Ultralow-loss high-dielectric ceramic composition

Abstract

The invention discloses an ultra-low-loss high-dielectric ceramic composition, which relates to the technical field of ceramic materials and comprises the following components in parts by mole: 100 parts of Ba and Ti-containing perovskite compound, 0.1-15 parts of Mg-containing compound, 0.1-30 parts of Sr-containing compound, 0.01-3 parts of Fe-containing compound and 0.1-6 parts of R-containing oxide. The ultralow-loss high-dielectric ceramic composition disclosed by the invention is ultralow in dielectric loss and high in dielectric constant.

Description

Technical Field

[0001] The invention relates to the technical field of ceramic materials, and in particular to an ultra-low loss high dielectric ceramic composition. Background Art

[0002] The development of microelectronic information technology has put forward requirements for miniaturization, integration, lightweight and intelligence of devices such as dielectric capacitors. Dielectric materials are a very important component of microelectronic devices. Therefore, people are very concerned about dielectric materials with high dielectric constant and low dielectric loss, especially their application in dielectric energy storage capacitors.

[0003] Conventional dielectric ceramic materials generally have a dielectric constant of about 3000 and a loss of more than 1%. In order to solve the above problem, a Chinese invention patent application with the publication number CN116589273A discloses a dielectric material having a general formula of AMO 3 A dielectric ceramic composition of a main component particle of a perovskite structure, wherein the A site contains Ba, the M site contains Ti, the D50 of the main component particle is less than 960nm, and the D90 of the main component particle is less than 1460nm. The voltage characteristics of the electrostatic capacitance of the material are good, but the dielectric constant needs to be further improved and the dielectric loss needs to be further reduced.

[0004] It can be seen that the development of an ultra-low loss high dielectric ceramic composition with ultra-low dielectric loss and high dielectric constant meets market demand, has broad market value and application prospects, and is of great significance to promoting the development of the field of dielectric ceramic materials. Summary of the invention

[0005] The purpose of the present invention is to overcome the deficiencies of the prior art and provide an ultra-low loss high dielectric ceramic composition with ultra-low dielectric loss and high dielectric constant.

[0006] To achieve the above-mentioned purpose, the technical solution adopted by the present invention is: an ultra-low loss high dielectric ceramic composition, comprising the following components in molar parts: 100 molar parts of a perovskite compound containing Ba and Ti, 0.1-15 molar parts of a compound containing Mg, 0.1-30 molar parts of a compound containing Sr, 0.01-3 molar parts of a compound containing Fe, and 0.1-6 molar parts of an oxide containing R.

[0007] Preferably, the perovskite compound containing Ba and Ti is BaTiO 3 .

[0008] Preferably, the compound containing Mg is MgO, MgCO 3 At least one of .

[0009] Preferably, the compound containing Sr is at least one of strontium oxide and strontium carbonate.

[0010] Preferably, the compound containing Fe is at least one of iron carbonate and ferric oxide.

[0011] Preferably, R is at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu.

[0012] Another object of the present invention is to provide a method for preparing the ultra-low loss high dielectric ceramic composition, comprising the following steps:

[0013] Step S1: BaCO 3 、TiO 2 , the compound containing Sr is prepared according to the molar ratio, ball-milled, dried, crushed, passed through a 40-100 mesh standard sieve and then calcined;

[0014] Step S2, adding a compound containing Mg, a compound containing Fe, and an oxide containing R, using anhydrous alcohol as a dispersion medium for ball milling mixing, drying, crushing, passing through a 30-50 mesh standard sieve, granulating and dry pressing, debinding the molded body, and then sintering to obtain an ultra-low loss high dielectric ceramic composition.

[0015] Preferably, the calcination temperature in step S1 is 1050-1150° C. and the calcination time is 1-4 h.

[0016] Preferably, the pressure of the dry pressing in step S2 is 1T / cm 2 .

[0017] Preferably, the debinding temperature in step S2 is 550-650° C., and the holding time is 1-3 hours.

[0018] Preferably, the sintering temperature in step S2 is 1200-1350° C. and the sintering time is 1-4 hours.

[0019] Due to the application of the above-mentioned technical scheme, the present invention has the following beneficial effects: the present invention enables the components to cooperate with each other through the reasonable selection of the composition formula and the preparation process parameters, giving the manufactured product the advantages of ultra-low dielectric loss and high dielectric constant. In the process of realizing the miniaturization, integration, high capacity, high frequency, high reliability and other characteristics of MLCC, it has important practical application value, scientific and technological value, and environmental protection value, and the development prospects are very broad. DETAILED DESCRIPTION

[0020] The following description is used to disclose the present invention so that those skilled in the art can implement the present invention. The preferred embodiments described below are only examples, and those skilled in the art may think of other obvious variations.

[0021] Embodiment 1

[0022] An ultra-low loss high dielectric ceramic composition comprises the following components in molar parts: 100 molar parts of a perovskite compound containing Ba and Ti, 0.1 molar parts of a compound containing Mg, 0.1 molar parts of a compound containing Sr, 0.01 molar parts of a compound containing Fe, and 0.1 molar parts of an oxide containing R.

[0023] The perovskite compound containing Ba and Ti is BaTiO 3 ; The compound containing Mg is MgO; the compound containing Sr is strontium oxide; the compound containing Fe is iron carbonate; and R is Y.

[0024] A method for preparing the ultra-low loss high dielectric ceramic composition comprises the following steps:

[0025] Step S1: BaCO 3 、TiO 2 , the compound containing Sr is prepared according to the molar ratio, ball-milled, dried, crushed, passed through a 40-mesh standard sieve, and then calcined;

[0026] Step S2, adding a compound containing Mg, a compound containing Fe, and an oxide containing R, using anhydrous alcohol as a dispersion medium for ball milling mixing, drying, crushing, passing through a 30-mesh standard sieve, granulating and dry-pressing, debinding the molded body, and then sintering to obtain an ultra-low loss high dielectric ceramic composition.

[0027] The calcination temperature in step S1 is 1050°C and the time is 1h; the dry pressing pressure in step S2 is 1T / cm 2 ; The debinding temperature in step S2 is 550°C and the holding time is 1h; The sintering temperature in step S2 is 1200°C and the time is 1h.

[0028] Embodiment 2

[0029] An ultra-low loss high dielectric ceramic composition comprises the following components in molar parts: 100 molar parts of a perovskite compound containing Ba and Ti, 5 molar parts of a compound containing Mg, 5 molar parts of a compound containing Sr, 1 molar part of a compound containing Fe, and 2 molar parts of an oxide containing R.

[0030] The perovskite compound containing Ba and Ti is BaTiO 3; The compound containing Mg is MgCO 3 ; The compound containing Sr is strontium carbonate; the compound containing Fe is ferric oxide; and R is La.

[0031] A method for preparing the ultra-low loss high dielectric ceramic composition comprises the following steps:

[0032] Step S1: BaCO 3 、TiO 2 , the compound containing Sr is prepared according to the molar ratio, ball-milled, dried, crushed, passed through a 60-mesh standard sieve, and then calcined;

[0033] Step S2, adding a compound containing Mg, a compound containing Fe, and an oxide containing R, using anhydrous alcohol as a dispersion medium for ball milling mixing, drying, crushing, passing through a 35-mesh standard sieve, granulating and dry-pressing, debinding the molded body, and then sintering to obtain an ultra-low loss high dielectric ceramic composition.

[0034] The calcination temperature in step S1 is 1080°C for 2 hours; the dry pressing pressure in step S2 is 1T / cm 2 The debinding temperature in step S2 is 570°C and the holding time is 1.5h; the sintering temperature in step S2 is 1250°C and the holding time is 2h.

[0035] Embodiment 3

[0036] An ultra-low loss high dielectric ceramic composition comprises the following components in molar parts: 100 molar parts of a perovskite compound containing Ba and Ti, 8 molar parts of a compound containing Mg, 15 molar parts of a compound containing Sr, 1.5 molar parts of a compound containing Fe, and 4 molar parts of an oxide containing R.

[0037] The perovskite compound containing Ba and Ti is BaTiO 3 ; The compound containing Mg is MgO; the compound containing Sr is strontium oxide; the compound containing Fe is ferric oxide; and R is Tb.

[0038] A method for preparing the ultra-low loss high dielectric ceramic composition comprises the following steps:

[0039] Step S1: BaCO 3 、TiO 2 , the compound containing Sr is prepared according to the molar ratio, ball-milled, dried, crushed, passed through an 80-mesh standard sieve, and then calcined;

[0040] Step S2, adding a compound containing Mg, a compound containing Fe, and an oxide containing R, using anhydrous alcohol as a dispersion medium for ball milling mixing, drying, crushing, passing through a 40-mesh standard sieve, granulating and dry pressing, debinding the formed body, and then sintering to obtain an ultra-low loss high dielectric ceramic composition.

[0041] The calcination temperature in step S1 is 1100°C and the time is 2.5 hours; the dry pressing pressure in step S2 is 1T / cm 2 ; The debinding temperature in step S2 is 600°C and the holding time is 2h; The sintering temperature in step S2 is 1310°C and the time is 2.5h.

[0042] Embodiment 4

[0043] An ultra-low loss high dielectric ceramic composition comprises the following components in molar parts: 100 molar parts of a perovskite compound containing Ba and Ti, 13 molar parts of a compound containing Mg, 28 molar parts of a compound containing Sr, 2.5 molar parts of a compound containing Fe, and 5 molar parts of an oxide containing R.

[0044] The perovskite compound containing Ba and Ti is BaTiO 3 ; The compound containing Mg is MgO, MgCO 3 The compound containing Sr is a mixture of strontium oxide and strontium carbonate in a molar ratio of 1:1; the compound containing Fe is a mixture of iron carbonate and ferric oxide in a molar ratio of 2:5; and R is a mixture of Pr, Nd, Pm and Sm in a molar ratio of 1:1:2:3.

[0045] A method for preparing the ultra-low loss high dielectric ceramic composition comprises the following steps:

[0046] Step S1: BaCO 3 、TiO 2 , the compound containing Sr is prepared according to the molar ratio, ball-milled, dried, crushed, passed through a 90-mesh standard sieve, and then calcined;

[0047] Step S2, adding a compound containing Mg, a compound containing Fe, and an oxide containing R, using anhydrous alcohol as a dispersion medium for ball milling mixing, drying, crushing, passing through a 45-mesh standard sieve, granulating and dry pressing, debinding the formed body, and then sintering to obtain an ultra-low loss high dielectric ceramic composition.

[0048] The calcination temperature in step S1 is 1140°C and the time is 3.5 hours; the dry pressing pressure in step S2 is 1T / cm 2The debinding temperature in step S2 is 640°C and the holding time is 2.5h; the sintering temperature in step S2 is 1340°C and the holding time is 3.5h.

[0049] Embodiment 5

[0050] An ultra-low loss high dielectric ceramic composition comprises the following components in molar parts: 100 molar parts of a perovskite compound containing Ba and Ti, 15 molar parts of a compound containing Mg, 30 molar parts of a compound containing Sr, 3 molar parts of a compound containing Fe, and 6 molar parts of an oxide containing R.

[0051] The perovskite compound containing Ba and Ti is BaTiO 3 ; The compound containing Mg is MgO; the compound containing Sr is strontium oxide; the compound containing Fe is ferric oxide; and R is Tm.

[0052] A method for preparing the ultra-low loss high dielectric ceramic composition comprises the following steps:

[0053] Step S1: BaCO 3 、TiO 2 , the compound containing Sr is prepared according to the molar ratio, ball-milled, dried, crushed, passed through a 100-mesh standard sieve, and then calcined;

[0054] Step S2, adding a compound containing Mg, a compound containing Fe, and an oxide containing R, using anhydrous alcohol as a dispersion medium for ball milling mixing, drying, crushing, passing through a 50-mesh standard sieve, granulating and dry pressing, debinding the formed body, and then sintering to obtain an ultra-low loss high dielectric ceramic composition.

[0055] The calcination temperature in step S1 is 1150°C and the time is 4 hours; the dry pressing pressure in step S2 is 1T / cm 2 The debinding temperature in step S2 is 650°C and the holding time is 3h; the sintering temperature in step S2 is 1350°C and the holding time is 4h.

[0056] Comparative Example 1

[0057] An ultra-low loss high dielectric ceramic composition is substantially the same as Example 1, except that no oxide containing R is added.

[0058] Comparative Example 2

[0059] An ultra-low loss high dielectric ceramic composition is substantially the same as Example 1, except that no Mg-containing compound is added.

[0060] In order to further illustrate the beneficial technical effects of the ultra-low loss and high dielectric ceramic compositions involved in each embodiment of the present invention, relevant performance tests were carried out on the ultra-low loss and high dielectric ceramic compositions involved in Examples 1-5 and Comparative Examples 1-2. The test results are shown in Table 1. The test method is as follows: silver is brushed on both sides of the obtained ultra-low loss and high dielectric ceramic compositions, sintered at 640°C for 20 minutes, silver electrodes are fired, and the dielectric properties of the ceramic materials are tested using an Agilent 4294A precision impedance analyzer and an E4980A LCR tester, respectively; the insulation resistance is the resistance value after applying DC500V for 60 seconds at room temperature using a digital resistance meter (4339B manufactured by Agilent Technologies).

[0061] Table 1

[0062]

[0063] As can be seen from Table 1, the ultra-low loss high dielectric ceramic compositions involved in the embodiments of the present invention have a larger dielectric constant, lower dielectric loss and higher insulation resistance than the comparative products, and the combined use of an oxide containing R and a compound containing Mg has a beneficial effect on improving the above-mentioned properties.

[0064] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with this technology to understand the contents of the present invention and implement them accordingly. They cannot be used to limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. An ultra-low loss high dielectric ceramic composition, characterized in that: The invention comprises the following components in molar parts: 100 molar parts of a perovskite compound containing Ba and Ti, 0.1-15 molar parts of a compound containing Mg, 0.1-30 molar parts of a compound containing Sr, 0.01-3 molar parts of a compound containing Fe, and 0.1-6 molar parts of an oxide containing R.

2. The ultra-low loss high dielectric ceramic composition according to claim 1, characterized in that: The perovskite compound containing Ba and Ti is BaTiO3.

3. The ultra-low loss high dielectric ceramic composition according to claim 1, characterized in that: The compound containing Mg is at least one of MgO and MgCO3.

4. The ultra-low loss high dielectric ceramic composition according to claim 1, characterized in that: The compound containing Sr is at least one of strontium oxide and strontium carbonate.

5. The ultra-low loss high dielectric ceramic composition according to claim 1, characterized in that: The compound containing Fe is at least one of iron carbonate and ferric oxide.

6. The ultra-low loss high dielectric ceramic composition according to claim 1, characterized in that: The R is at least one of Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu.

7. A method for preparing the ultra-low loss high dielectric ceramic composition according to any one of claims 1 to 6, characterized in that: The steps include: Step S1, BaCO3, TiO2, and a compound containing Sr are mixed according to a molar ratio, ball-milled, dried, crushed, passed through a 40-100 mesh standard sieve, and then calcined; Step S2, adding a compound containing Mg, a compound containing Fe, and an oxide containing R, using anhydrous alcohol as a dispersion medium for ball milling mixing, drying, crushing, passing through a 30-50 mesh standard sieve, granulating and dry pressing, debinding the molded body, and then sintering to obtain an ultra-low loss high dielectric ceramic composition.

8. The method for preparing the ultra-low loss high dielectric ceramic composition according to claim 7, characterized in that: The calcination temperature in step S1 is 1050-1150° C. and the calcination time is 1-4 hours.

9. The method for preparing the ultra-low loss high dielectric ceramic composition according to claim 7, characterized in that: The pressure of the dry pressing in step S2 is 1T / cm 2 ; The debinding temperature in step S2 is 550-650°C and the insulation time is 1-3h.

10. The method for preparing the ultra-low loss high dielectric ceramic composition according to claim 7, characterized in that: The sintering temperature in step S2 is 1200-1350° C. and the sintering time is 1-4 hours.

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