CN114315344B - 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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- CN114315344B CN114315344B CN202111519213.1A CN202111519213A CN114315344B CN 114315344 B CN114315344 B CN 114315344B CN 202111519213 A CN202111519213 A CN 202111519213A CN 114315344 B CN114315344 B CN 114315344B
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Abstract
The invention belongs to the technical field of ceramic dielectric materials,in order to solve the problem that the capacitance temperature coefficient of the current ceramic dielectric material is positive and negative in the range of 25-200 ℃ and continuously changes, the ceramic dielectric material with negative temperature coefficient and the preparation method thereof are provided, wherein the ceramic dielectric material with negative temperature coefficient consists of 0.94BaO-0.12CaO-0.04TiO with the mass percentage of 80-90 percent 2 And 10-20% of Y 2 O 3 ‑ZnO‑H 3 BO 3 Composition is prepared. 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 greatly developed, and demands for thin, light, small-sized electronic devices such as notebook computers and smart phones have been rapidly increased, so that electronic components are promoted to be miniaturized. The surface assembly technology is a novel assembly technology, which is developed from the basis of a semiconductor chip integration technology and a thick film hybrid integration technology, and the chip components are mounted on the surface of a printed circuit board through wave soldering, reflow soldering and other methods, so that the high-density assembly of a circuit is realized, the circuit area is greatly reduced, and the method is very suitable for the production of 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 patch devices, is mainly applied to oscillation and coupling circuits in various military and civil whole machines, and is applied to the fields of industrial ports such as computers, mobile phones, digital household appliances, automobile appliances and the like. The MLCC consists of three parts, namely an inner electrode, a ceramic layer and a terminal electrode. The dielectric material and the internal electrode are stacked in a staggered manner, and then sintered and formed at a high temperature, and then metal layers are sealed at both ends of the chip, to obtain a monolithic-like structure, so that the MLCC is also called a "monolithic capacitor".
Although the ceramic dielectric materials reported at present are various, the capacitance temperature coefficient of the ceramic materials is positive and negative in the range of 25-200 ℃ and continuously changes. The invention provides a negative capacitance temperature coefficient high dielectric material which can be used as a temperature compensation material and a functional device material, and the invention is helpful for enriching the requirements of the products. In addition, because the capacitor generates power loss and generates heat under the action of voltage in the use process, the temperature of the capacitor is increased, and the temperature increase is determined by the applied alternating voltage, the high and low capacitance of frequency and the loss, and is also influenced by the heat dissipation coefficient and the heat dissipation area. Such a temperature rise results in a decrease or increase in the actual capacitance. The development of the ceramic dielectric material with the negative temperature coefficient is also used for preventing the capacitance of the capacitor from being reduced due to temperature rise or other factors in the use process, thereby improving the reliability and having important significance.
Disclosure of Invention
The invention provides a ceramic dielectric material with negative temperature coefficient and a preparation method thereof, which aims to solve the problem that the capacitance temperature coefficient of the traditional ceramic dielectric material is positive and negative in the range of 25-200 ℃ and continuously changes.
The invention is realized by the following technical scheme: a ceramic dielectric material with negative temperature coefficient is prepared from 80-90% of 0.94BaO-0.12CaO-0.04TiO 2 And 10-20% of Y 2 O 3 -ZnO-H 3 BO 3 Composition is prepared.
The preparation method of the negative temperature coefficient ceramic dielectric material comprises the following steps:
(1) The raw material BaCO 3 、CaCO 3 And TiO 2 According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO 2 Carrying out batching ball milling, drying in a common oven with a temperature of 3.3kw at 100 ℃ for 4-5 hours, passing through 120-250 holes/cm 2 Sample separating sieve, heating to 960 ℃, and preserving heat for 2-4 hours to obtain a frit A;
(2) Raw material Y 2 O 3 ZnO and H 3 BO 3 According to chemical formula Y 2 O 3 -ZnO-H 3 BO 3 Carrying out batching ball milling, drying in a common oven with a temperature of 3.3kw at 100 ℃ for 4-5 hours, passing through 120-250 holes/cm 2 Sample separation sieve, heating to 500 ℃, and preserving heat for 2-4 hours to obtain a frit B;
(3) Mixing 10-20% of the frit B and 80-90% of the frit A according to the mass percentage to obtain a mixture C;
(4) Adding 70ml of absolute ethanol into the mixture 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 120-250 holes/cm 2 And (3) adding 5-8% of binder into a sample separating sieve, granulating, pressing to obtain a green body with the pressure of 8MPa, heating to 400-500 ℃ at the heating rate of 2 ℃/min, heating to 1200-1250 ℃ at the heating rate of 10 ℃/min, preserving heat for 1 hour, and cooling to obtain the ceramic medium.
The ball milling time in the step (1) is 4-6 hours; the temperature rising rate in the step (1) is 5-10 ℃/min. Preferably, the temperature rising rate in the step (1) is 7 ℃/min.
The ball milling time in the step (2) is 4-6 hours; the temperature rising rate in the step (2) is 5-10 ℃/min. Preferably, the temperature rising rate in the step (2) is 7 ℃/min.
The temperature rising rate in the step (4) is to rise to 450 ℃ at a temperature rising rate of 2 ℃/min, and then to rise to 1200-1250 ℃ at a temperature rising rate of 10 ℃/min for 1 hour. The adhesive in the step (4) is polyvinyl alcohol or paraffin wax.
Drawings
FIG. 1 is a graph showing the results of temperature coefficient testing of the ceramic dielectric materials with negative temperature coefficients prepared in examples 1, 2, 3 and 4.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
Example 1: a ceramic dielectric material with negative temperature coefficient is prepared from Y (10 wt.%) 2 O 3 -ZnO-H 3 BO 3 And 90% of 0.94BaO-0.12CaO-0.04TiO 2 Composition is prepared.
The preparation method of the negative temperature coefficient ceramic dielectric material comprises the following steps: the raw material BaCO 3 、CaCO 3 And TiO 2 According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO 2 Compounding, ball milling in a ball mill with rotation speed of 400r/min for 6 hr, drying in a common oven with rotation speed of 3.3kw at 100deg.C for 4 hr, and passing through 250 holes/cm 2 The sample was sieved, heated to 960℃at 5℃per minute and incubated at 960℃for 3 hours to give frit A.
Raw material Y 2 O 3 ZnO and H 3 BO 3 According to chemical formula Y 2 O 3 -ZnO-H 3 BO 3 Compounding, ball milling in a ball mill with rotation speed of 400r/min for 6 hr, drying in a common oven with rotation speed of 3.3kw at 100deg.C for 4 hr, and passing through 250 holes/cm 2 Sample separation sieves are heated to 500 ℃ at 5 ℃/min and are kept at 500 ℃ for 3 hours to obtain the frit B.
Mixing, adding 70ml of absolute ethanol, ball milling for 8 hr in a ball mill with rotation speed of 400r/min, drying at 120deg.C for 4 hr, and passing through 250 holes/cm 2 Sample separating sieve, adding 8wt% stoneGranulating wax, pressing to obtain green compact with pressure of 8MPa, heating to 450 ℃ at a heating rate of 2 ℃/min, heating to 1200 ℃ at a heating rate of 10 ℃/min, sintering, preserving heat for 1 hour, and cooling to obtain the ceramic medium. The test results (test frequency is 1 KHz) of the dielectric properties of the prepared negative temperature coefficient ceramic dielectric materials are shown in table 1 and fig. 1. For example 1, it can be seen 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 is clear from the table, the sample has a high dielectric constant and a low loss at room temperature.
Example 2: a ceramic dielectric material with negative temperature coefficient is prepared from 15% of Y by mass 2 O 3 -ZnO-H 3 BO 3 And 85% of 0.94BaO-0.12CaO-0.04TiO 2 Composition is prepared.
The preparation method of the negative temperature coefficient ceramic dielectric material comprises the following steps: the raw material BaCO 3 、CaCO 3 And TiO 2 According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO 2 Proportioning, ball milling for 5 hours on a ball mill with the rotating speed of 400r/min, drying for 5 hours at 100 ℃ in a common oven with the speed of 3.3kw, and passing through 200 holes/cm 2 Sample separation sieves were warmed to 960 ℃ at 7 ℃/min and incubated at 960 ℃ for 2 hours to obtain frit a.
Raw material Y 2 O 3 ZnO and H 3 BO 3 According to chemical formula Y 2 O 3 -ZnO-H 3 BO 3 Proportioning, ball milling for 5 hours on a ball mill with the rotating speed of 400r/min, drying for 5 hours at 100 ℃ in a common oven with the speed of 3.3kw, and passing through 200 holes/cm 2 Sample separation sieves were heated to 500℃at 7℃per minute and incubated at 500℃for 2 hours to give frit B.
Mixing, adding 70ml of absolute ethanol, ball milling for 8 hr in a ball mill with rotation speed of 400r/min, drying at 120deg.C for 4 hr, and sieving with 200 holes/cm 2 Sample separating sieve, adding paraffin wax in 7wt% to granulate, pressing to obtain green body with pressure of 8MPa, heating to 500 deg.C at 2 deg.C/min, heating to 1210 deg.C at 10 deg.C/min, sintering, maintaining for 1 hr, coolingThe ceramic medium is prepared. The test results (test frequency is 1 KHz) of the dielectric properties of the prepared negative temperature coefficient ceramic dielectric materials are shown in table 1 and fig. 1. For example 2, it can be seen 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 is clear from the table, the sample has a high dielectric constant and a low loss at room temperature.
Example 3: a ceramic dielectric material with negative temperature coefficient is prepared from 20% of Y by mass 2 O 3 -ZnO-H 3 BO 3 And 80% of 0.94BaO-0.12CaO-0.04TiO 2 Composition is prepared.
The preparation method of the negative temperature coefficient ceramic dielectric material comprises the following steps: the raw material BaCO 3 、CaCO 3 And TiO 2 According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO 2 Proportioning, ball milling for 4 hours on a ball mill with the rotating speed of 400r/min, drying for 5 hours at 100 ℃ in a common oven with the speed of 3.3kw, and passing through 120 holes/cm 2 The sample was sieved, heated to 960℃at 10℃per minute and incubated at 960℃for 4 hours to give frit A.
Raw material Y 2 O 3 ZnO and H 3 BO 3 According to chemical formula Y 2 O 3 -ZnO-H 3 BO 3 Proportioning, ball milling for 4 hours on a ball mill with the rotating speed of 400r/min, drying for 5 hours at 100 ℃ in a common oven with the speed of 3.3kw, and passing through 120 holes/cm 2 Sample separation sieves are heated to 500 ℃ at 10 ℃/min and are kept at 500 ℃ for 4 hours to obtain the frit B.
Mixing, adding 70ml of absolute ethanol, ball milling for 8 hr in a ball mill with rotation speed of 400r/min, drying at 120deg.C for 5 hr, and passing through 120 holes/cm 2 And (3) a sample separating sieve, adding 5wt% of paraffin wax for granulating, pressing to obtain a green body 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, sintering, preserving heat for 1 hour, and cooling to obtain the ceramic medium. The test results (test frequency is 1 KHz) of the dielectric properties of the prepared negative temperature coefficient ceramic dielectric materials are shown in table 1 and fig. 1. For example 3, the graph can beIt is seen 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 is clear from the table, the sample has a high dielectric constant and a low dielectric loss at room temperature.
Example 4: a ceramic dielectric material with negative temperature coefficient is prepared from 11% of Y by mass 2 O 3 -ZnO-H 3 BO 3 And 89% of 0.94BaO-0.12CaO-0.04TiO 2 Composition is prepared.
The preparation method of the negative temperature coefficient ceramic dielectric material comprises the following steps: the raw material BaCO 3 、CaCO 3 And TiO 2 According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO 2 Compounding, ball milling in a ball mill with rotation speed of 400r/min for 6 hr, drying in a common oven with rotation speed of 3.3kw at 100deg.C for 5 hr, and passing through 250 holes/cm 2 The sample was sieved, heated to 960℃at 5℃per minute and incubated at 960℃for 3 hours to give frit A.
Raw material Y 2 O 3 ZnO and H 3 BO 3 According to chemical formula Y 2 O 3 -ZnO-H 3 BO 3 Proportioning, ball milling for 6 hours on a ball mill with the rotating speed of 400r/min, drying for 5 hours at 100 ℃ in a common oven with the speed of 3.3kw, and passing through 200 holes/cm 2 Sample separation sieves are heated to 500 ℃ at 5 ℃/min and are kept at 500 ℃ for 3 hours to obtain the frit B.
Mixing, adding 70ml deionized water, ball milling for 8 hr in a ball mill with rotation speed of 400r/min, drying at 120deg.C for 5 hr, and passing through 250 holes/cm 2 And (3) a sample separating sieve, adding 8wt% of paraffin wax for granulating, pressing to obtain a green body 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, sintering, preserving heat for 1 hour, and cooling to obtain the ceramic medium. The test results (test frequency is 1 KHz) of the dielectric properties of the prepared negative temperature coefficient ceramic dielectric materials are shown in table 1 and fig. 1. For example 4, it can be seen 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, at room temperature, the sampleHigh dielectric constant and low dielectric loss.
TABLE 1
From a combination of the four examples, it can be seen from Table 1 and FIG. 1 that the dielectric constants of the samples decrease with increasing temperature in the temperature range of 25℃to 200℃and are characterized by a negative temperature coefficient, and that the dielectric constants are both high and the dielectric losses are small.
The test method and the test equipment used in the invention are as follows:
1. test of dielectric constant ε and loss tan δ: the capacitance C and dielectric loss tan δ (test frequency 1 KHz) of the capacitor were measured using a HEWLETT PACKARD 4278A capacitance tester, and the dielectric constant epsilon was calculated by the following formula:
wherein: capacitance of the C-sample, unit pF; d-thickness of the sample piece, unit cm; d-diameter of sintered sample piece, unit cm.
2. Temperature coefficient of capacitance alpha c (25-200 ℃) calculation formula:
wherein: reference temperature t 0 Selecting 25 deg.C, alpha c Is of the unit of 10 -6 /℃。
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (7)
1. A method of a negative temperature coefficient ceramic dielectric material, characterized by: the method comprises the following steps:
(1) The raw material BaCO 3 、CaCO 3 And TiO 2 According to the chemical formula of 0.94BaO-0.12CaO-0.04TiO 2 Carrying out batching ball milling, drying in a common oven with a temperature of 3.3kw at 100 ℃ for 4-5 hours, passing through 120-250 holes/cm 2 Sample separating sieve, heating to 960 ℃, and preserving heat for 2-4 hours to obtain a frit A;
(2) Raw material Y 2 O 3 ZnO and H 3 BO 3 According to chemical formula Y 2 O 3 -ZnO-H 3 BO 3 Carrying out batching ball milling, drying in a common oven with a temperature of 3.3kw at 100 ℃ for 4-5 hours, passing through 120-250 holes/cm 2 Sample separation sieve, heating to 500 ℃, and preserving heat for 2-4 hours to obtain a frit B;
(3) Mixing 10-20% of the frit B and 80-90% of the frit A according to the mass percentage to obtain a mixture C;
(4) Adding 70ml of absolute ethanol into the mixture 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 120-250 holes/cm 2 Granulating by adding 5-8% of binder with the mass percentage of the ingredients C, pressing into green bodies under the pressure of 8MPa, heating to 400-500 ℃ at the heating rate of 2 ℃/min, heating to 1200-1250 ℃ at the heating rate of 10 ℃/min, preserving heat for 1 hour, and cooling to obtain the ceramic medium.
2. The method of preparing a negative temperature coefficient ceramic dielectric material according to claim 1, wherein: ball milling is carried out on a ball mill with the rotating speed of 400r/min for 4 to 6 hours in the step (1); the temperature rising rate in the step (1) is 5-10 ℃/min.
3. The method of preparing a negative temperature coefficient ceramic dielectric material according to claim 2, wherein: the temperature rising rate in the step (1) is 7 ℃/min.
4. The method of preparing a negative temperature coefficient ceramic dielectric material according to claim 1, wherein: ball milling is carried out on a ball mill with the rotating speed of 400r/min for 4 to 6 hours in the step (2); the temperature rising rate in the step (2) is 5-10 ℃/min.
5. The method for preparing a negative temperature coefficient ceramic dielectric material according to claim 4, wherein: the temperature rising rate in the step (2) is 7 ℃/min.
6. The method of preparing a negative temperature coefficient ceramic dielectric material according to claim 1, wherein: the temperature rising rate in the step (4) is to rise to 450 ℃ at a temperature rising rate of 2 ℃/min, and then to rise to 1200-1250 ℃ at a temperature rising rate of 10 ℃/min for 1 hour.
7. The method of preparing a negative temperature coefficient ceramic dielectric material according to claim 1, wherein: the adhesive in the step (4) is polyvinyl alcohol or paraffin wax.
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