An ultra-low loss high dielectric ceramic composition
By adding oxides of Mg, Sr, Fe and R to perovskite compounds and combining them with specific processes, ultra-low loss high dielectric ceramic materials are prepared, solving the problems of low dielectric constant and high loss of existing materials, and realizing high-frequency and integrated microelectronic device applications.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- KUNSHAN QINGYUAN ELECTRONIC TECHNOLOGY CO LTD
- Filing Date
- 2025-02-27
- Publication Date
- 2026-07-24
AI Technical Summary
Existing dielectric ceramic materials have low dielectric constants and high dielectric losses, making it difficult to meet the requirements of miniaturization, integration, and high frequency operation of microelectronic devices.
Using BaTiO3-based perovskite compounds, combined with oxides of Mg, Sr, Fe and R, an ultra-low loss high dielectric ceramic composition was prepared through specific ball milling, drying, pulverizing, sieving, granulation and sintering processes.
This invention achieves ceramic materials with ultra-low dielectric loss and high dielectric constant, which are suitable for miniaturized, integrated, high-capacity and high-frequency microelectronic devices and have important application value.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of ceramic materials technology, and in particular to an ultra-low loss high dielectric ceramic composition. Background Technology
[0002] The development of microelectronic information technology has put forward requirements for miniaturization, integration, lightweighting 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 typically have a dielectric constant of around 3000 and a loss greater than 1%. To address these issues, Chinese invention patent application CN116589273A discloses a dielectric ceramic composition with main component particles having a perovskite structure represented by the general formula AMO3. The A sites contain Ba, the M sites contain Ti, the D50 of the main component particles is below 960 nm, and the D90 of the main component particles is below 1460 nm. This material exhibits good voltage characteristics in its capacitance, but its dielectric constant needs further improvement, and its dielectric loss needs further reduction.
[0004] It is evident that developing 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 this invention is to overcome the shortcomings 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 objectives, the technical solution adopted by the present invention is: an ultra-low loss high dielectric ceramic composition, comprising the following components in molar amounts: 100 molar parts of a perovskite-type 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 BaTiO3.
[0008] Preferably, the Mg-containing compound is at least one of MgO and MgCO3.
[0009] Preferably, the Sr-containing compound is at least one of strontium oxide and strontium carbonate.
[0010] Preferably, the Fe-containing compound is at least one of ferric 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: BaCO3, TiO2, and Sr-containing compounds are mixed according to the molar ratio, ball-milled, dried, pulverized, passed through a 40-100 mesh standard sieve, and then calcined using water as the dispersion medium.
[0014] Step S2: Add compounds containing Mg, compounds containing Fe, and oxides containing R. Mix them by ball milling with anhydrous ethanol as the dispersion medium, dry, pulverize, pass through a 30-50 mesh standard sieve, granulate, and dry press. Remove the binder from the molded body and then sinter to obtain an ultra-low loss high dielectric ceramic composition.
[0015] Preferably, the calcination temperature in step S1 is 1050-1150℃ and the time is 1-4h.
[0016] Preferably, the pressure for dry pressing in step S2 is 1 T / cm. 2 .
[0017] Preferably, the temperature for discharging the adhesive in step S2 is 550-650℃, and the heat preservation time is 1-3h.
[0018] Preferably, the sintering temperature in step S2 is 1200-1350℃ and the time is 1-4h.
[0019] Due to the application of the above technical solutions, the present invention has the following beneficial effects: Through the rational selection of composition formulation and preparation process parameters, the present invention enables the components to cooperate and work together, giving the manufactured product the advantages of ultra-low dielectric loss and high dielectric constant. It has important practical application value, scientific and technological value, and environmental protection value in the development of MLCC miniaturization, integration, high capacity, high frequency, and high reliability, and has a very broad development prospect. Detailed Implementation
[0020] The following description is intended to disclose the invention and enable those skilled in the art to implement it. The preferred embodiments described below are merely examples, and other obvious variations will occur to those skilled in the art.
[0021] Example 1
[0022] An ultra-low loss high dielectric ceramic composition comprises the following components in molar amounts: 100 moles of a perovskite-type compound containing Ba and Ti, 0.1 moles of a compound containing Mg, 0.1 moles of a compound containing Sr, 0.01 moles of a compound containing Fe, and 0.1 moles of an oxide containing R.
[0023] The perovskite-type compound containing Ba and Ti is BaTiO3; 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 includes the following steps:
[0025] Step S1: BaCO3, TiO2, and Sr-containing compounds are mixed according to the molar ratio, ball-milled, dried, pulverized, passed through a 40-mesh standard sieve, and then calcined using water as the dispersion medium.
[0026] Step S2: Add a compound containing Mg, a compound containing Fe, and an oxide containing R. Mix them by ball milling with anhydrous ethanol as the dispersion medium, dry, pulverize, pass through a 30-mesh standard sieve, granulate, and dry press. Remove the binder from the molded body and then sinter to obtain an ultra-low loss high dielectric ceramic composition.
[0027] The calcination temperature in step S1 is 1050℃, and the time is 1 hour; the dry pressing pressure in step S2 is 1 T / cm. 2 The temperature for removing the adhesive in step S2 is 550℃, and the holding time is 1h; the temperature for sintering in step S2 is 1200℃, and the time is 1h.
[0028] Example 2
[0029] An ultra-low loss high dielectric ceramic composition comprises the following components in molar amounts: 100 molar parts of a perovskite-type 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-type compound containing Ba and Ti is BaTiO3; the compound containing Mg is MgCO3; 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 includes the following steps:
[0032] Step S1: BaCO3, TiO2, and Sr-containing compounds are mixed according to the molar ratio, ball-milled, dried, pulverized, passed through a 60-mesh standard sieve, and then calcined using water as the dispersion medium.
[0033] Step S2: Add compounds containing Mg, compounds containing Fe, and oxides containing R. Mix them by ball milling with anhydrous ethanol as the dispersion medium, dry, pulverize, pass through a 35-mesh standard sieve, granulate, and dry press. Remove the binder from the molded body and then sinter to obtain an ultra-low loss high dielectric ceramic composition.
[0034] The calcination temperature in step S1 is 1080℃, and the time is 2 hours; the dry pressing pressure in step S2 is 1 T / cm. 2 The temperature for removing the adhesive in step S2 is 570℃, and the holding time is 1.5h; the temperature for sintering in step S2 is 1250℃, and the time is 2h.
[0035] Example 3
[0036] An ultra-low loss high dielectric ceramic composition comprises the following components in molar amounts: 100 molar parts of a perovskite-type 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-type compound containing Ba and Ti is BaTiO3; 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 includes the following steps:
[0039] Step S1: BaCO3, TiO2, and Sr-containing compounds are mixed according to the molar ratio, ball-milled, dried, pulverized, passed through an 80-mesh standard sieve, and then calcined using water as the dispersion medium.
[0040] Step S2: Add a compound containing Mg, a compound containing Fe, and an oxide containing R. Mix them by ball milling with anhydrous ethanol as the dispersion medium, dry, pulverize, pass through a 40-mesh standard sieve, granulate, and dry press. Remove the binder from the molded body and then sinter to obtain an ultra-low loss high dielectric ceramic composition.
[0041] The calcination temperature in step S1 is 1100℃, and the time is 2.5h; the dry pressing pressure in step S2 is 1T / cm. 2The temperature for removing the adhesive in step S2 is 600℃, and the holding time is 2h; the temperature for sintering in step S2 is 1310℃, and the time is 2.5h.
[0042] Example 4
[0043] An ultra-low loss high dielectric ceramic composition comprises the following components in molar amounts: 100 molar parts of a perovskite-type 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-type compound containing Ba and Ti is BaTiO3; the compound containing Mg is a mixture of MgO and MgCO3 in a molar ratio of 1:2; 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 ferric 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 includes the following steps:
[0046] Step S1: BaCO3, TiO2, and Sr-containing compounds are mixed according to the molar ratio, ball-milled, dried, pulverized, passed through a 90-mesh standard sieve, and then calcined using water as the dispersion medium.
[0047] Step S2: Add compounds containing Mg, compounds containing Fe, and oxides containing R. Mix them by ball milling with anhydrous ethanol as the dispersion medium, dry, pulverize, pass through a 45-mesh standard sieve, granulate, and dry press. Remove the binder from the molded body and then sinter to obtain an ultra-low loss high dielectric ceramic composition.
[0048] The calcination temperature in step S1 is 1140℃, and the time is 3.5h; the dry pressing pressure in step S2 is 1T / cm. 2 The temperature for removing the adhesive in step S2 is 640℃, and the holding time is 2.5h; the temperature for sintering in step S2 is 1340℃, and the time is 3.5h.
[0049] Example 5
[0050] An ultra-low loss high dielectric ceramic composition comprises the following components in molar amounts: 100 molar parts of a perovskite-type 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-type compound containing Ba and Ti is BaTiO3; 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 includes the following steps:
[0053] Step S1: BaCO3, TiO2, and Sr-containing compounds are mixed according to the molar ratio, ball-milled, dried, pulverized, passed through a 100-mesh standard sieve, and then calcined using water as the dispersion medium.
[0054] Step S2: Add compounds containing Mg, compounds containing Fe, and oxides containing R. Mix them by ball milling with anhydrous ethanol as the dispersion medium, dry, pulverize, pass through a 50-mesh standard sieve, granulate, and dry press. Remove the binder from the molded body and then sinter to obtain an ultra-low loss high dielectric ceramic composition.
[0055] The calcination temperature in step S1 is 1150℃, and the time is 4 hours; the dry pressing pressure in step S2 is 1 T / cm. 2 The temperature for removing the adhesive in step S2 is 650℃, and the holding time is 3h; the temperature for sintering in step S2 is 1350℃, and the time is 4h.
[0056] Comparative Example 1
[0057] An ultra-low loss high dielectric ceramic composition is basically the same as that in Example 1, except that no oxide containing R is added.
[0058] Comparative Example 2
[0059] An ultra-low loss high dielectric ceramic composition is basically the same as that in Example 1, except that no Mg-containing compound is added.
[0060] To further illustrate the beneficial technical effects of the ultra-low loss high dielectric ceramic compositions involved in the various embodiments of the present invention, relevant performance tests were conducted on the ultra-low loss high dielectric ceramic compositions involved in Examples 1-5 and Comparative Examples 1-2. The test results are shown in Table 1. The test methods are as follows: Silver was brushed on both sides of the prepared ultra-low loss high dielectric ceramic composition, and sintered at 640°C for 20 min to prepare silver electrodes. The dielectric properties of the ceramic material were tested using an Agilent 4294A precision impedance analyzer and an E4980A LCR meter, respectively. The insulation resistance was read using a digital ohmmeter (Agilent Technologies 4339B) after applying DC 500V for 60 seconds at room temperature.
[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 product. The combined use of oxides containing R and compounds 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. Their purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly. They should not be used to limit the scope of protection of the present invention. All equivalent changes or modifications made in accordance with the spirit and essence of the present invention should be covered within the scope of protection of the present invention.
Claims
1. A low-loss, high-dielectric ceramic composition, characterized in that, The compound comprises the following components in molar amounts: 100 molar parts of a perovskite-type 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; wherein R is selected from any one of Tb, Tm, and a mixture of Pr, Nd, Pm, and Sm in a molar ratio of 1:1:2:3; the perovskite-type compound containing Ba and Ti is BaTiO3; the compound containing Mg is at least one of MgO and MgCO3; the compound containing Sr is at least one of strontium oxide and strontium carbonate; and the compound containing Fe is at least one of ferric carbonate and ferric oxide.
2. A method for preparing the ultra-low loss high dielectric ceramic composition according to claim 1, characterized in that, Includes the following steps: Step S1: BaCO3, TiO2, and Sr-containing compounds are mixed according to the molar ratio, ball-milled, dried, pulverized, passed through a 40-100 mesh standard sieve, and then calcined using water as the dispersion medium. Step S2: Add compounds containing Mg, compounds containing Fe, and oxides containing R. Mix them by ball milling with anhydrous ethanol as the dispersion medium, dry, pulverize, pass through a 30-50 mesh standard sieve, granulate, and dry press. Remove the binder from the molded body and then sinter to obtain an ultra-low loss high dielectric ceramic composition.
3. The method for preparing the ultra-low loss high dielectric ceramic composition according to claim 2, characterized in that, The calcination temperature in step S1 is 1050-1150℃, and the time is 1-4h.
4. The method for preparing the ultra-low loss high dielectric ceramic composition according to claim 2, characterized in that, The pressure for dry pressing in step S2 is 1 T / cm. 2 The temperature for discharging adhesive in step S2 is 550-650℃, and the heat preservation time is 1-3h.
5. The method for preparing the ultra-low loss high dielectric ceramic composition according to claim 2, characterized in that, The sintering temperature in step S2 is 1200-1350℃, and the time is 1-4h.