CN110105065B - Temperature-stable ceramic dielectric material and preparation method thereof - Google Patents
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Abstract
The invention relates to the field of ceramic dielectric materials, in particular to a temperature-stable ceramic dielectric material and a preparation method thereof. Is prepared from KNbO (5-20 wt%)310-20% of SrTiO3And 70-85% of BiMg0.1Ti0.7O3The components are as follows. The invention provides a temperature stable ceramic dielectric material, SrTiO3‑BiMg0.1Ti0.7O3The dielectric ceramic has moderate sintering temperature generally around 1050 ℃, has higher dielectric constant, adjustable temperature coefficient of capacity and lower loss, and is a dielectric ceramic material with excellent performance. The invention selects SrTiO3‑BiMg0.1Ti0.7O3System, adopting KNbO addition3The method is a doping modification method, so that the temperature stability is met, and the advantages of high dielectric constant and low dielectric loss are achieved.
Description
Technical Field
The invention relates to the field of ceramic dielectric materials, in particular to a temperature-stable ceramic dielectric material and a preparation method thereof.
Background
With the development of integrated circuits, terminals of electronic communication devices are being miniaturized, and chip multilayer ceramic capacitors can be well adapted to the trend, so that the integrated circuits are widely applied. With the development of the technology, the excellent performance of the capacitor is more and more obvious, and the capacitor tends to gradually replace tantalum capacitors and electrolytic capacitors. Hundreds of billions of products are sold in the market all the year round, and are widely applied to various surface-mounted circuits of electronic information products
In recent years, with the popularization and wide application of electronic information equipment in various industries, especially in some special industries and extreme environments, higher requirements are put forward on the dielectric temperature change rate performance of the multilayer ceramic capacitor. In the field of automobile control, for example, an Electronic Control Unit (ECU) of an engine, an anti-lock braking system (ABS), an air/fuel ratio control module, etc. installed in an engine compartment, a high temperature operating temperature range of the multilayer ceramic capacitor is required to reach about 150 ℃. Meanwhile, in the fields of avionics, automotive electronics, environmental testing and the like, the electronic system is required to work normally under extremely harsh conditions, which requires that the high-temperature working temperature of the multilayer ceramic capacitor is extended to more than 150 ℃ and even more than 200 ℃. The dielectric temperature characteristics of the large-capacity capacitor in a high-temperature section have become one of the key factors for the normal operation of the electronic equipment in a high-temperature environment. The study of temperature stable dielectric materials over a wider temperature range is currently an urgent need
At present, more temperature-stable ceramic capacitor materials are reported to be a tungsten bronze structure ceramic system, a lead-based relaxor ferroelectric ceramic system and BaTiO3The dielectric ceramic materials such as the ferroelectric ceramic system and the like have the problems of containing a large amount of heavy metal lead, high sintering temperature, narrow working temperature range, low dielectric constant, high loss and the like.
Disclosure of Invention
The invention aims to provide a temperature-stable ceramic dielectric material and a preparation method thereof, and the material has the advantages of high dielectric constant, low dielectric loss, no lead and environmental protection, and the sintering temperature of the method is low.
The invention is realized by the following technical scheme: a temperature stable ceramic dielectric material is prepared from 5-20 wt% KNbO310-20% of SrTiO3And 70-85% of BiMg0.1Ti0.7O3The components are as follows.
The invention further provides a preparation method of the temperature-stable ceramic dielectric material, which comprises the following steps:
(1) the raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Carrying out burdening and ball milling, heating to 800 ℃, and preserving heat for 2-4 hours to prepare a frit A;
(2) 5-20% of KNbO by mass310-20% of SrTiO3And 70-85% of the frit A are subjected to secondary batching to obtain a batching B;
(3) ball milling the material B, adding 5-8 wt% of adhesive for granulation, pressing into green body, heating to 400-500 deg.c, heating to 1020-1050 deg.c, maintaining for 1 hr, and cooling to obtain the temperature stable ceramic dielectric material.
As a further improvement of the technical scheme of the preparation method, in the step (1), the heating rate of heating to 800 ℃ is 5-10 ℃/min.
As a further improvement of the technical scheme of the preparation method, in the step (1), the heating rate of heating to 800 ℃ is 7 ℃/min.
As a further improvement of the technical scheme of the preparation method, in the step (3), the heating is carried out to 400-500 ℃ at the heating rate of 2 ℃/min, and then the heating is carried out to 1020-1050 ℃ at the heating rate of 10 ℃/min.
As a further improvement of the technical scheme of the preparation method, the adhesive is polyvinyl alcohol or paraffin.
As a further improvement of the technical scheme of the preparation method, the ball-milled materials in the steps (1) and (3) need to pass through 250 pores/cm of 120-2And (5) separating and screening.
The invention provides a temperature stable ceramic dielectric material, SrTiO3-BiMg0.1Ti0.7O3The dielectric ceramic has a perovskite structure, has moderate sintering temperature generally around 1050 ℃, has higher dielectric constant, adjustable capacity temperature coefficient and lower loss, and is a dielectric ceramic material with excellent performance. The invention selects SrTiO3-BiMg0.1Ti0.7O3System, adopting KNbO addition3For the method of doping modification, K+And Nb5+Can be respectively dissolved in the A site and the B site of the perovskite structure of the system in a solid mode, and the lattice parameter of the system is changed, so that the working temperature range of the perovskite structure is widened, and the perovskite structure has the advantages of high dielectric constant and low dielectric loss. The dielectric constant of the ceramic dielectric material obtained by the preparation method is between 850-900, and the dielectric loss of the ceramic dielectric material is between 0.01 and 0.02.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a graph showing the test results of temperature coefficients TCC of ceramic dielectric materials obtained in example 1, example 2, example 3 and example 4. As can be seen from the figure: as the temperature rises, the temperature coefficients all show a slow rising trend, peak values appear around 25 ℃, and then gradually decline, but the temperature coefficients are all within +/-15%, and the temperature stability is high.
FIG. 2 is an SEM image of a ceramic dielectric material prepared according to the present invention. As can be seen from the figure: the crystal grain growth is good, the appearance is regular and uniform, the average grain diameter is 2.3 mu m, and the density is high.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
A temperature stable ceramic dielectric material is prepared from 5-20 wt% KNbO310-20% of SrTiO3And 70-85% of BiMg0.1Ti0.7O3The components are as follows.
A preparation method of a temperature-stable ceramic dielectric material comprises the following steps:
(1) the raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Carrying out burdening and ball milling, heating to 800 ℃, and preserving heat for 2-4 hours to prepare a frit A;
(2) 5-20% of KNbO by mass310-20% of SrTiO3And 70-85% of the frit A are subjected to secondary batching to obtain a batching B;
(3) ball milling the material B, adding 5-8 wt% of adhesive for granulation, pressing into green body, heating to 400-500 deg.c, heating to 1020-1050 deg.c, maintaining for 1 hr, and cooling to obtain the temperature stable ceramic dielectric material.
In the invention, the binder added in the step (3) can volatilize in the subsequent heating process, and the sintering process in the step (3) of the invention is mainly used for leading the ceramic dielectric material to achieve the aim of densification.
In the present invention, it is preferable that the temperature increase rate of the temperature increase to 1100 ℃ in the step (1) is 5 to 10 ℃/min.
In the present invention, it is preferable that in the step (1), the temperature increase rate of the temperature increase to 1100 ℃ is 7 ℃/min.
In the present invention, it is preferable that in the step (3), the temperature is raised to 400-500 ℃ at a temperature raising rate of 2 ℃/min, and then heated to 1020-1050 ℃ at a temperature raising rate of 10 ℃/min.
In the present invention, preferably, the binder is polyvinyl alcohol or paraffin wax.
In the present invention, preferably, the ball-milled material obtained in the steps (1) and (3) is sieved through a 120-250-hole/cm 2 sample sieve. In specific implementation, the medium for ball milling is zirconia balls with the diameter of 1 mm.
The test method and test equipment used in the present invention are as follows:
1. measurement of dielectric constant ε and loss tan. delta
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. Test of temperature coefficient TCC (-55 ℃ to 200 ℃)
The capacitance temperature coefficient (the testing frequency is 1KHz) of the capacitor is obtained by measuring the capacitance variation of the sample with temperature by using a model 6425 WAYKERR bridge, a GZ-ESPEC MC-710F high-low temperature box and a special tester for the C-T/V characteristic of the HM27002 type capacitor, and the calculation formula is as follows:
wherein: the reference temperature is 25 ℃, C0At a temperature of 25 ℃ in volume, C1Is a temperature t1The capacity of (c).
The technical solution of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
The raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C in a 3.3kw ordinary oven, and passing through 250 holes/cm2And (4) separating a sample, sieving, heating to 800 ℃ at the speed of 5 ℃/min, and preserving heat at 800 ℃ for 3 hours to obtain the frit A.
Performing secondary batching according to the KNbO of 5 percent 310% of SrTiO3Mixing with 85% of frit A, ball milling with deionized water in a ball mill at 400r/min for 8 hr, drying at 120 deg.C, and sieving with 250 pores/cm2And (3) separating a sample, sieving, adding 8 wt% of paraffin wax for granulation, pressing into a green body, heating to 450 ℃ according to the heating rate of 2 ℃/min, heating to 1020 ℃ according to the heating rate of 10 ℃/min for sintering, preserving heat for 1 hour, and cooling to obtain the ceramic dielectric material.
The results of the dielectric properties test (test frequency of 1KHz) for the ceramic dielectric materials of the above examples are detailed in Table 1 below and FIG. 1.
TABLE 1
Item | Firing temperature (. degree. C.) | Incubation time (h) | Dielectric constant ε | Loss tan delta |
Example 1 | 1020 | 1 | 850 | 0.015 |
Example 2
The raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C in a 3.3kw ordinary oven, and passing through 250 holes/cm2And (4) separating a sample, sieving, heating to 800 ℃ at the speed of 5 ℃/min, and preserving heat at 800 ℃ for 3 hours to obtain the frit A.
Performing secondary batching according to KNbO of 10 percent 320% of SrTiO3Mixing with 70% of frit A, ball milling with deionized water in a ball mill at 400r/min for 8 hr, drying at 120 deg.C, and sieving with 250 pores/cm2And (3) separating a sample, sieving, adding 8 wt% of paraffin wax for granulation, pressing into a green body, heating to 450 ℃ according to the heating rate of 2 ℃/min, heating to 1030 ℃ according to the heating rate of 10 ℃/min for sintering, preserving heat for 1 hour, and cooling to obtain the ceramic dielectric material.
The results of the dielectric property test (test frequency of 1KHz) of the above examples are shown in Table 2 below and FIG. 1.
TABLE 2
Item | Firing temperature (. degree. C.) | Incubation time (h) | Dielectric constant ε | Loss tan delta |
Example 2 | 1030 | 1 | 870 | 0.013 |
Example 3
The raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C in a 3.3kw ordinary oven, and passing through 250 holes/cm2And (4) separating a sample, sieving, heating to 800 ℃ at the speed of 5 ℃/min, and preserving heat at 800 ℃ for 3 hours to obtain the frit A.
Performing secondary batching according to 20 percent KNbO 310% of SrTiO3Mixing with 70% of frit A, ball milling with deionized water in a ball mill at 400r/min for 8 hr, drying at 120 deg.C, and sieving with 250 pores/cm2And (3) separating a sample, sieving, adding 8 wt% of paraffin wax for granulation, pressing into a green body, heating to 450 ℃ according to the heating rate of 2 ℃/min, heating to 1040 ℃ according to the heating rate of 10 ℃/min for sintering, preserving heat for 1 hour, and cooling to obtain the ceramic dielectric material.
The results of the dielectric property test (test frequency of 1KHz) of the above examples are shown in Table 3 below and FIG. 1.
TABLE 3
Item | Firing temperature (. degree. C.) | Incubation time (h) | Dielectric constant ε | Loss tan delta |
Example 3 | 1040 | 1 | 880 | 0.0121 |
Example 4
The raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C in a 3.3kw ordinary oven, and passing through 250 holes/cm2And (4) separating a sample, sieving, heating to 800 ℃ at the speed of 5 ℃/min, and preserving heat at 800 ℃ for 3 hours to obtain the frit A.
Performing secondary batching according to KNbO of 10 percent 310% of SrTiO3Mixing with 80% of frit A, ball milling with deionized water in a ball mill at 400r/min for 8 hr, drying at 120 deg.C, and sieving with 250 pores/cm2And (3) separating a sample, sieving, adding 8 wt% of paraffin wax for granulation, pressing into a green body, heating to 450 ℃ according to the heating rate of 2 ℃/min, heating to 1050 ℃ according to the heating rate of 10 ℃/min for sintering, preserving heat for 1 hour, and cooling to obtain the ceramic dielectric material.
The results of the dielectric property test (test frequency of 1KHz) of the above examples are shown in Table 4 below and FIG. 1.
TABLE 4
Item | Firing temperature (. degree. C.) | Incubation time (h) | Dielectric constant ε | Loss tan delta |
Example 4 | 1050 | 1 | 900 | 0.0181 |
Example 5
The raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C in a 3.3kw ordinary oven, and passing through 120 holes/cm2And (4) screening, heating to 800 ℃ at the speed of 10 ℃/min, and preserving heat for 2 hours at 800 ℃ to obtain the frit A.
Performing secondary batching according to KNbO of 10 percent 310% of SrTiO3Mixing with 80% of frit A, ball milling with deionized water in a ball mill at 400r/min for 8 hr, drying at 120 deg.C, and sieving with 120 pores/cm2And (3) separating a sample, sieving, adding 6 wt% of polyvinyl alcohol for granulation, pressing into a green body, heating to 400 ℃ according to the heating rate of 2 ℃/min, heating to 1050 ℃ according to the heating rate of 10 ℃/min, sintering, keeping the temperature for 1 hour, and cooling to obtain the ceramic dielectric material.
Example 6
The raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C in a common oven of 3.3kw, and passing through 200 holes/cm2And (4) separating a sample, sieving, heating to 800 ℃ at the speed of 7 ℃/min, and preserving heat for 4 hours at the temperature of 800 ℃ to obtain the frit A.
Performing secondary batching according to KNbO of 10 percent 310% of SrTiO3Mixing with 80% of frit A, ball milling with deionized water in a ball mill at 400r/min for 8 hr, drying at 120 deg.C, and sieving with 200 holes/cm2And (3) separating a sample, sieving, adding 5 wt% of polyvinyl alcohol for granulation, pressing into a green body, heating to 500 ℃ at the heating rate of 2 ℃/min, heating to 1050 ℃ at the heating rate of 10 ℃/min, sintering, keeping the temperature for 1 hour, and cooling to obtain the ceramic dielectric material.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (6)
1. The preparation method of the temperature-stable ceramic dielectric material is characterized by comprising the following steps of:
(1) the raw material Bi2O3MgO and TiO2According to the general formula BiMg0.1Ti0.7O3Carrying out burdening and ball milling, heating to 800 ℃, and preserving heat for 2-4 hours to prepare a frit A;
(2) 5-20% of KNbO by mass310-20% of SrTiO3And 70-85% of the frit A are subjected to secondary batching to obtain a batching B;
(3) ball milling the material B, adding 5-8 wt% of adhesive for granulation, pressing into green body, heating to 400-500 deg.c, heating to 1020-1050 deg.c, maintaining for 1 hr, and cooling to obtain the temperature stable ceramic dielectric material.
2. The method according to claim 1, wherein in step (1), the heating rate of the ceramic dielectric material to 800 ℃ is 5-10 ℃/min.
3. The method according to claim 2, wherein in the step (1), the heating rate of the temperature to 800 ℃ is 7 ℃/min.
4. The method as claimed in claim 1, wherein the step (3) is performed by heating to 400-500 ℃ at a heating rate of 2 ℃/min, and then heating to 1020-1050 ℃ at a heating rate of 10 ℃/min.
5. The method of claim 1, 2, 3 or 4, wherein the binder is polyvinyl alcohol or paraffin wax.
6. The method as claimed in claim 5, wherein the ball-milled materials obtained in steps (1) and (3) are processed through 250 pores/cm and 120 pores/cm2And (5) separating and screening.
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CN1562867A (en) * | 2004-03-16 | 2005-01-12 | 天津大学 | High frequency ceramic dielectric material in thermal stability and preparaton method |
CN101314545A (en) * | 2008-07-02 | 2008-12-03 | 广东风华高新科技股份有限公司 | Spray coating method for producing dielectric ceramic powder body and obtained products thereof |
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