CN114315344A - Negative temperature coefficient ceramic dielectric material and preparation method thereof - Google Patents
Negative temperature coefficient ceramic dielectric material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic dielectric materials, and provides a negative temperature coefficient ceramic dielectric material and a preparation method thereof, aiming at solving the problem that the capacitance temperature coefficient of the existing ceramic dielectric material is continuously changed with the positive or negative in the range of 25-200 ℃, wherein the negative temperature coefficient ceramic dielectric material is prepared from 80-90% of 0.94BaO-0.12CaO-0.04TiO in percentage by mass2And 10-20% of Y2O3‑ZnO‑H3BO3And (4) forming. Has the characteristics of high dielectric constant, low dielectric loss and negative temperature coefficient.
Description
Technical Field
The invention belongs to the technical field of ceramic dielectric materials, and particularly relates to a negative temperature coefficient ceramic dielectric material and a preparation method thereof.
Background
In the current world, electronic technology has been developed dramatically, and the demand of people for light, thin and small electronic devices such as notebook computers and smart phones has been increased rapidly, which promotes the development of electronic components toward miniaturization. The surface assembling technology is a new assembling technology developed on the basis of semiconductor chip integrating technology and thick film mixed integrating technology, and chip elements are mounted on the surface of printed circuit board by wave soldering, reflow soldering and other methods to realize high-density assembling of circuit, so that the circuit area is greatly reduced, and the method is very suitable for producing miniaturized electronic equipment. The multilayer ceramic capacitor (MLCC) is used as a basic electronic element, has the characteristics of wide temperature range, small volume, high capacitance range and the like, is the most widely applied device in passive chip devices, is mainly applied to oscillation and coupling circuits in various military and civil integrated machines, and covers the industrial ports of computers, mobile phones, digital household appliances, automobile electrical appliances and the like. The MLCC consists of three parts, namely an internal electrode, a ceramic layer and a terminal electrode. The dielectric material and the internal electrode are stacked in a staggered manner, then sintered and fired at high temperature to form, and then the metal layer is sealed at the two ends of the chip to obtain a structure body similar to a monolithic body, so that the MLCC is also called a monolithic capacitor.
Although the ceramic dielectric materials reported at present are various, the temperature coefficient of capacitance of the ceramic materials is positive or negative within the range of 25 ℃ to 200 ℃ and changes continuously. The invention provides a dielectric material with high negative capacitance temperature coefficient, which can be used as a temperature compensation material and a functional device material, and the invention of the dielectric material is helpful for enriching the requirements of the products. In addition, because the capacitor generates power loss and generates heat to raise the temperature of the capacitor under the action of voltage in the using process, the temperature rise is determined by the external alternating voltage, the high and low capacitance of the frequency and the loss, and is also influenced by the heat dissipation coefficient and the heat dissipation area. This temperature rise results in a decrease or increase in the actual capacitance. The ceramic dielectric material with negative temperature coefficient is developed to prevent the capacitance reduction of the capacitor caused by temperature rise or other factors in the use process, thereby improving the reliability and having important significance.
Disclosure of Invention
The invention provides a negative temperature coefficient ceramic dielectric material and a preparation method thereof, aiming at solving the problem that the capacitance temperature coefficient of the existing ceramic dielectric material is changed continuously with the positive or negative in the range of 25-200 ℃, and the ceramic dielectric material has high dielectric constant, low dielectric loss and negative capacitance temperature coefficient.
The invention is realized by the following technical scheme: a negative temperature coefficient ceramic dielectric material is composed of 80-90 wt% of 0.94BaO-0.12CaO-0.04TiO2And 10-20% of Y2O3-ZnO-H3BO3And (4) forming.
The method for preparing the negative temperature coefficient ceramic dielectric material comprises the following steps:
(1) mixing the raw material BaCO3、CaCO3And TiO2According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO2Performing material mixing and ball milling, drying in a common oven of 3.3kw at 100 ℃ for 4-5 hours, passing through 120-250 holes/cm2Separating and sieving, heating to 960 deg.C, and maintaining for 2-4 hr to obtain frit A;
(2) mixing raw material Y2O3ZnO and H3BO3According to the formula Y2O3-ZnO-H3BO3Performing material mixing and ball milling, drying in a common oven of 3.3kw at 100 ℃ for 4-5 hours, passing through 120-250 holes/cm2Separating and sieving, heating to 500 deg.C, and maintaining for 2-4 hr to obtain frit B;
(3) blending 10-20% of the frit B and 80-90% of the frit A according to the mass percentage to obtain a blend C;
(4) adding 70ml of absolute ethyl alcohol into the ingredient C, ball-milling for 8 hours on a ball mill with the rotating speed of 400r/min, drying for 4-5 hours at 120 ℃, and passing through 250 holes/cm of 120-2And (3) a sample separation sieve, adding a binding agent accounting for 5-8% of the ingredient C by mass for granulation, pressing into a green compact with the pressure of 8MPa, heating to 400-1250 ℃ at the heating rate of 2 ℃/min, then heating to 1200-1250 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1 hour, and cooling to obtain the ceramic medium.
The ball milling time in the step (1) is 4-6 hours; in the step (1), the heating rate is 5-10 ℃/min. Preferably, the temperature increase rate in step (1) is 7 ℃/min.
The ball milling time in the step (2) is 4-6 hours; in the step (2), the heating rate is 5-10 ℃/min. Preferably, the temperature increase rate in step (2) is 7 ℃/min.
In the step (4), the temperature is raised to 450 ℃ at the temperature raising rate of 2 ℃/min, and then heated to 1200 ℃ and 1250 ℃ at the temperature raising rate of 10 ℃/min for 1 hour. The adhesive in the step (4) is polyvinyl alcohol or paraffin.
Drawings
FIG. 1 is a graph showing the results of temperature coefficient measurements of negative temperature coefficient ceramic dielectric materials prepared in examples 1, 2, 3 and 4.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
Example 1: a negative temperature coefficient ceramic dielectric material, which is composed of 10 percent of Y by mass2O3-ZnO-H3BO3And 90% of 0.94BaO-0.12CaO-0.04TiO2And (4) forming.
The method for preparing the negative temperature coefficient ceramic dielectric material comprises the following steps: mixing the raw material BaCO3、CaCO3And TiO2According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO2Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C for 4 hr in a 3.3kw ordinary oven, and passing through 250 holes/cm2And (4) separating a sample, sieving, heating to 960 ℃ at the speed of 5 ℃/min, and preserving heat at 960 ℃ for 3 hours to obtain the frit A.
Mixing raw material Y2O3ZnO and H3BO3According to the formula Y2O3-ZnO-H3BO3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C for 4 hr in a 3.3kw ordinary oven, and passing through 250 holes/cm2And (4) separating a sample, sieving, heating to 500 ℃ at the speed of 5 ℃/min, and preserving heat at the temperature of 500 ℃ for 3 hours to obtain the frit B.
Mixing, mixing uniformly according to the mass relationship of 90% frit A and 10% frit B, adding 70ml of anhydrous ethanol, ball milling for 8 hr in a ball mill with the rotation speed of 400r/min, drying at 120 deg.C for 4 hr, and passing through 250 holes/cm2And (3) separating a sample, sieving, adding 8 wt% of paraffin wax for granulation, pressing into a green blank with the pressure of 8MPa, heating to 450 ℃ at the heating rate of 2 ℃/min, heating to 1200 ℃ at the heating rate of 10 ℃/min for sintering, keeping the temperature for 1 hour, and cooling to obtain the ceramic medium. The dielectric property test result (test frequency is 1KHz) of the prepared negative temperature coefficient ceramic dielectric material is shown in table 1 and figure 1. In example 1, it can be seen from the graph that the dielectric constant gradually decreases with increasing temperature in the temperature range of 25 ℃ to 200 ℃. The sample has a negative temperature coefficient characteristic. As can be seen from the table, the dielectric constant of the sample was high and the loss was low at room temperature.
Example 2: a negative temperature coefficient ceramic dielectric material, which is prepared from 15 percent of Y by mass2O3-ZnO-H3BO3And 85% of 0.94BaO-0.12CaO-0.04TiO2And (4) forming.
The method for preparing the negative temperature coefficient ceramic dielectric material comprises the following steps: mixing the raw material BaCO3、CaCO3And TiO2According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO2The materials are mixed, ball milled for 5 hours on a ball mill with the rotating speed of 400r/min, and then put in a common oven with the rotating speed of 3.3kw and the rotating speed of 1 hourDrying at 00 deg.C for 5 hr, passing through 200 holes/cm2And (4) separating a sample, sieving, heating to 960 ℃ at the speed of 7 ℃/min, and preserving heat at the temperature of 960 ℃ for 2 hours to obtain the frit A.
Mixing raw material Y2O3ZnO and H3BO3According to the formula Y2O3-ZnO-H3BO3Mixing, ball milling for 5 hr in a ball mill at 400r/min, drying at 100 deg.C for 5 hr in a 3.3kw ordinary oven, and passing through 200 holes/cm2And (4) separating a sample, sieving, heating to 500 ℃ at the speed of 7 ℃/min, and preserving heat at the temperature of 500 ℃ for 2 hours to obtain the frit B.
Mixing, mixing uniformly according to the mass relationship of 85% frit A and 15% frit B, adding 70ml of anhydrous ethanol, ball milling for 8 hr in a ball mill with the rotation speed of 400r/min, drying at 120 deg.C for 4 hr, and passing through 200 holes/cm2And (3) separating a sample, sieving, adding 7 wt% of paraffin wax for granulation, pressing into a green blank with the pressure of 8MPa, heating to 500 ℃ at the heating rate of 2 ℃/min, heating to 1210 ℃ at the heating rate of 10 ℃/min for sintering, preserving heat for 1 hour, and cooling to obtain the ceramic medium. The dielectric property test result (test frequency is 1KHz) of the prepared negative temperature coefficient ceramic dielectric material is shown in table 1 and figure 1. In example 2, it can be seen from the graph that the dielectric constant gradually decreases with increasing temperature in the temperature range of 25 ℃ to 200 ℃. The sample has a negative temperature coefficient characteristic. As can be seen from the table, the dielectric constant of the sample was high and the loss was low at room temperature.
Example 3: a negative temperature coefficient ceramic dielectric material, which is prepared from 20 percent of Y by mass2O3-ZnO-H3BO3And 80% of 0.94BaO-0.12CaO-0.04TiO2And (4) forming.
The method for preparing the negative temperature coefficient ceramic dielectric material comprises the following steps: mixing the raw material BaCO3、CaCO3And TiO2According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO2Mixing, ball milling for 4 hr in a ball mill at 400r/min, drying at 100 deg.C for 5 hr in a 3.3kw ordinary oven, and passing through 120 holes/cm2And (4) separating a sample, sieving, heating to 960 ℃ at the speed of 10 ℃/min, and preserving heat at the temperature of 960 ℃ for 4 hours to obtain the frit A.
Mixing raw material Y2O3ZnO and H3BO3According to the formula Y2O3-ZnO-H3BO3Mixing, ball milling for 4 hr in a ball mill at 400r/min, drying at 100 deg.C for 5 hr in a 3.3kw ordinary oven, and passing through 120 holes/cm2And (4) separating a sample, sieving, heating to 500 ℃ at the speed of 10 ℃/min, and preserving heat at the temperature of 500 ℃ for 4 hours to obtain the frit B.
Mixing, mixing uniformly according to the mass relationship of 80% frit A and 20% frit B, adding 70ml of anhydrous ethanol, ball milling for 8 hr in a ball mill with rotation speed of 400r/min, drying at 120 deg.C for 5 hr, and sieving with 120 holes/cm2And (3) separating a sample, sieving, adding 5 wt% of paraffin wax for granulation, pressing into a green compact with the pressure of 8MPa, heating to 400 ℃ at the heating rate of 2 ℃/min, heating to 1220 ℃ at the heating rate of 10 ℃/min for sintering, keeping the temperature for 1 hour, and cooling to obtain the ceramic medium. The dielectric property test result (test frequency is 1KHz) of the prepared negative temperature coefficient ceramic dielectric material is shown in table 1 and figure 1. In example 3, it can be seen from the graph that the dielectric constant gradually decreases with increasing temperature in the temperature range of 25 ℃ to 200 ℃. The sample has a negative temperature coefficient characteristic. As can be seen from the table, the dielectric constant of the sample was high and the dielectric loss was low at room temperature.
Example 4: a negative temperature coefficient ceramic dielectric material, which is composed of 11 mass percent of Y2O3-ZnO-H3BO3And 89% of 0.94BaO-0.12CaO-0.04TiO2And (4) forming.
The method for preparing the negative temperature coefficient ceramic dielectric material comprises the following steps: mixing the raw material BaCO3、CaCO3And TiO2According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO2Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C for 5 hr in a 3.3kw ordinary oven, and passing through 250 holes/cm2And (4) separating a sample, sieving, heating to 960 ℃ at the speed of 5 ℃/min, and preserving heat at 960 ℃ for 3 hours to obtain the frit A.
Mixing raw material Y2O3ZnO and H3BO3According to the formula Y2O3-ZnO-H3BO3Mixing the materialsBall milling for 6 hours in a ball mill with the rotation speed of 400r/min, drying for 5 hours in a common oven with the temperature of 100 ℃ of 3.3kw, and passing through 200 holes/cm2And (4) separating a sample, sieving, heating to 500 ℃ at the speed of 5 ℃/min, and preserving heat at the temperature of 500 ℃ for 3 hours to obtain the frit B.
Mixing, mixing with 89% of frit A and 11% of frit B, adding 70ml deionized water, ball milling at 400r/min for 8 hr, drying at 120 deg.C for 5 hr, and sieving with 250 holes/cm2And (3) separating a sample, sieving, adding 8 wt% of paraffin wax for granulation, pressing into a green blank with the pressure of 8MPa, heating to 450 ℃ at the heating rate of 2 ℃/min, heating to 1250 ℃ at the heating rate of 10 ℃/min for sintering, preserving heat for 1 hour, and cooling to obtain the ceramic medium. The dielectric property test result (test frequency is 1KHz) of the prepared negative temperature coefficient ceramic dielectric material is shown in table 1 and figure 1. In example 4, it can be seen from the graph that the dielectric constant gradually decreases with increasing temperature in the temperature range of 25 ℃ to 200 ℃. The sample has a negative temperature coefficient characteristic. As can be seen from the table, the dielectric constant of the sample was high and the dielectric loss was low at room temperature.
TABLE 1
In combination with the four examples, as shown in table 1 and fig. 1, in the temperature range of 25 ℃ to 200 ℃, the dielectric constant of the sample decreases with the increase of temperature, and the sample has the characteristics of negative temperature coefficient, higher dielectric constant and small dielectric loss.
The test method and test equipment used in the present invention are as follows:
1. measurement of dielectric constant ε and loss tan δ: the capacitance C and the dielectric loss tan delta (test frequency 1KHz) of the capacitor were measured using a HEWLETT PACKARD 4278A capacitance tester, and the dielectric constant ε was calculated by the following equation:
wherein: c-capacitance of the sample, in pF; d-thickness of the sample piece, unit cm; d-diameter of the sintered D-sample piece in cm.
2. Temperature coefficient of capacitance alphac(25 ℃ C. to 200 ℃ C.) by the following calculation formula:
wherein: reference temperature t0Selecting the temperature of 25 ℃ and alphacHas a unit of 10-6/℃。
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (8)
1. A negative temperature coefficient ceramic dielectric material is characterized in that: consists of 80-90 wt% of 0.94BaO-0.12CaO-0.04TiO2And 10-20% of Y2O3-ZnO-H3BO3And (4) forming.
2. The method for preparing the negative temperature coefficient ceramic dielectric material of claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) mixing the raw material BaCO3、CaCO3And TiO2According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO2Performing material mixing and ball milling, drying in a common oven of 3.3kw at 100 ℃ for 4-5 hours, passing through 120-250 holes/cm2Separating and sieving, heating to 960 deg.C, and maintaining for 2-4 hr to obtain frit A;
(2) mixing raw material Y2O3ZnO and H3BO3According to the formula Y2O3-ZnO-H3BO3Performing material mixing and ball milling, drying in a common oven of 3.3kw at 100 ℃ for 4-5 hours, passing through 120-250 holes/cm2Separating and sieving, heating to 500 deg.C, and maintaining for 2-4 hr to obtain frit B;
(3) blending 10-20% of the frit B and 80-90% of the frit A according to the mass percentage to obtain a blend C;
(4) adding 70ml of absolute ethyl alcohol into the ingredient C, ball-milling for 8 hours on a ball mill with the rotating speed of 400r/min, drying for 4-5 hours at 120 ℃, and passing through 250 holes/cm of 120-2And (3) a sample separation sieve, adding a binding agent accounting for 5-8% of the ingredient C by mass for granulation, pressing into a green compact with the pressure of 8MPa, heating to 400-1250 ℃ at the heating rate of 2 ℃/min, then heating to 1200-1250 ℃ at the heating rate of 10 ℃/min, and preserving heat for 1 hour, and cooling to obtain the ceramic medium.
3. The method of preparing a negative temperature coefficient ceramic dielectric material of claim 2, wherein: ball-milling for 4-6 hours on a ball mill with the rotating speed of 400r/min in the step (1); in the step (1), the heating rate is 5-10 ℃/min.
4. The method of preparing a negative temperature coefficient ceramic dielectric material of claim 3, wherein: the heating rate in the step (1) is 7 ℃/min.
5. The method of preparing a negative temperature coefficient ceramic dielectric material of claim 2, wherein: ball-milling for 4-6 hours on a ball mill with the rotating speed of 400r/min in the step (2); in the step (2), the heating rate is 5-10 ℃/min.
6. The method of preparing a negative temperature coefficient ceramic dielectric material of claim 5, wherein: the heating rate in the step (2) is 7 ℃/min.
7. The method of preparing a negative temperature coefficient ceramic dielectric material of claim 2, wherein: in the step (4), the temperature is raised to 450 ℃ at the temperature raising rate of 2 ℃/min, and then heated to 1200 ℃ and 1250 ℃ at the temperature raising rate of 10 ℃/min for 1 hour.
8. The method of preparing a negative temperature coefficient ceramic dielectric material of claim 2, wherein: the adhesive in the step (4) is polyvinyl alcohol or paraffin.
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