CN115010488B - Low-firing low-dielectric high-Q high-stability microwave porcelain for capacitor - Google Patents

Low-firing low-dielectric high-Q high-stability microwave porcelain for capacitor Download PDF

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CN115010488B
CN115010488B CN202210050318.5A CN202210050318A CN115010488B CN 115010488 B CN115010488 B CN 115010488B CN 202210050318 A CN202210050318 A CN 202210050318A CN 115010488 B CN115010488 B CN 115010488B
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weight
sintering aid
microwave
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CN115010488A (en
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程华容
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Beijing Yuanlu Hongyuan Electronic Technology Co ltd
Yuanliuhongyuan Suzhou Electronic Technology Co ltd
BEIJING YUANLIU HONGYUAN ELECTRONIC TECHNOLOGY CO LTD
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Beijing Yuanlu Hongyuan Electronic Technology Co ltd
Yuanliuhongyuan Suzhou Electronic Technology Co ltd
BEIJING YUANLIU HONGYUAN ELECTRONIC TECHNOLOGY CO LTD
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Abstract

The invention discloses a low-firing microwave porcelain for a low-dielectric high-Q high-stability capacitor, which comprises the following components in percentage by weight: main materials, a sintering aid and a modified additive. The main material is Ca 0.9‑y‑z Sr 0.1 Mg y Mn z (Zr 0.96 Ti 0.02 Hf 0.02 ) m O 1+2m Wherein y is more than or equal to 0.05 and less than or equal to 0.10, z is more than or equal to 0.02 and less than or equal to 0.08, and m is more than or equal to 0.95 and less than or equal to 1.05; the sintering aid component comprises: baO, B 2 O 3 、SiO 2 And CuO; the modifying additive comprises: y is 2 O 3 、Dy 2 O 3 、Sc 2 O 3 、Al 2 O 3 、CaMgSi 2 O 6 And BaZrO 3 . The microwave ceramic material can be sintered in a reducing atmosphere, can be used for preparing a low-sintering, low-dielectric, high-Q, high-stability and narrow-temperature-coefficient copper electrode multilayer ceramic dielectric capacitor, and has a good application prospect in the field of radio frequency microwaves. And (3) putting the main material, the sintering aid and the modified additive into a ball milling tank filled with a ball milling medium, performing ball milling, drying, grinding and sieving to obtain the microwave porcelain.

Description

Low-firing low-dielectric high-Q high-stability microwave porcelain for capacitor
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a low-firing microwave ceramic material for a low-dielectric high-Q high-stability capacitor.
Background
Ceramic capacitors are one of the electronic components that are used in large numbers in electronic devices, and are widely used in electronic circuits such as blocking direct current, storing electric charges, filtering, coupling, and tuning loops. A multilayer ceramic capacitor (MLCC) is one of chip passive components, and has the advantages of small volume, high specific volume, low dielectric loss, low price, and the like, so that the application range of the MLCC is wider and wider.
The traditional multilayer ceramic capacitor electrode material is a pure palladium or palladium-silver alloy electrode, the cost of the silver-palladium electrode material accounts for more than 70% of the cost of the whole capacitor, and along with the rapid development of the capacitor manufacturing technology, the high frequency, high power, miniaturization and base metal become inevitable trends, so that the inner electrode material for the capacitor is gradually changed into a base metal electrode material such as nickel, copper and the like from a precious metal silver-palladium material.
The nickel and copper electrode materials are not very different in price but the copper electrode has better conductivity. The capacitor manufacture requires co-firing of electrode materials and ceramic materials, and sintering of both nickel and copper electrode capacitors in a reducing atmosphere, wherein the sintering temperature of the nickel electrode is usually 1200-1300 ℃ and the sintering temperature of the copper electrode capacitor is not higher than 1050 ℃. The copper electrode capacitor product can meet the high-frequency and high-Q requirement of the microwave capacitor due to the low price of the electrode but the conductivity of the electrode is similar to that of silver, and the development trend of the modern communication technology is met. How to provide a microwave porcelain material for a low-firing low-dielectric high-Q high-stability capacitor, which is used for cooling sintering and is matched with a copper electrode in a co-firing way is a technical problem to be solved urgently.
Disclosure of Invention
Aiming at the defects in the problems, the invention provides a microwave porcelain for a low-firing low-dielectric high-Q high-stability capacitor, which comprises the following components in part by weight: main materials, a sintering aid and a modified additive.
The main material is Ca 0.9-y-z Sr 0.1 Mg y Mn z (Zr 0.96 Ti 0.02 Hf 0.02 ) m O 1+2m Wherein y is more than or equal to 0.05 and less than or equal to 0.10, z is more than or equal to 0.02 and less than or equal to 0.08, and m is more than or equal to 0.95 and less than or equal to 1.05; the sintering aid comprises: baO, B 2 O 3 、SiO 2 And CuO; the modifying additive comprises: y is 2 O 3 、Dy 2 O 3 、Sc 2 O 3 、Al 2 O 3 、CaMgSi 2 O 6 And BaZrO 3 。
As a further improvement of the invention, the microwave porcelain comprises the following components in parts by weight: 100 weight portions of main material, 9.0 to 12.0 weight portions of sintering aid and Y 2 O 3 0.5 to 3.0 weight portions of Dy 2 O 3 1.0 to 2.0 weight portionsAmount of Sc 2 O 3 0 to 1.0 part by weight of Al 2 O 3 1.0 to 5.0 weight portions of CaMgSi 2 O 6 4.0 to 6.0 parts by weight and BaZrO 3 1.0 to 2.0 parts by weight.
As a further improvement of the invention, the particle size of the sintering aid is controlled to be D 50 ≤0.8μm、D 90 ≤2.0μm。
As a further improvement of the invention, baO and SiO 2 The particle sizes of both CuO and CuO are controlled to be D 50 Less than or equal to 0.3 mu m; baO is made from a carbonate, oxide or hydroxide of Ba; siO 2 2 From oxides or hydroxides of Si; cuO is made from a carbonate, oxide or hydroxide of Cu.
As a further improvement of the invention, the microwave porcelain can be prepared by the following preparation method:
step one, putting a main material, a sintering aid and a modified additive into a ball milling tank filled with a ball milling medium;
step two, adding water, and then performing ball milling, drying, grinding and sieving; adding the sieved mixture material into an absolute ethyl alcohol solution in which polyvinyl butyral is dissolved for granulation;
and step three, pressing the granulated ceramic blank into a wafer, discharging glue in an air furnace, and sintering and densifying in an atmosphere sintering furnace.
As a further improvement of the invention, in the first step, the weight portions are as follows: 100 weight portions of main material, 9.0 to 12.0 weight portions of sintering aid and Y 2 O 3 0.5 to 3.0 weight portions of Dy 2 O 3 1.0 to 2.0 parts by weight of Sc 2 O 3 0 to 1.0 part by weight of Al 2 O 3 1.0 to 5.0 weight portions of CaMgSi 2 O 6 4.0 to 6.0 parts by weight and BaZrO 3 1.0 to 2.0 parts by weight.
As a further improvement of the invention, the ball milling media are zirconia balls.
As a further improvement of the invention, in the first step, the main material is made of CaCO 3 、SrCO 3 、Mg(OH) 2 、MnCO 3 、TiO 2 、ZrO 2 And HfO 2 In proportion ofBall milling, mixing, stoving, sieving and calcining at 1100-1200 deg.c for 2-5 hr.
As a further improvement of the invention, in the first step, the sintering aid is composed of BaO and B 2 O 3 、SiO 2 Mixing with CuO in proportion, melting and cold quenching at 1100-1200 deg.C in a crucible, ball milling, and sieving.
As a further improvement of the invention, in the second step, the mass percentage of the polyvinyl butyral ester in the absolute ethyl alcohol solution is 10wt%.
As a further improvement of the invention, in the third step, the ceramic blank after granulation is pressed into round pieces, and the glue is discharged for 6 hours at 400 ℃ in an air furnace, and then sintered and densified at 980 +/-30 ℃ in an atmosphere sintering furnace.
The invention also provides an application of the microwave porcelain in preparing a multilayer ceramic capacitor, the microwave porcelain can be used for preparing a copper electrode multilayer ceramic capacitor, and the prepared capacitor has the characteristics of low sintering, low dielectric, high Q, high stability and narrow temperature coefficient.
Compared with the prior art, the invention has the beneficial effects that:
1. the main material selected by the microwave porcelain has a stable perovskite phase structure, and is easy for batch production; mg, mn and Hf in the perovskite structure enter perovskite lattices in a solid solution mode, zr is effectively prevented from being separated out in a second phase due to the addition of Mn, and meanwhile free MgO is prevented from reducing the service life of a material system.
2. CaMgSi selected by the invention 2 O 6 And Al 2 O 3 Has the advantages of low dielectric constant (7-9), positive temperature coefficient of capacity (+ 105 ppm/DEG C), low loss and the like, and BaZrO 3 The material has high dielectric constant (32-35) and negative temperature coefficient of capacity (-330 ppm/DEG C), and the material not only has good compatibility with the main material of the perovskite structure, but also can effectively adjust the dielectric constant and the temperature coefficient of the capacity by adjusting the proportion.
3. The sintering aid selected by the invention not only has an effective cooling and sintering effect, but also has a low dielectric constant, and the modifier is added on the basis, particularly the anti-reducing property of a material system can be improved and grains can be refined by adding the rare earth elements Y, dy and Sc in a matching way, so that the obtained dielectric material realizes good microwave performance and keeps the temperature characteristic of C0G within the range of-55-125 ℃.
4. The microwave ceramic material can be sintered in a reducing atmosphere and can be used for preparing a low-sintering, low-dielectric, high-Q, high-stability and narrow-temperature-coefficient copper electrode multilayer ceramic capacitor.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a low-firing microwave porcelain for a low-dielectric high-Q high-stability capacitor. The main material is Ca 0.9-y-z Sr 0.1 Mg y Mn z (Zr 0.96 Ti 0.02 Hf 0.02 ) m O 1+2m (y is more than or equal to 0.05 and less than or equal to 0.10, z is more than or equal to 0.02 and less than or equal to 0.08, and m is more than or equal to 0.95 and less than or equal to 1.05); the sintering aid comprises: baO, B 2 O 3 、SiO 2 And CuO; the modifying additive comprises: y is 2 O 3 、Dy 2 O 3 、Sc 2 O 3 、Al 2 O 3 、CaMgSi 2 O 6 And BaZrO 3 . The microwave porcelain comprises the following components in parts by weight: 100 weight portions of main material, 9.0 to 12.0 weight portions of sintering aid and Y 2 O 3 0.5 to 3.0 weight portions of Dy 2 O 3 1.0 to 2.0 parts by weight of Sc 2 O 3 0 to 1.0 part by weight of Al 2 O 3 1.0 to 5.0 weight portions of CaMgSi 2 O 6 4.0 to 6.0 parts by weight and BaZrO 3 1.0 to 2.0 parts by weight.
Main material Ca 0.9-y-z Sr 0.1 Mg y Mn z (Zr 0.96 Ti 0.02 Hf 0.02 ) m O 1+2m Weighing raw material CaCO according to stoichiometric ratio (y is more than or equal to 0.05 and less than or equal to 0.10, z is more than or equal to 0.02 and less than or equal to 0.08, and m is more than or equal to 0.95 and less than or equal to 1.05) 3 、SrCO 3 、Mg(OH) 2 、MnCO 3 、TiO 2 、ZrO 2 And HfO 2 Adding deionized water and grinding medium, ball milling, drying, sieving, and calcining at 1100-1200 deg.c for 2-5 hr. A few Ca are listed below 0.9-y-z Sr 0.1 Mg y Mn z (Zr 0.96 Ti 0.02 Hf 0.02 ) m O 1+2m The main material comprises y more than or equal to 0.05 and less than or equal to 0.10, z more than or equal to 0.02 and less than or equal to 0.08, and m more than or equal to 0.95 and less than or equal to 1.05. The y, z and m values of the main material ZL1 are respectively 0.1, 0.08 and 0.95; the values of y, z and m in the main material ZL2 are respectively 0.08, 0.05 and 1.0; the values of y, z and m in the main material ZL3 are respectively 0.05, 0.02 and 1.05; other proportions can also meet the requirements, and are not set forth herein.
The combustion assistant BBSC is composed of BaO and B 2 O 3 、SiO 2 Mixing with CuO in proportion, melting, cold quenching and reprocessing at 1100-1200 ℃, and controlling the particle size of the sintering aid to be D 50 ≤0.8μm、D 90 Less than or equal to 2.0 mu m. Wherein, baO and SiO 2 And CuO in submicron order (D) 50 Less than or equal to 0.3 μm) carbonate, oxide or hydroxide powder. Specifically, 33.45-40.35 wt% of BaO and 20.50-21.51 wt% of B are used as sintering aid BBSC 2 O 3 25.0 to 41.67 weight percent of SiO 2 And 4.38 to 13.15 weight percent of CuO are weighed according to the proportion, mixed and sieved by a 40-mesh sieve, a platinum crucible is adopted for melting cold quenching, secondary ball milling is carried out until the granularity reaches a certain value, and then the mixture is packaged for later use. The BBSC sintering aid composition and melting temperature are listed below, wherein the sintering aid GF1 is 40.35wt% of BaO and 21.51wt% of B 2 O 3 25.0% by weight of SiO 2 And 13.15wt% of CuO, the melting temperature is 1200 ℃; the sintering aid GF2 is 33.45wt percent of BaO and 20.50wt percent of B 2 O 3 41.67wt% SiO 2 And 4.38wt% of CuO, the melting temperature being 1100 ℃; other ratios and melting temperatures may also meet the requirements and are not set forth herein.
Mixing the main material and the combustion-supporting agentThe modified additive comprises the following components in parts by weight: 100 weight portions of main material, 9.0 to 12.0 weight portions of sintering aid and Y 2 O 3 0.5 to 3.0 weight portions of Dy 2 O 3 1.0 to 2.0 parts by weight of Sc 2 O 3 0 to 1.0 part by weight of Al 2 O 3 1.0 to 5.0 weight portions of CaMgSi 2 O 6 4.0 to 6.0 parts by weight and BaZrO 3 1.0 to 2.0 weight portions, and then the mixture is put into a ball milling tank filled with zirconia balls; adding a proper amount of deionized water, and then performing ball milling, drying, grinding and sieving; adding the sieved mixture material into 10wt% of absolute ethyl alcohol solution of polyvinyl butyral ester for granulation; pressing the granulated ceramic blank into a wafer, discharging glue in an air furnace, then discharging glue in the air furnace for 6 hours at 400 ℃, and then sintering and densifying in an atmosphere sintering furnace at 980 +/-30 ℃ to obtain the microwave ceramic material.
The sintered microwave ceramic wafer is subjected to double-side polishing, diameter and thickness measurement, silver coating, silver firing and other processes to manufacture a simple single-chip capacitor, and the capacitance, loss, insulation resistance, the change value of the capacitance along with the temperature and the like are tested. 5 samples were taken for each formulation test and the final values given are the average of the calculated samples.
The microwave porcelain for the low-firing low-dielectric high-Q high-stability capacitor provided by the invention is described in detail below, the formula design is shown in table 1 (the components in table 1 are in parts by mass, wherein the main material is 100 parts by mass), and the performance of a microwave porcelain wafer sample after sintering in an atmosphere furnace is shown in table 2.
Table 1 recipe ingredients and content composition
Figure BDA0003473731960000051
Table 2 shows the corresponding performance parameters of the formulation in Table 1, wherein the temperature coefficient of capacitance is measured in the range of-55 deg.C to 125 deg.C, and the insulation resistance is measured for 1 minute. Thus, the dielectric constant of the wafer capacitor sample prepared by the microwave porcelain provided by the invention is 18-20, and the loss (1.7-4.0) x 10 -4 Room temperature insulation resistivity > 10 12 Omega cm even up to 10 13 Omega cm, and the content temperature coefficient is within (0 + -30) ppm/DEG C, which is C0G, in the temperature range of-55 to 125 ℃.
TABLE 2 disc capacitor sample Properties corresponding to the formulations
Figure BDA0003473731960000061
A multilayer ceramic capacitor is trial-produced according to a preferable formula 8 of comprehensive properties (size 0603 made by English), both an inner electrode and an outer electrode of the capacitor are made of copper, and the performance test of the capacitor after sintering in a reducing atmosphere is shown in Table 3 (Q value test frequency 1 GHz). The multi-layer ceramic capacitor shown in the table 3 has low loss, the Q value is up to 1730, and the multi-layer ceramic capacitor has a smaller capacity temperature coefficient (within the range of minus 55-125 ℃, is narrower than C0G, and meets the requirement of (0 +/-15) ppm/DEG C).
TABLE 3 Electrical Properties of the trial-produced multilayer ceramic dielectric capacitors
Figure BDA0003473731960000062
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A low-firing low-dielectric high-Q high-stability microwave porcelain for capacitors, which comprises: main materials, a sintering aid and a modified additive;
the main material is Ca 0.9-y-z Sr 0.1 Mg y Mn z (Zr 0.96 Ti 0.02 Hf 0.02 ) m O 1+2m Wherein y is more than or equal to 0.05 and less than or equal to 0.10, z is more than or equal to 0.02 and less than or equal to 0.08, and m is more than or equal to 0.95 and less than or equal to 1.05;
the sintering aid comprises: baO, B 2 O 3 、SiO 2 And CuO;
the modifying additive comprises: y is 2 O 3 、Dy 2 O 3 、Sc 2 O 3 、Al 2 O 3 、CaMgSi 2 O 6 And BaZrO 3 ，
The microwave porcelain comprises the following components in parts by weight:
100 weight portions of main material, 9.0 to 12.0 weight portions of sintering aid and Y 2 O 3 0.5 to 3.0 weight portions of Dy 2 O 3 1.0 to 2.0 parts by weight of Sc 2 O 3 0 to 1.0 part by weight of Al 2 O 3 1.0 to 5.0 weight portions of CaMgSi 2 O 6 4.0 to 6.0 parts by weight and BaZrO 3 1.0 to 2.0 parts by weight.
2. The microwave porcelain according to claim 1, wherein the particle size of the sintering aid is controlled to be D 50 ≤0.8μm、D 90 ≤2.0μm。
3. Microwave porcelain according to claim 1, characterized in that the BaO, siO 2 The particle sizes of both CuO and CuO are controlled to be D 50 ≤0.3μm；
The BaO is prepared from carbonate, oxide or hydroxide of Ba;
the SiO 2 From oxides or hydroxides of Si;
the CuO is made of carbonate, oxide or hydroxide of Cu.
4. The microwave porcelain according to claim 1, wherein the main material is made of CaCO 3 、SrCO 3 、Mg(OH) 2 、MnCO 3 、TiO 2 、ZrO 2 And HfO 2 Ball milling and mixing evenly according to the proportion, drying, sieving and calcining for 2-5 hours at 1100-1200 ℃.
5. The microwave porcelain according to claim 1, wherein the sintering aid is selected from the group consisting of BaO,B 2 O 3 、SiO 2 Mixing with CuO in proportion, melting and cold quenching at 1100-1200 ℃ in a crucible, ball milling and sieving to obtain the alloy.
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