting: performing secondary ball milling and drying on the pre-sintered powder obtained in the step two, then adding a polyvinyl alcohol solution, grinding uniformly, sieving and pressing into a blank;
step four, removing glue: placing the blank obtained in the step three into a muffle furnace for removing glue to obtain a glue-removed blank;
step five, sintering: placing the blank after the glue discharging obtained in the fourth step into a muffle furnace, covering the blank with powder of the same component for burning, heating to 930-970 ℃ at a heating speed of 3-10 ℃/min, preserving heat for 1.5-3 h at the temperature, and naturally cooling to room temperature after the heat preservation is finished to obtain a ceramic wafer;
step six, silver burning: polishing the surface of the ceramic wafer sintered in the fifth step, then coating silver paste on the upper surface and the lower surface of the ceramic wafer, then placing the ceramic wafer in a muffle furnace for silver burning, and naturally cooling to room temperature to obtain a silver-coated ceramic wafer;
step seven, polarization: and putting the silver-coated ceramic wafer obtained in the sixth step into silicone oil at 100-140 ℃, and applying an electric field to polarize to obtain the low-dielectric-loss lead antimonate manganese-lead zirconate titanate piezoelectric ceramic sintered at low temperature.
Further limiting, the process of pre-burning in the step two is as follows: heating to 730-770 ℃ at a heating rate of 3-10 ℃/min, and preserving heat for 1.5-3 h at the temperature to obtain the pre-sintered powder.
Further limiting, the adding amount of the polyvinyl alcohol solution in the third step is 5 wt% -7 wt% of the pre-sintering powder obtained in the second step.
Further limiting, in the third step, the sieving is carried out by sieving with a sieve of 80-200 meshes.
Further limiting, the pressing pressure in the third step is 150 MPa-300 MPa.
Further limiting, the glue discharging process in the fourth step is as follows: raising the temperature to 180-220 ℃ at a temperature raising speed of 0.5-1.5 ℃/min, preserving the heat for 1.5-2.5 h, raising the temperature to 580-620 ℃ at a temperature raising speed of 0.2-0.4 ℃/min, and preserving the heat for 1.5-2.5 h.
Further limiting, the silver firing process in the sixth step is as follows: heating to 630-670 ℃ at a heating rate of 3-10 ℃/min, and keeping the temperature for 20-40 min.
And further limiting, wherein the electric field intensity of the polarization in the seventh step is 3 kV/mm-4 kV/mm, and the polarization time is 5 min-15 min.
Compared with the prior art, the invention has the following advantages:
compared with the prior art, the invention has the following advantages:
1)Li2CO3the addition of the (B) provides a liquid phase in the solid phase reaction, improves the sintering driving force, accelerates the speed of the solid phase reaction, simultaneously, a liquid phase film among crystal grains plays a lubricating role, promotes the rearrangement of the crystal grains to be carried out in the direction of reducing air holes, reduces the surface free energy of a system, obviously reduces the sintering temperature of the ceramic, improves the piezoelectric property of the ceramic, greatly expands the selection range of the inner electrode in the preparation of the multilayer ceramic, and reduces the preparation cost of the multilayer ceramic.
2) Added Li2CO3Too little, less liquid phase can be provided during sintering, and the effect of reducing the sintering temperature is limited. When added Li2CO3When the amount is too much, the liquid phase required in the ceramic sintering process tends to be saturated, and the liquid phase continues to be saturatedThe increase does not continuously reduce the sintering temperature, but produces doping effect on the ceramic, and the electrical property of the ceramic is deteriorated.
3) In the preparation process, the presintering temperature lower than 800 ℃ is far away from the melting point of PbO, so that the grain size in the presintering powder is small. The final sintering temperature is lower than 1000 ℃, so that the formation of larger-size crystal grains in the ceramic is limited, and the electrical property of the ceramic is improved.
4) The product of the invention is prepared by introducing a suitable content of Li2CO3The piezoelectric performance is improved by 27-34%, and the sintering temperature of the ceramic is obviously reduced. The sintering temperature of about 950 ℃ greatly reduces the requirements on the sintering furnace and reduces the energy cost. In addition, base metal internal electrodes such as copper internal electrodes and nickel internal electrodes can be completely used in the preparation of the multilayer ceramic stack, and compared with platinum internal electrodes and silver-palladium internal electrodes, the cost is reduced by hundreds of times.
Drawings
FIG. 1 shows 0.05Pb (Mn) prepared in example 11/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+0.4wt％Li2CO3A micro-topography of the ceramic;
FIG. 2 is 0.05Pb (Mn) prepared in example 11/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+0.6wt％Li2CO3Dielectric temperature spectrum of ceramics.
Detailed Description
Example 1: the chemical formula of the low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic of the embodiment is 0.05Pb (Mn)1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3Wherein x is 0.1, 0.2, 0.4, 0.6, 0.8, 1.
The method for preparing the low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic of the embodiment 1 comprises the following steps:
step one, batching: in MnO2、PbO、TiO2、ZrO2、Sb2O3、LiCO3As a raw material, is prepared by0.05Pb (Mn)1/ 3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3Weighing raw materials according to the stoichiometric ratio, wherein the mass of PbO is excessive by 1.5%, and performing ball milling and drying; wherein MnO is2、PbO、TiO2、ZrO2、Sb2O3、LiCO3The raw materials are all chemical pure raw materials (the purity is more than or equal to 99 percent) sold in the market; the ball milling and drying process comprises the following steps: the ball milling medium is alcohol, the mass of the added alcohol is 80 percent of the total mass of the raw materials, the diameter of the grinding balls is 8mm, the number of the grinding balls is that the ball milling tank 1/3 is covered, and the ball milling is carried out for 24 hours and then the drying is carried out;
step two, pre-burning: putting the dried powder in the step one into a crucible, heating to 750 ℃ in a muffle furnace at a heating rate of 5 ℃/min, and preserving heat for 2 hours at the temperature to obtain pre-sintered powder;
step three, tabletting: performing secondary ball milling on the pre-sintered powder obtained in the step two for 24 hours, drying, then adding a polyvinyl alcohol solution, uniformly grinding, sieving by using a 100-mesh sieve, and pressing under 150MPa to prepare a disc-shaped blank with the diameter of 13mm and the thickness of 1 mm; the addition amount of the polyvinyl alcohol solution is 5 wt% of the pre-sintering powder obtained in the step two;
step four, removing glue: putting the blank obtained in the step three into a muffle furnace, heating to 200 ℃ at the heating rate of 1 ℃/min, preserving heat for 2h, heating to 600 ℃ at the heating rate of 0.3 ℃/min, preserving heat for 2h, and discharging glue to obtain a blank after glue discharging;
step five, sintering: placing the blank after the glue removal obtained in the step four in a muffle furnace, covering the blank with powder with the same components for burning, heating to 950 ℃ at a heating speed of 5 ℃/min, preserving heat for 2.5 hours at the temperature, and naturally cooling to room temperature after heat preservation to obtain a ceramic wafer;
step six, silver burning: polishing the surface of the ceramic wafer sintered in the fifth step, then coating silver paste on the upper surface and the lower surface of the ceramic wafer, then placing the ceramic wafer in a muffle furnace, heating to 650 ℃ at the heating rate of 5 ℃/min, preserving heat at the temperature for 30min, burning silver, and naturally cooling to room temperature to obtain a silver-coated ceramic wafer;
step seven, polarization: obtained in the sixth stepThe silver-coated ceramic sheet was placed in 120 ℃ silicone oil, and polarization was carried out for 10min by applying an electric field of 3.5kV/mm to obtain 0.05Pb (Mn)1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3The ceramic is low-dielectric-loss piezoelectric ceramic of lead antimonate manganese-lead zirconate titanate sintered at low temperature.
Comparative example: this example differs from example 1 in that: 0.05Pb (Mn)1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3Wherein x is 0, the sintering temperature is 1200 ℃, and the temperature is kept for 2.5 h. The other steps and parameters were the same as in example 1.
And (3) testing: the ceramics prepared in example 1 and comparative example were left to stand at room temperature for 24 hours to test their electrical properties, and the results of the electrical property tests are shown in table 1.
TABLE 1 test results of electrical properties
Claims (10)
1. The low-dielectric-loss piezoelectric ceramic is characterized in that the chemical general formula of the low-dielectric-loss piezoelectric ceramic is 0.05Pb (Mn)1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3Wherein 0 is<x≤1。
2. The low-temperature-sintered lead antimonate manganese-zirconate titanate low-dielectric-loss piezoelectric ceramic as claimed in claim 1, wherein the chemical formula of the low-dielectric-loss piezoelectric ceramic is 0.05Pb (Mn)1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+1wt％Li2CO3。
3. The method for preparing low-temperature sintered lead antimonate manganese-lead zirconate titanate low dielectric loss piezoelectric ceramic according to claim 1 or 2, which is carried out according to the following steps:
step one, batching: in MnO2、PbO、TiO2、ZrO2、Sb2O3、LiCO3Weighing raw materials according to the stoichiometric ratio of low-dielectric-loss piezoelectric ceramics sintered at low temperature, wherein the mass of PbO is excessive by 1.5 percent, and performing ball milling and drying;
step two, pre-burning: placing the dried powder in the first step into a crucible, and then presintering the powder in a muffle furnace;
step three, tabletting: performing secondary ball milling and drying on the pre-sintered powder obtained in the step two, then adding a polyvinyl alcohol solution, grinding uniformly, sieving and pressing into a blank;
step four, removing glue: placing the blank obtained in the step three into a muffle furnace for removing glue to obtain a glue-removed blank;
step five, sintering: placing the blank after the glue discharging obtained in the fourth step into a muffle furnace, covering the blank with powder of the same component for burning, heating to 930-970 ℃ at a heating speed of 3-10 ℃/min, preserving heat for 1.5-3 h at the temperature, and naturally cooling to room temperature after the heat preservation is finished to obtain a ceramic wafer;
step six, silver burning: polishing the surface of the ceramic wafer sintered in the fifth step, then coating silver paste on the upper surface and the lower surface of the ceramic wafer, then placing the ceramic wafer in a muffle furnace for silver burning, and naturally cooling to room temperature to obtain a silver-coated ceramic wafer;
step seven, polarization: and putting the silver-coated ceramic wafer obtained in the sixth step into silicone oil at 100-140 ℃, and applying an electric field to polarize to obtain the low-dielectric-loss lead antimonate manganese-lead zirconate titanate piezoelectric ceramic sintered at low temperature.
4. The method for preparing low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic according to claim 3, wherein the pre-sintering process in the second step is as follows: heating to 730-770 ℃ at a heating rate of 3-10 ℃/min, and preserving heat for 1.5-3 h at the temperature to obtain the pre-sintered powder.
5. The method for preparing low-temperature sintered lead antimonate-lead zirconate titanate low-dielectric-loss piezoelectric ceramic according to claim 3, wherein the addition amount of the polyvinyl alcohol solution in the third step is 5-7 wt% of the pre-sintered powder obtained in the second step.
6. The preparation method of the low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic according to claim 3, wherein the sieving in the third step is carried out by sieving with a sieve of 80-200 meshes.
7. The method for preparing low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic according to claim 3, wherein the pressing pressure in the third step is 150MPa to 300 MPa.
8. The method for preparing low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic according to claim 3, wherein the glue discharging process in the fourth step is as follows: raising the temperature to 180-220 ℃ at a temperature raising speed of 0.5-1.5 ℃/min, preserving the heat for 1.5-2.5 h, raising the temperature to 580-620 ℃ at a temperature raising speed of 0.2-0.4 ℃/min, and preserving the heat for 1.5-2.5 h.
9. The method for preparing low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic according to claim 3, wherein the silver firing process in the sixth step is as follows: heating to 630-670 ℃ at a heating rate of 3-7 ℃/min, and keeping the temperature for 20-40 min.
10. The method for preparing low-temperature sintered lead antimonate-lead zirconate titanate low-dielectric-loss piezoelectric ceramic according to claim 3, wherein the electric field intensity of the polarization in the seventh step is 3 kV/mm-4 kV/mm, and the polarization time is 5 min-15 min.
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