CN112062555A - Preparation method of BNT-BT-based lead-free negative electricity card material by doping induction of functional groups - Google Patents
Preparation method of BNT-BT-based lead-free negative electricity card material by doping induction of functional groups Download PDFInfo
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Abstract
The invention relates to a preparation method of a BNT-BT-based lead-free negative electricity card material by doping and inducing functional groups, belonging to the technical field of chemical engineering. A preparation method of a BNT-BT based lead-free negative electricity card material induced by functional group doping comprises the steps of weighing the obtained raw materials according to the stoichiometric ratio of (1-z) { (1-x) BNT-xBT } -z { (1-y) BT-yBMT } and preparing mixed slurry by ball milling in a medium of absolute ethyl alcohol; drying the obtained product to obtain raw material powder; pre-pressing and molding the obtained raw material powder, and then calcining to obtain a calcined block; ball milling the obtained calcined block; drying and sieving the obtained product; pressing the obtained product into a sample with the diameter of 5-10mm and the thickness of 1-2mm, and then performing cold isostatic pressing to prepare a sample blank; sintering the obtained sample blank, grinding the sample blank into a sheet with the thickness of 500-1000um after the sample blank is cooled to room temperature. The preparation method can regulate and control the structure and the electric card performance of the ceramic material by changing the doping proportion of the functional groups, and is a convenient and rapid preparation technology.
Description
Technical Field
The invention relates to a preparation method of a BNT-BT-based lead-free negative electricity card material by doping and inducing functional groups, belonging to the technical field of chemical engineering.
Background
The ferroelectric ceramic is a very important functional material and is widely applied to various aspects of human life and production, such as national defense and military, aerospace, electronic communication, medical field, industrial field, daily household appliances and the like.
Since lead has toxicity and is harmful to the environment, many countries have legislation that prohibits the use of lead-containing materials, scientists are concerned about the research of high-performance lead-free ferroelectric materials, and the development of high-performance lead-free ferroelectric materials is one of the important research subjects.
Disclosure of Invention
The invention aims to provide a preparation method of a BNT-BT-based high-performance lead-free negative electricity card material by utilizing functional group doping induction. The invention utilizes the lead-free relaxation ferroelectric ceramic material (1-x) Bi with wide temperature zone and larger electrocaloric effect0.5Na0.5TiO3-xBaTiO3(abbreviated as (1-x) BNT-xBT) and (1-y) BaTiO doped at different ratios by a solid-phase sintering method3-yBiMg0.5Ti0.5O3(abbreviated as (1-y) BT-yBMT) functional groups to regulate and control the electrocaloric performance of the ceramic material and provide a new method for preparing high-performance refrigeration ceramic.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a BNT-BT based lead-free negative electricity card material by utilizing functional group doping induction comprises the following steps:
1) mixing MgO and Na2CO3、Bi2O3、TiO2、BaCO3、CaCO3Drying to remove water;
2) weighing the raw materials obtained in the step 1) according to the stoichiometric ratio of (1-z) { (1-x) BNT-xBT } -z { (1-y) BT-yBMT }, wherein the value of x is 0.06-0.12, the value of y is 0.3-0.8, and the value of z is 0-0.6, and preparing mixed slurry by ball milling in a medium of absolute ethyl alcohol;
3) drying the product obtained in the step 2) to obtain raw material powder;
4) pre-pressing and molding the raw material powder obtained in the step 3), and then calcining to obtain a calcined block;
5) ball-milling the calcined block obtained in the step 4);
6) drying and sieving the product obtained in the step 5);
7) pressing the product obtained in the step 6) into a sample with the diameter of 5-10mm and the thickness of 1-2mm, and then performing cold isostatic pressing to obtain a sample blank;
8) sintering the sample blank obtained in the step 7), grinding the sample blank into a sheet with the thickness of 500-1000um after cooling to room temperature.
Preferably, the calcination in the step 4) is performed in a low-temperature box-type furnace at a temperature rising rate of 3 ℃/min to 800-900 ℃ for 4-8 h.
Preferably, the cold isostatic pressure in the step 7) is 200-300MPa, and the pressure maintaining time is 5-10 min.
Preferably, the sample blank in step 8) is sintered for 4-8h in a low-temperature chamber furnace at a heating rate of 3-5 ℃/min to 1100-1300 ℃.
The invention has the beneficial effects that: the ceramic material with the advantages of high purity, good compactness, high electric field breakdown strength, large electrocaloric effect, wide operating temperature range and the like is obtained; the preparation method is relatively simple, the structure and the electric card performance of the ceramic material can be regulated and controlled by changing the doping ratio of the functional groups, and the preparation method is a convenient and rapid preparation technology. In addition, the invention does not need annealing, but the obtained ceramic has good performance and meets the use requirement.
Drawings
FIG. 1 is a graph showing the electrical card properties of the functional group doping-induced (1-x) BNT-xBT ceramic material obtained in example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited to the scope of the examples. These examples are intended to illustrate the invention only and are not intended to limit the scope of the invention. In addition, various modifications may occur to those skilled in the art upon reading the present disclosure, and such equivalent variations are within the scope of the present invention as defined in the appended claims.
Example 1
(1) Adding excessive Na and Bi as raw materials Na2CO3、Bi2O3、TiO2、BaCO3、CaCO3Drying in a ventilation oven at 100 ℃ for 10h to remove the moisture of the raw materials;
(2) drying the obtained product in the step (1)The dry starting materials were weighed in the stoichiometric ratio of pure (1-x) BNT-xBT, where x is 0.06, y is 0.3, and z is 0, i.e. 0.94Bi0.5Na0.5TiO3-0.06BaTiO3Ball-milling for about 10 hours at a rotating speed of 400r/min by using a planetary ball mill in a medium of absolute ethyl alcohol to obtain uniformly mixed slurry;
(3) pouring the dry and uniform mixed slurry obtained in the step (2) into a culture dish, and drying for 8 hours in a ventilation drying oven at 100 ℃ to obtain uniform dry raw material powder;
(4) pre-pressing and molding the uniformly dried raw material powder obtained in the step (3), heating to 800 ℃ in a low-temperature box type furnace at the heating rate of 3 ℃/min, calcining for 4 hours, and cooling to room temperature along with the furnace to obtain a calcined block;
(5) grinding the calcined block obtained in the step (4) by using a mortar, and then ball-milling for 10 hours at a rotating speed of 400r/min by using a planetary ball mill to obtain calcined mixed slurry;
(6) pouring the calcined mixed slurry obtained in the step (5) into a culture dish, drying for 8 hours in a ventilating drying box at 100 ℃, and then sieving the dried powder to obtain powder with uniform particle size;
(7) pressing the powder with uniform particle size obtained in the step (6) into a sample with the diameter of 5mm and the thickness of 1mm by using a uniform die, then placing the sample into a rubber sleeve, performing vacuum-pumping treatment, and placing the sample into a cold isostatic press to maintain the pressure at 200MPa for 5min to prepare a sample blank;
(8) and (4) heating the sample blank obtained in the step (7) to 1100 ℃ in a low-temperature box furnace at the heating rate of 3 ℃/min, sintering for 4h, cooling to room temperature along with the furnace, taking out, and grinding into a sheet with the thickness of 500um by using abrasive paper, thus finally obtaining the sample.
Example 2
(1) Excess raw materials of Mg, Na and Bi such as MgO and Na2CO3、Bi2O3、TiO2、BaCO3、CaCO3Drying in a ventilation oven at 100 ℃ for 10h to remove the moisture of the raw materials;
(2) the dry starting material obtained in step (1) is stoichiometrically pure (1-z) { (1-x) BNT-xBT } -z { (1-y) BT-yBMT }In the formula, x is 0.1, y is 0.5, and z is 0.5, i.e., 0.5{0.9Bi {0.5Na0.5TiO3-0.1BaTiO3}-0.5{(0.5BaTiO3-0.5BiMg0.5Ti0.5O3Ball-milling for about 10 hours at a rotating speed of 400r/min by using a planetary ball mill in the medium of absolute ethyl alcohol to obtain uniformly mixed slurry;
(3) pouring the dry and uniform mixed slurry obtained in the step (2) into a culture dish, and drying for 8 hours in a ventilation drying oven at 100 ℃ to obtain uniform dry raw material powder;
(4) pre-pressing and molding the uniformly dried raw material powder obtained in the step (3), heating to 800 ℃ in a low-temperature box type furnace at the heating rate of 3 ℃/min, calcining for 4 hours, and cooling to room temperature along with the furnace to obtain a calcined block;
(5) grinding the calcined block obtained in the step (4) by using a mortar, and then ball-milling for 10 hours at a rotating speed of 400r/min by using a planetary ball mill to obtain calcined mixed slurry;
(6) pouring the calcined mixed slurry obtained in the step (5) into a culture dish, drying for 8 hours in a ventilating drying box at 100 ℃, and then sieving the dried powder to obtain powder with uniform particle size;
(7) pressing the powder with uniform particle size obtained in the step (6) into a sample with the diameter of 5mm and the thickness of 1mm by using a uniform die, then placing the sample into a rubber sleeve, performing vacuum-pumping treatment, and placing the sample into a cold isostatic press to maintain the pressure at 200MPa for 5min to prepare a sample blank;
(8) and (4) heating the sample blank obtained in the step (7) to 1100 ℃ in a low-temperature box furnace at the heating rate of 3 ℃/min, sintering for 4h, cooling to room temperature along with the furnace, taking out, and grinding into a sheet with the thickness of 500um by using abrasive paper, thus finally obtaining the sample.
Example 3
(1) Excess raw materials of Mg, Na and Bi such as MgO and Na2CO3、Bi2O3、TiO2、BaCO3、CaCO3Drying in a ventilation oven at 120 ℃ for 12h to remove the moisture of the raw materials;
(2) the dry raw material obtained in the step (1) is pure (1-z)) { (1-x) BNT-xBT } -z { (1-y) BT-yBMT } is weighed in a stoichiometric ratio, where x is 0.1, y is 0.5, and z is 0.5, i.e., 0.5{0.9Bi }0.5Na0.5TiO3-0.1BaTiO3}-0.5{(0.5BaTiO3-0.5BiMg0.5Ti0.5O3Ball-milling for about 12 hours at a rotating speed of 500r/min by using a planetary ball mill in the medium of absolute ethyl alcohol to obtain uniformly mixed slurry;
(3) pouring the dry and uniform mixed slurry obtained in the step (2) into a culture dish, and drying for 10 hours in a ventilating drying oven at 120 ℃ to obtain uniform dry raw material powder;
(4) pre-pressing and molding the uniformly dried raw material powder obtained in the step (3), heating to 850 ℃ at a heating rate of 3 ℃/min in a low-temperature box type furnace, calcining for 6 hours, and cooling to room temperature along with the furnace to obtain a calcined block;
(5) grinding the calcined block obtained in the step (4) by using a mortar, and then ball-milling for 12 hours at a rotating speed of 500r/min by using a planetary ball mill to obtain calcined mixed slurry;
(6) pouring the calcined mixed slurry obtained in the step (5) into a culture dish, drying the mixed slurry in a ventilating drying box at the temperature of 120 ℃ for 10 hours, and then sieving the dried powder to obtain powder with uniform particle size;
(7) pressing the powder with uniform particle size obtained in the step (6) into a sample with the diameter of 6mm and the thickness of 1.5mm by using a uniform die, then placing the sample into a rubber sleeve, performing vacuum-pumping treatment, and placing the sample into a cold isostatic press to maintain the pressure for 6min under the pressure of 250MPa to prepare a sample blank;
(8) and (4) heating the sample blank obtained in the step (7) to 1200 ℃ in a low-temperature box type furnace at the heating rate of 4 ℃/min, sintering for 6h, cooling to room temperature along with the furnace, taking out, and grinding into a sheet with the thickness of 800um by using abrasive paper, thus finally obtaining the sample.
Example 4
(1) Excess raw materials of Mg, Na and Bi such as MgO and Na2CO3、Bi2O3、TiO2、BaCO3、CaCO3Drying in a ventilation oven at 150 ℃ for 15h to remove the moisture of the raw materials;
(2) the dried starting material obtained in step (1) was weighed according to the stoichiometric ratio of pure (1-z) { (1-x) BNT-xBT } -z { (1-y) BT-yBMT } where x is 0.12, y is 0.8, and z is 0.6, i.e.:
0.4{0.88Bi0.5Na0.5TiO3-0.12BaTiO3}-0.6{(0.2BaTiO3-0.8BiMg0.5Ti0.5O3ball-milling for about 15 hours at a rotating speed of 600r/min by using a planetary ball mill in the medium of absolute ethyl alcohol to obtain uniformly mixed slurry;
(3) pouring the dry and uniform mixed slurry obtained in the step (2) into a culture dish, and drying for 12 hours in a ventilating drying oven at 150 ℃ to obtain uniform dry raw material powder;
(4) pre-pressing and molding the uniformly dried raw material powder obtained in the step (3), heating to 900 ℃ at the heating rate of 3 ℃/min in a low-temperature box type furnace, calcining for 8 hours, and cooling to room temperature along with the furnace to obtain a calcined block;
(5) grinding the calcined block obtained in the step (4) by using a mortar, and then ball-milling for 15 hours at a rotating speed of 600r/min by using a planetary ball mill to obtain calcined mixed slurry;
(6) pouring the calcined mixed slurry obtained in the step (5) into a culture dish, drying the mixed slurry in a ventilating drying box at 150 ℃ for 12 hours, and then sieving the dried powder to obtain powder with uniform particle size;
(7) pressing the powder with uniform particle size obtained in the step (6) into a sample with the diameter of 10mm and the thickness of 2mm by using a uniform die, then placing the sample into a rubber sleeve, performing vacuum-pumping treatment, and placing the sample into a cold isostatic press to maintain the pressure at 300MPa for 10min to prepare a sample blank;
(8) and (4) heating the sample blank obtained in the step (7) to 1300 ℃ in a low-temperature box type furnace at the heating rate of 5 ℃/min, sintering for 8h, cooling to room temperature along with the furnace, taking out, and grinding into a sheet with the thickness of 1000um by using abrasive paper, thus finally obtaining the sample.
Claims (4)
1. A preparation method of a BNT-BT based lead-free negative electronic card material by utilizing functional group doping induction, which is characterized by comprising the following steps:
1) mixing MgO and Na2CO3、Bi2O3、TiO2、BaCO3、CaCO3Drying to remove water;
2) weighing the raw materials obtained in the step 1) according to the stoichiometric ratio of (1-z) { (1-x) BNT-xBT } -z { (1-y) BT-yBMT } in the general formula, wherein the value of x is 0.06-0.12, the value of y is 0.3-0.8, and the value of z is 0-0.6, and preparing mixed slurry by ball milling in a medium of absolute ethyl alcohol;
3) drying the product obtained in the step 2) to obtain raw material powder;
4) pre-pressing and molding the raw material powder obtained in the step 3), and then calcining to obtain a calcined block;
5) ball-milling the calcined block obtained in the step 4);
6) drying and sieving the product obtained in the step 5);
7) pressing the product obtained in the step 6) into a sample with the diameter of 5-10mm and the thickness of 1-2mm, and then performing cold isostatic pressing to obtain a sample blank;
8) sintering the sample blank obtained in the step 7), grinding the sample blank into a sheet with the thickness of 500-1000um after cooling to room temperature.
2. The method as claimed in claim 1, wherein the step 4) of calcining is performed in a low temperature chamber furnace at a temperature rising rate of 3 ℃/min to 800-900 ℃ for 4-8 h.
3. The method for preparing the BNT-BT based lead-free negative electricity card material doped and induced by functional groups according to claim 1, wherein the cold isostatic pressure of step 7) is 200-300MPa, and the pressure holding time is 5-10 min.
4. The method as claimed in claim 1, wherein the step 8) of sintering the sample blank in a low temperature chamber furnace at a temperature raising rate of 3-5 ℃/min to 1100-1300 ℃ for 4-8 h.
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Application publication date: 20201211 |