CN111646795B - high-Curie-point piezoelectric material and preparation method thereof - Google Patents
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Abstract
The invention discloses a high Curie point piezoelectric material and a preparation method thereof, according to BaCO360 to 65 portions of CaCO33-7 parts of TiO225-30 parts of ZrO21-5 parts of SnO21-5 parts of Sm2O30 to 0.08 portion of Li2CO3Weighing 0.4-0.8 part of each raw material, taking deionized water as a ball milling medium, ball milling and mixing for 6-12h, drying until complete drying, and sieving with a 50-2000-mesh sieve; calcining at 950 ℃ and 1100 ℃ for 3-4h, and cooling to room temperature along with the furnace; then deionized water is used as a ball milling medium, ball milling is carried out for 6-12 hours, drying is carried out until complete drying is achieved, and screening is carried out by a 50-2000-mesh sieve; adding binder 5-8% of the total weight, and pressing under 10-30Mpa to obtain 10mm diameter wafer; keeping the temperature at 1000-800 deg.C for 4h, naturally cooling to room temperature, taking out, coating silver paste on two sides, and treating with 800-600 deg.CoC, silver is burnt for 10-30 minutes, and then polarization treatment is carried out to obtain the high Curie point piezoelectric material. The invention has excellent electrical property, high Curie point, energy saving and environmental protection.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a high-Curie-point piezoelectric material and a preparation method of the high-Curie-point piezoelectric material.
Background
Piezoelectric materials are crystalline materials that develop a voltage between two end faces when subjected to a pressure, and the application fields can be roughly classified into two categories: i.e., vibrational energy and ultrasonic vibrational energy-electrical energy transducer applications including electro-acoustic, underwater, and ultrasonic transducers, among others, as well as other sensor and driver applications. Most of piezoelectric materials used in the market are lead-based piezoelectric materials PZT; as is well known, PZT devices cause lead pollution in various links such as production, application, recovery and treatment, thereby harming human health; in addition, the lead-based piezoelectric material has high sintering temperature and large energy consumption in the preparation process.
BaTiO3Is the earliest perovskite (ABO)3) One of the ferroelectric materials has been found to be popular in the industrial and academic fields because it does not contain lead, but it is required to further improve various electrical properties, especially curie temperature, as an environment-friendly piezoelectric material by substituting a lead-based piezoelectric material to realize the practical use of the environment-friendly piezoelectric ceramic material. By adding Bi2O3And Li2CO3The prepared composite sintering aid reduces the sintering temperature, but the process has the requirement on the particle size of the raw material powder at a nanometer level, thereby increasing the material cost; yao et al in Ba0.85Ca0.15Ti0.9Zr0.1-xSnxSnO doping in environment-friendly piezoelectric ceramic material2The electrical property of the environment-friendly piezoelectric ceramic is greatly improved, but the sintering temperature in the preparation process is up to 1350 ℃, the Curie temperature is low, and the maximum temperature is about 60 ℃; the channel of the channel is in Ba0.85Ca0.15Zr0.1Ti0.9O3Sm doped in leadless piezoelectric ceramic2O3The curie temperature was increased, but only to 95 ℃. Along with the changing of increasingly diversified and complicated requirements of piezoelectric ceramic components, the existing barium calcium zirconate titanate Ba0.85Ca0.15Zr0.1Ti0.9O3Various electrics of environment-friendly piezoelectric ceramicThe performance has not been satisfactory.
Disclosure of Invention
The invention aims to overcome the defects and provide the high-Curie-point piezoelectric material which has excellent electrical performance, high Curie point, energy conservation and environmental protection.
The invention also aims to provide a preparation method of the high-Curie-point piezoelectric material.
The invention relates to a high Curie point piezoelectric material which is prepared from the following raw materials in parts by mass: BaCO360 to 65 portions of CaCO33-7 parts of TiO225-30 parts of ZrO21-5 parts of SnO21-5 parts of Sm2O30 to 0.08 portion of Li2CO30.4 to 0.8 portion.
The above-mentioned high Curie point piezoelectric material, preferably Sm2O3The mass portion of (A) is 0.02-0.06.
The above high Curie point piezoelectric material, more preferably Sm2O3The mass part of (b) is 0.04.
The invention relates to a preparation method of a high Curie point piezoelectric material, which comprises the following steps:
(1) weighing the raw materials according to the formula, taking deionized water as a ball milling medium, ball milling the mixed materials for 6-12h, drying until the mixed materials are completely dried, and sieving the mixed materials by a 50-2000-mesh sieve;
(2) calcining the sieved material in an environment of 950 ℃ and 1100 ℃ for 3-4h, and cooling to room temperature along with the furnace;
(3) the cooled material is then ball milled for 6 to 12 hours by using deionized water as a ball milling medium, dried to be completely dry and sieved by a 50 to 2000-mesh sieve;
(4) adding binder 5-8% of the total weight of the dried material, and pressing into a wafer with a diameter of 10mm under a pressure of 10-30 Mpa;
(5) and (3) keeping the wafer at the temperature of 1000-1200 ℃ for 4h, naturally cooling the wafer to room temperature along with the furnace, taking out the wafer, coating silver paste on two surfaces of the wafer, burning the silver for 10-30 minutes at the temperature of 600-800 ℃, and then performing polarization treatment to obtain the high Curie point piezoelectric material.
The method for preparing the high curie point piezoelectric material comprises the following steps: in the step (4), the binder is polyvinyl butyral (PVB).
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can be seen as follows: the invention uses BaCO3、CaCO3、TiO2And ZrO2As main component, tin phase and samarium phase are used as doping components, according to the theory of allowable gap factor, that is, when the radius of the doped ion is smaller than that of the doped ion
When doping ion replaces ABO3B site of the type structure, replacing B ion, when the radius of the doped ion is larger than that of the B ion
When the radius of the replacement ion is between
To
In between, the substitutional ions may occupy the a site and also the B site. Radius r (Sm) of samarium ion3+) Is composed of
Thus Sm3+To occupy the A position for substituting a part of Ba2+Radius of tin ion r (Sn)4+) Is composed of
Thus Sn4+To occupy the B-position for replacing a part of Ti4+. Adopts a mode of composite doping of two ions and utilizes Sn4+By acceptor doping into ABO3B-substituted partial Ti of perovskite phase of type4+，Sm3+By donor doping into ABO3A-site substituted Ba moiety of perovskite-type phase2+By using Sn4+And Sm3+The composite doping of the ceramic promotes the ceramicThe formation of ceramic morphotropic phase boundary, so as to improve the electrical property; meanwhile, the composite doping can also change the lattice constant of the ceramic, so that the crystal axis ratio is increased, the tetragonality is enhanced, and the ceramic can be changed into a paraelectric phase only by needing higher energy, thereby achieving the purpose of improving the Curie temperature; sm3+Substituted Ba2+High price replaces low price, is easy to promote the generation of barium vacancy concentration, and is beneficial to improving dielectric property and the like. By addition of Li2CO3As a sintering aid, the sintering is carried out at low temperature, and the low-temperature sintering greatly saves energy. And the main component and the doping component do not contain lead element, thereby achieving the purpose of environmental protection.
Drawings
FIG. 1 shows Sm doped with 0, 0.02, 0.04, 0.06 and 0.08 in terms of impurity content2O3Curie temperature diagram of piezoelectric material.
Detailed Description
Example 1:
a preparation method of a high Curie point piezoelectric material comprises the following steps:
(1) according to BaCO360 portions of CaCO33 parts of TiO225 parts of ZrO21 part of SnO21 part of Li2CO30.4 part of deionized water is used as a ball milling medium, ball milling and mixing are carried out for 6 hours, drying is carried out till complete drying, and the mixture is sieved by a 50-mesh sieve;
(2) calcining the sieved material in an environment of 1000 ℃ for 4 hours, and cooling to room temperature along with the furnace;
(3) the cooled material is then used as a ball milling medium, ball milled for 6 hours, dried to be completely dry and sieved by a 50-mesh sieve;
(4) adding polyvinyl butyral (PVB) accounting for 5 percent of the total weight of the dried material into the dried material, and pressing the mixture into a wafer with the diameter of 10mm under the pressure of 10 Mpa;
(5) and (3) keeping the temperature of the wafer at 1200 ℃ for 4h, naturally cooling the wafer to room temperature along with the furnace, taking out the wafer, coating silver paste on two sides, burning silver for 30 minutes at 600 ℃, and then performing polarization treatment to obtain the high Curie point piezoelectric material.
Example 2:
a preparation method of a high Curie point piezoelectric material comprises the following steps:
(1) according to BaCO362 parts of CaCO34 parts of TiO226 parts of ZrO22 parts of SnO22 parts of Sm2O30.02 part of Li2CO30.5 part of ingredients, taking deionized water as a ball milling medium, ball milling the mixed materials for 8 hours, drying the mixed materials till complete drying, and sieving the mixed materials by a 200-mesh sieve;
(2) calcining the sieved material in an environment of 950 ℃ for 4 hours, and cooling to room temperature along with the furnace;
(3) the cooled material is then used as a ball milling medium, ball milled for 8 hours, dried to be completely dry and sieved by a 200-mesh sieve;
(4) adding 6 percent of polyvinyl butyral (PVB) in the dried material, and pressing the mixture into a wafer with the diameter of 10mm under the pressure of 20 Mpa;
(5) and (3) keeping the temperature of the wafer at 1000 ℃ for 4h, naturally cooling the wafer to room temperature along with the furnace, taking out the wafer, coating silver paste on two sides, burning silver for 25 minutes at 650 ℃, and then performing polarization treatment to obtain the high Curie point piezoelectric material.
Example 3:
a preparation method of a high Curie point piezoelectric material comprises the following steps:
(1) according to BaCO363 parts of CaCO35 parts of TiO227 parts of ZrO23 parts of SnO23 parts of Sm2O30.04 part of Li2CO30.6 part of ingredients, taking deionized water as a ball milling medium, ball milling the mixed materials for 10 hours, drying the mixed materials till complete drying, and sieving the mixed materials by a 1000-mesh sieve;
(2) calcining the sieved material in an environment of 1000 ℃ for 3.5h, and cooling to room temperature along with the furnace;
(3) the cooled material is then used as a ball milling medium, ball milled for 10 hours, dried to be completely dry and sieved by a 1000-mesh sieve;
(4) adding polyvinyl butyral (PVB) accounting for 7% of the total weight of the dried material into the dried material, and pressing the mixture into a wafer with the diameter of 10mm under the pressure of 20 Mpa;
(5) and (3) keeping the temperature of the wafer at 1050 ℃ for 4h, naturally cooling the wafer to room temperature along with the furnace, taking out the wafer, coating silver paste on two sides, burning silver for 20 minutes at 700 ℃, and then performing polarization treatment to obtain the high Curie point piezoelectric material.
Example 4:
a preparation method of a high Curie point piezoelectric material comprises the following steps:
(1) according to BaCO364 parts of CaCO36 parts of TiO228 parts of ZrO24 parts of SnO24 parts of Sm2O30.06 part of Li2CO30.7 part of ingredients, ball milling the mixed materials for 11 hours by taking deionized water as a ball milling medium, drying the mixed materials till complete drying, and sieving the dried mixed materials by a 2000-mesh sieve;
(2) calcining the sieved material in an environment of 1050 ℃ for 3.5h, and cooling to room temperature along with the furnace;
(3) the cooled material is used as a ball milling medium by deionized water, is dried to be completely dry after ball milling for 11 hours, and is sieved by a 2000-mesh sieve;
(4) adding polyvinyl butyral (PVB) accounting for 8% of the total weight of the dried material into the dried material, and pressing the mixture into a wafer with the diameter of 10mm under the pressure of 20 Mpa;
(5) and (3) keeping the temperature of the wafer at 1100 ℃ for 4h, naturally cooling the wafer to room temperature along with the furnace, taking out the wafer, coating silver paste on two sides, burning silver for 15 minutes at 750 ℃, and then performing polarization treatment to obtain the high Curie point piezoelectric material.
Example 5:
a preparation method of a high Curie point piezoelectric material comprises the following steps:
(1) according to BaCO365 parts of CaCO37 parts of TiO230 parts of ZrO25 parts of SnO25 parts of Sm2O30.08 part of Li2CO30.8 part of ingredients, taking deionized water as a ball milling medium, ball milling the mixed materials for 12 hours, drying the mixed materials till complete drying, and sieving the mixed materials by a 2000-mesh sieve;
(2) calcining the sieved material in an environment of 1100 ℃ for 3 hours, and cooling to room temperature along with the furnace;
(3) the cooled material is then used as a ball milling medium, ball milled for 12 hours, dried to be completely dry and sieved by a 2000-mesh sieve;
(4) adding 6 percent of polyvinyl butyral (PVB) in the dried material, and pressing the mixture into a wafer with the diameter of 10mm under the pressure of 30 Mpa;
(5) and (3) keeping the temperature of the wafer at 1150 ℃ for 4h, naturally cooling the wafer to room temperature along with the furnace, taking out the wafer, coating silver paste on two sides, burning silver for 10 minutes at 800 ℃, and then performing polarization treatment to obtain the high Curie point piezoelectric material.
Comparative experimental example:
1. the experimental method comprises the following steps:
the experimental example is provided with five groups of experiments, wherein the first group is undoped Sm2O3As in example 1 of the present invention, the second group of BCZTS piezoelectric materials was obtained by using example 2 of the present invention, the third group was obtained by using example 3 of the present invention, the fourth group was obtained by using example 4 of the present invention, the fifth group was obtained by using example 5 of the present invention, and the curie temperature, sintering temperature, and piezoelectric constant of each of the materials in the five groups were measured by using the GB/T3389-2008 test standards.
2. The experimental results are as follows:
the Curie temperature was determined as shown in FIG. 1, and the other corresponding results are shown in the following table. Visible, and undoped Sm2O3Compared with the environment-friendly piezoelectric material, Sm is doped2O3The Curie temperature and various electrical properties of the environment-friendly piezoelectric material are improved, the sintering temperature is reduced to some extent, and energy is saved.
3. Analysis of experiments
As shown by the five experimental results, Sm is doped2O3The performance of the piezoelectric material is improved, the piezoelectric constant and the Curie temperature are both improved, and the addition of the sintering aid greatly reduces the energy consumption in the preparation process of the material and saves the energy. Sm3+By donor doping into ABO3A-site substituted Ba moiety of perovskite-type phase2+By using Sn4+And Sm3+The composite doping is carried out, so that the formation of a ceramic morphotropic phase boundary is promoted, and the electrical property is improved; meanwhile, the composite doping can also change the lattice constant of the ceramic, so that the crystal axis ratio is increased, the tetragonality is enhanced, and the ceramic can be changed into a paraelectric phase only by needing higher energy, thereby improving the Curie temperature of the ceramic. In conclusion, when Sm is doped2O3When the amount of (b) is 0.04 parts by mass, all properties are the best.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the present invention without departing from the technical spirit of the present invention.
Claims (5)
1. The high-Curie-point piezoelectric material is prepared from the following raw materials in parts by mass: BaCO360 to 65 portions of CaCO33-7 parts of TiO225-30 parts of ZrO21-5 parts of SnO21-5 parts of Sm2O3 0 to 0.08 portion of Li2CO30.4 to 0.8 portion.
2. The high curie point piezoelectric material of claim 1, wherein: sm2O3The mass portion of (A) is 0.02-0.06.
3. The high curie point piezoelectric material of claim 1 or 2, wherein: sm2O3The mass part of (b) is 0.04.
4. A method of making a high curie point piezoelectric material as claimed in claim 3, comprising the steps of:
(1) weighing the raw materials according to the formula, taking deionized water as a ball milling medium, ball milling the mixed materials for 6-12h, drying until the mixed materials are completely dried, and sieving the mixed materials by a 50-2000-mesh sieve;
(2) calcining the sieved material in an environment of 950 ℃ and 1100 ℃ for 3-4h, and cooling to room temperature along with the furnace;
(3) the cooled material is then used as a ball milling medium, ball milled for 6 to 12 hours, dried to be completely dry and sieved by a 50 to 2000-mesh sieve;
(4) adding binder 5-8% of the total weight of the dried material, and pressing into a wafer with a diameter of 10mm under a pressure of 10-30 Mpa;
(5) keeping the wafer at the temperature of 1000-800 ℃ for 4h, naturally cooling the wafer to room temperature along with the furnace, taking out the wafer, coating silver paste on two surfaces of the wafer, and performing 600-800 DEG heatingoC, silver is burnt for 10-30 minutes, and then polarization treatment is carried out to obtain the high Curie point piezoelectric material.
5. The method of making a high curie point piezoelectric material of claim 4, wherein: in the step (4), the binder is polyvinyl butyral.
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