CN112521129A - Low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC and preparation method thereof - Google Patents

Low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC and preparation method thereof Download PDF

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CN112521129A
CN112521129A CN202011565436.7A CN202011565436A CN112521129A CN 112521129 A CN112521129 A CN 112521129A CN 202011565436 A CN202011565436 A CN 202011565436A CN 112521129 A CN112521129 A CN 112521129A
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吉岸
王晓慧
金镇龙
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WUXI XINSHENG HUILONG NANO CERAMIC TECHNOLOGY CO LTD
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Abstract

The invention discloses a low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC (multilayer ceramic chip carrier), wherein the phase of the ceramic dielectric material comprises Mg2TiO3、CaTiO3、Ba3B6SiO14And LiBSiO4And the chemical composition of the ceramic dielectric material is aMgO-bCaO-cTiO2‑dBaO‑eB2O3‑fSiO2‑gLi2O, a, b, c, d, e, f and g are respectively and independently expressed as mole percentages. The ceramic dielectric material has lower dielectric constant and dielectric loss, the frequency temperature coefficient of the ceramic dielectric material conforms to the NP0/C0G standard, the sintering temperature of the ceramic dielectric material has wider adaptability, very stable dielectric property and lower production cost, and the ceramic dielectric material can be widely used for manufacturing radio frequency MLCC devices.

Description

Low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC and preparation method thereof
Technical Field
The invention belongs to the technical field of electronic information materials, and particularly relates to a low-dielectric-constant ceramic dielectric material for a low-temperature sintered MLCC (multilayer ceramic chip carrier) and a preparation method thereof.
Background
In order to meet the requirements of communication equipment, military industry, medical equipment and the like on high frequency and high power of electronic components, radio frequency high Q chip type multilayer ceramic capacitors (MLCC) with high current carrying capacity are rapidly developed. The radio frequency high-Q value MLCC has the characteristics of high current carrying capacity, low equivalent series resistance, low equivalent series inductance, high Q value, high series resonance frequency and the like, is widely applied to radio frequency circuits of communication, WLAN, satellite broadcasting equipment, medical electronics, missile systems, aircraft radars, navigation systems and the like, and plays roles of coupling, bypassing, impedance matching, tuning and the like.
At present, a relatively important application short board exists in low-temperature sintering radio-frequency low-dielectric-constant MLCC materials in the MLCC ceramic industry, namely, the stability of the batch of products is poor, and the reason is that the low-temperature sintering state of the adopted dielectric material is not stable enough, particularly, the sintering temperature range of the materials in the 900 ℃ accessory temperature range applied to a pure silver inner electrode is narrow, so that the sintering density and consistency of the materials can be influenced by small change of the sintering environment. The dielectric property of the existing MLCC ceramic dielectric material is unstable, the dielectric loss is large, the absolute value of the frequency temperature coefficient is large, and the NP0/C0G standard cannot be met.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a low dielectric constant ceramic dielectric material for MLCC sintered at low temperature and a preparation method thereof; the ceramic dielectric material has lower dielectric constant and dielectric loss, the frequency temperature coefficient of the ceramic dielectric material conforms to the NP0/C0G standard, the sintering temperature of the ceramic dielectric material has wider adaptability, very stable dielectric property and lower production cost, and the ceramic dielectric material can be widely used for manufacturing radio frequency MLCC devices.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC (multilayer ceramic chip capacitor) is prepared from Mg2TiO3、CaTiO3、Ba3B6SiO14And LiBSiO4And the chemical composition of the ceramic dielectric material is represented as aMgO-bCaO-cTiO2-dBaO-eB2O3-fSiO2-gLi2O, a, b, c, d, e, f and g independently represent mole percentages and satisfy the following conditions: a is more than or equal to 45 mol% and less than or equal to 55 mol%, b is more than or equal to 2 mol% and less than or equal to 5 mol%, c is more than or equal to 20 mol% and less than or equal to 30 mol%, d is more than or equal to 5 mol% and less than or equal to 15 mol%, e is more than or equal to 5 mol% and less than or equal to 15 mol%, f is more than or equal to 5 mol% and less than or equal to 15 mol%, g is more than or equal to 5 mol% and less than or equal to 15 mol%, and a + b + c +.
Further, the dielectric constant DK of the ceramic dielectric material is 13-15; dielectric loss DF is less than or equal to 0.05 percent, and the absolute value of the temperature coefficient of frequency tau f is less than 30 ppm/DEG C.
The invention further provides a preparation method of the low-dielectric-constant ceramic dielectric material for the low-temperature sintered MLCC, which comprises the following steps:
(1) aMgO-bCaO-cTiO according to chemical composition2-dBaO-eB2O3-fSiO2-gLi2O, mixing the starting raw materials, and mixing the raw materials by taking deionized water as a dispersion medium; wherein a, b, c, d, e, f and g respectively and independently represent mole percent and satisfy the following conditions: a is more than or equal to 45 mol% and less than or equal to 55 mol%, b is more than or equal to 2 mol% and less than or equal to 5 mol%, c is more than or equal to 20 mol% and less than or equal to 30 mol%, d is more than or equal to 5 mol% and less than or equal to 15 mol%, e is more than or equal to 5 mol% and less than or equal to 15 mol%, f is more than or equal to 5 mol% and less than or equal to 15 mol%, g is more than or equal to 5 mol% and less than or equal to 15 mol%, and a + b + c +;
wherein, the chemical composition system aMgO-bCaO-cTiO2-dBaO-eB2O3-fSiO2-gLi2O represents an element compound system and can represent a starting material system, but the starting materials for preparing the ceramic dielectric material are not limited to oxides of each element, carbonates, nitrates and the like of each constituent element can be used instead, and the purity of each starting material is more than 99%, but is not particularly limited;
(2) dispersing and crushing the mixed powder to prepare slurry;
(3) drying the slurry, calcining for 2-10 h at 700-900 ℃ to synthesize matrix powder;
(4) dispersing, crushing and drying the matrix powder;
(5) adding a binder into the matrix powder treated in the step (4), mixing, granulating, and pressing into a ceramic blank;
(6) and sintering the ceramic blank at 850-950 ℃ for 2-10 h to prepare the low-dielectric-constant temperature-stable ceramic dielectric material for the MLCC.
Further, in the step (2), a ball milling process or a sand milling process is adopted for dispersing and crushing the powder.
Further, in the step (4), the dispersion and pulverization of the matrix powder is carried out by adopting a ball milling process or a sand milling process.
Further, the binder is selected from one or a mixture of at least two of polyvinyl alcohol solution, polyvinyl butyral solution, acrylic solution and methyl cellulose.
Further, the mass percentage of the binder relative to the ceramic dielectric material is 10-20%.
Further, the pressing pressure of the step (5) is 4Mpa, and the ceramic blank after press forming is a cylinder.
Further, the sintering in the step (6) is performed under an atmospheric atmosphere.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses a chemical composition system aMgO-bCaO-cTiO2-dBaO-eB2O3-fSiO2-gLi2Compounds of each element in O are used as starting materials to prepare the compound containing Mg2TiO3、CaTiO3、Ba3B6SiO14And LiBSiO4The ceramic dielectric material with the stable phase can keep the following radio frequency performance under the condition of low-temperature sintering (850-950 ℃): the dielectric constant DK is 13-15, DF is less than or equal to 0.05 percent (representing the high Q value of the MLCC device), and the temperature coefficient of frequency tau f conforms to the NP0/C0G standard, and the absolute value of the temperature coefficient of frequency tau f is less than 30 ppm/DEG C. The ceramic dielectric material has lower dielectric constant and lower dielectric loss; the sintering temperature of the ceramic dielectric material is 850-950 ℃, the sintering temperature range is as wide as 100 ℃, the dielectric properties in the sintering temperature range are relatively stable, and the influence of the change of the sintering environment on the sintering density and consistency of the material is extremely small; the ceramic dielectric material can meet the technical requirements in the fields of microwave mobile communication, satellite communication, radar systems and the like, and has the advantages of low cost of raw materials and process, no toxic elements such as lead, cadmium, arsenic and the like contained in the material, and important industrial application value.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC (multilayer ceramic chip carrier), wherein the phase of the ceramic dielectric material comprises Mg2TiO3、CaTiO3、Ba3B6SiO14And LiBSiO4The chemical composition system of the ceramic dielectric material can be expressed as aMgO-bCaO-cTiO2-dBaO-eB2O3-fSiO2-gLi2O, a, b, c, d, e, f and g independently represent mole percentages and satisfy the following conditions: a is more than or equal to 45% mol and less than or equal to 55% mol, b is more than or equal to 2% mol and less than or equal to 5% mol, c is more than or equal to 20% mol and less than or equal to 30% mol, d is more than or equal to 5% mol and less than or equal to 15% mol, e is more than or equal to 5% mol and less than or equal to 15% mol, f is more than or equal to 5% mol and less than or equal to 15% mol, g is more than or equal to 5% mol and less than or equal to 15% mol;
chemical composition aMgO-bCaO-cTiO2-dBaO-eB2O3-fSiO2-gLi2O represents only an element compound system, the starting materials for preparing the ceramic dielectric material are not limited to the oxides of each element, and carbonates, nitrates, organic metal salts and the like of each constituent element can be used instead, and the purity of each starting material is more than 99%, but is not particularly limited;
the dielectric constant DK of the ceramic dielectric material is 13-15; dielectric loss DF is less than or equal to 0.05 percent, and the absolute value of the temperature coefficient of frequency tau f is less than 30 ppm/DEG C.
The invention also provides a preparation method of the low-dielectric-constant ceramic dielectric material for the low-temperature sintered MLCC, which comprises the following steps:
(1) aMgO-bCaO-cTiO according to chemical composition2-dBaO-eB2O3-fSiO2-gLi2O, mixing the starting raw materials, and mixing the raw materials by taking deionized water as a dispersion medium; wherein a, b, c, d, e, f,g independently represents mole percent and satisfies the following conditions: a is more than or equal to 45% mol and less than or equal to 55% mol, b is more than or equal to 2% mol and less than or equal to 5% mol, c is more than or equal to 20% mol and less than or equal to 30% mol, d is more than or equal to 5% mol and less than or equal to 15% mol, e is more than or equal to 5% mol and less than or equal to 15% mol, f is more than or equal to 5% mol and less than or equal to 15% mol, g is more than or equal to 5% mol and less than or equal to 15% mol;
the starting materials for preparing the ceramic dielectric material are not limited to the oxides of the elements, and carbonates, nitrates, organic metal salts and the like of the constituent elements can be used instead, and the purity of each starting material is more than 99%, but is not particularly limited;
(2) dispersing and crushing the mixed powder to prepare slurry;
(3) drying the slurry, calcining for 2-10 h at 700-900 ℃ to synthesize matrix powder;
(4) dispersing, crushing and drying the matrix powder;
(5) adding a binder into the matrix powder treated in the step (4), mixing, granulating, and pressing into a ceramic blank;
(6) and sintering the ceramic blank at 850-950 ℃ for 2-10 h to prepare the low-dielectric-constant temperature-stable ceramic dielectric material for the MLCC.
Furthermore, in the step (2), the powder is dispersed and crushed by adopting a ball milling process or a sand milling process; in the step (4), the dispersion and the crushing of the matrix powder adopt a ball milling process or a sand milling process.
The binder used in the granulating process is selected from one or a mixture of at least two of polyvinyl alcohol solution, polyvinyl butyral solution, acrylic solution and methyl cellulose. And the mass percentage of the binder relative to the ceramic dielectric material is 10-20%.
And (5) the pressing pressure of the step (5) is 4Mpa, and the ceramic blank after pressing forming is a cylinder.
The sintering in step (6) is performed in an atmospheric atmosphere.
The following are specific examples of the present invention.
Examples 1 to 6:
the preparation method of the low-dielectric-constant ceramic dielectric material for the low-temperature sintered MLCC comprises the following steps of:
(1) aMgO-bCaO-cTiO according to chemical composition2-dBaO-eB2O3-fSiO2-gLi2O to MgO, CaO, TiO2、BaO、B2O3、SiO2、Li2O, mixing, and mixing the raw materials by taking deionized water as a dispersion medium; wherein a, b, c, d, e, f and g respectively and independently represent mole percent, and the specific values are shown in Table 1;
(2) dispersing and crushing the mixed powder by adopting a ball milling process to prepare slurry;
(3) calcining the slurry at 750 ℃ for 5 hours after drying the slurry to synthesize matrix powder;
(4) dispersing, crushing and drying the matrix powder by adopting a ball milling process;
(5) adding a polyvinyl alcohol solution into the matrix powder treated in the step (4), mixing, granulating, and pressing into a cylindrical ceramic blank; wherein the mass percentage of the polyvinyl alcohol solution relative to the ceramic dielectric material is 10 percent;
(6) and sintering the ceramic blank at the sintering temperature shown in the table 1 for 5 hours to prepare the low-dielectric-constant temperature-stable ceramic dielectric material for the MLCC. The radio frequency performance of the ceramic dielectric material was tested, and the results are shown in table 1.
TABLE 1 respective ratios, sintering temperatures and RF properties of ceramic dielectric materials for examples 1-6
Figure BDA0002860493990000071
The present invention will be further illustrated by comparison with comparative examples, in which MgO, CaO, TiO are each starting material in the production methods of comparative example 1, comparative example 2 and comparative example 32、BaO、B2O3、SiO2、Li2The molar percentages of O (values of a, b, c, d, e, f and g) and the sintering temperatures after granulation and molding are shown in Table 2, and the other preparation processes are the same as those of the inventive examples. Ceramic dielectric material of comparative exampleThe radio frequency properties of the material are shown in table 2.
TABLE 2 respective compounding ratios, sintering temperatures and radio frequency properties of the ceramic dielectric materials of comparative examples 1-3
Figure BDA0002860493990000072
As can be seen from the comparison between examples 1-6 and comparative examples 1-3, the ceramic dielectric materials of examples 1-6 of the present invention have lower dielectric constant and lower dielectric loss, the temperature coefficient of frequency τ f meets the NP0/C0G standard, and the dielectric properties are relatively stable.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents made by the contents of the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.

Claims (9)

1. A low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC is characterized in that: the phase of the ceramic dielectric material comprises Mg2TiO3、CaTiO3、Ba3B6SiO14And LiBSiO4And the chemical composition of the ceramic dielectric material is aMgO-bCaO-cTiO2-dBaO-eB2O3-fSiO2-gLi2O, a, b, c, d, e, f and g independently represent mole percentages and satisfy the following conditions: a is more than or equal to 45 mol% and less than or equal to 55 mol%, b is more than or equal to 2 mol% and less than or equal to 5 mol%, c is more than or equal to 20 mol% and less than or equal to 30 mol%, d is more than or equal to 5 mol% and less than or equal to 15 mol%, e is more than or equal to 5 mol% and less than or equal to 15 mol%, f is more than or equal to 5 mol% and less than or equal to 15 mol%, g is more than or equal to 5 mol% and less than or equal to 15 mol%, and a + b + c +.
2. The low-dielectric-constant temperature-stable ceramic dielectric material for MLCCs according to claim 1, wherein: the dielectric constant DK of the ceramic dielectric material is 13-15; dielectric loss DF is less than or equal to 0.05 percent, and the absolute value of the temperature coefficient of frequency tau f is less than 30 ppm/DEG C.
3. A preparation method of a low-dielectric-constant ceramic dielectric material for low-temperature sintered MLCC is characterized by comprising the following steps:
(1) aMgO-bCaO-cTiO according to chemical composition2-dBaO-eB2O3-fSiO2-gLi2O, mixing the starting raw materials, and mixing the raw materials by taking deionized water as a dispersion medium; wherein a, b, c, d, e, f and g respectively and independently represent mole percent and satisfy the following conditions: a is more than or equal to 45 mol% and less than or equal to 55 mol%, b is more than or equal to 2 mol% and less than or equal to 5 mol%, c is more than or equal to 20 mol% and less than or equal to 30 mol%, d is more than or equal to 5 mol% and less than or equal to 15 mol%, e is more than or equal to 5 mol% and less than or equal to 15 mol%, f is more than or equal to 5 mol% and less than or equal to 15 mol%, g is more than or equal to 5 mol% and less than or equal to 15 mol%, and a + b + c +;
(2) dispersing and crushing the mixed powder to prepare slurry;
(3) drying the slurry, calcining for 2-10 h at 700-900 ℃ to synthesize matrix powder;
(4) dispersing, crushing and drying the matrix powder;
(5) adding a binder into the matrix powder treated in the step (4), mixing, granulating, and pressing into a ceramic blank;
(6) and sintering the ceramic blank at 850-950 ℃ for 2-10 h to prepare the low-dielectric-constant temperature-stable ceramic dielectric material for the MLCC.
4. The method of claim 3, wherein the step (2) of dispersing and pulverizing the powder material is performed by a ball milling process or a sand milling process.
5. The method of claim 3, wherein the step (4) of dispersing and pulverizing the base powder comprises a ball milling process or a sand milling process.
6. The method as claimed in claim 3, wherein the binder is selected from one or a mixture of at least two of polyvinyl alcohol solution, polyvinyl butyral solution, acrylic solution and methyl cellulose.
7. The method according to claim 3, wherein the binder is 10-20% by mass of the ceramic dielectric material.
8. The method for preparing a low dielectric constant ceramic dielectric material for a low temperature sintered MLCC according to claim 3, wherein the pressing pressure of step (5) is 4MPa, and the ceramic green body after press forming is a cylinder.
9. The method of claim 3, wherein the sintering in the step (6) is performed in an atmospheric atmosphere.
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JPH0867556A (en) * 1994-08-26 1996-03-12 Matsushita Electric Ind Co Ltd Dielectric ceramic for planar antenna and planar antenna using the same
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