CN115472430A - Wide-temperature-zone high-temperature ceramic capacitor dielectric material and preparation method thereof - Google Patents
Wide-temperature-zone high-temperature ceramic capacitor dielectric material and preparation method thereof Download PDFInfo
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- CN115472430A CN115472430A CN202211146587.8A CN202211146587A CN115472430A CN 115472430 A CN115472430 A CN 115472430A CN 202211146587 A CN202211146587 A CN 202211146587A CN 115472430 A CN115472430 A CN 115472430A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
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- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
Abstract
The invention discloses a wide temperature zone high-temperature ceramic capacitor dielectric material and a preparation method thereof, wherein the chemical composition formula of the material is 0.985 (K) 0.5 Na 0.5 )NbO 3 ‑0.015La(Zn 0.5 Zr 0.5 )O 3 The preparation method comprises the following steps: drying the raw material powder, weighing according to a stoichiometric ratio, and performing ball milling to obtain slurry; drying the slurry, pre-burning, and grinding into powder; ball-milling the powder, drying, and grinding into powder; and granulating the powder, pressing into a sample, discharging glue at high temperature and sintering. The material has high and stable dielectric constant and low dielectric loss in a wide high-temperature range, has nontoxic raw materials, low cost and lower sintering temperature, and has good high-temperature application prospect.
Description
Technical Field
The invention belongs to the technical field of dielectric ceramic materials, and particularly relates to a wide-temperature-zone high-temperature ceramic capacitor dielectric material and a preparation method thereof.
Background
Chip multilayer ceramic capacitors (MLCCs) are widely used in various electronic device fields, such as electronic products for computers, mobile phones, automobiles, televisions, etc., and are currently the most widely used passive component products, because of their advantages of small size, high capacitance, low dielectric loss, high breakdown field strength, and easy miniaturization and integration.
With the continuous development of science and technology, high-temperature ceramic capacitors with working temperature of over 200 ℃ are required to be used in extreme environments such as automotive electronics, aerospace, oil well exploration and the like. However, the maximum working temperature of the conventional EIA X8R type ceramic capacitor is only 150 ℃, and the use temperature requirement of the extreme environment cannot be met, so that the development of a high-temperature ceramic capacitor dielectric material capable of working above 200 ℃ is urgently needed. In addition, the high dielectric constant is beneficial to the miniaturization of the high-temperature ceramic capacitor, and the low dielectric loss and the good dielectric temperature stability ensure that the high-temperature ceramic capacitor reliably and stably works in the working temperature range. In addition, the high-temperature ceramic capacitor dielectric material containing harmful elements such as lead and the like can cause serious harm to human health and ecological environment. Therefore, the development of the high-temperature ceramic capacitor dielectric material which has high and stable dielectric constant and low dielectric loss in a wide high-temperature range and is environment-friendly has important practical significance.
Disclosure of Invention
Aiming at the practical application requirements of the high-temperature ceramic capacitor dielectric material, the invention provides a temperature-stable type high-temperature ceramic capacitor dielectric material and a preparation method thereof. One of the purposes is to provide a dielectric material of a wide-temperature-zone high-temperature ceramic capacitor, which has a chemical composition formula of 0.985 (K) 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 The material has high and stable dielectric constant and low dielectric loss in a wide high-temperature range, and the raw materials are nontoxic. The second purpose is to provide a preparation method of the high-temperature ceramic capacitor dielectric material, which comprises the following steps: drying the raw material powder, weighing according to a stoichiometric ratio, and ball-milling to obtain slurry; drying the slurry, pre-burning, and grinding into powder; ball-milling the powder, drying, and grinding into powder; and granulating the powder, pressing into a sample, discharging glue at high temperature and sintering.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a wide temperature zone high-temperature ceramic capacitor dielectric material is characterized in that: the chemical composition formula of the dielectric material is 0.985 (K) 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 。
The preparation method of the wide-temperature-zone high-temperature ceramic capacitor dielectric material comprises the following steps:
(1) High-purity powder K with the purity of more than 99 percent 2 CO 3 、Na 2 CO 3 、Nb 2 O 5 、La 2 O 3 ZnO and ZrO 2 Oven drying at 120 deg.C for 24 hr, and mixing the dried powder with a weight ratio of 0.985 (K) 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 Precisely weighing (to 4 decimal places);
(2) Putting the precisely weighed powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill with the rotating speed of 360 revolutions per minute by taking zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry A;
(3) Putting the uniformly mixed slurry A into a thermostat at 120 ℃ for drying for 4 hours, grinding the dried slurry into powder by using an agate mortar, pressing the powder into a cylinder with the diameter of 20mm by using a press machine under the pressure of 150Mpa, heating the pressed cylinder to 900 ℃ in a high-temperature furnace at the speed of 5 ℃/min, and preserving heat for 2 hours for pre-sintering;
(4) Grinding the pre-sintered cylinder into uniform powder by using an agate mortar, putting the ground powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill with the rotation speed of 360 revolutions per minute by using zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry B;
(5) Putting the uniformly mixed slurry B into a thermostat at 120 ℃ for drying for 4 hours, grinding the slurry B into powder by using an agate mortar after drying, sieving the powder by using 5wt% of polyvinyl alcohol (PVA) aqueous solution as a binder through a 60-mesh sieve for granulation, and pressing the granulated powder into a cylindrical sample with the diameter of 10mm and the thickness of 1mm by using a press machine under the pressure of 350 Mpa;
(6) Heating the cylindrical sample to 550 ℃ at the speed of 1.5 ℃/min in a high-temperature furnace, preserving heat for 2 hours for glue discharging, putting the sample into an alumina crucible after the glue discharging, covering granulated powder, heating to 1150 ℃ at the speed of 5 ℃/min, preserving heat for 4 hours, and naturally cooling to room temperature along with the furnace.
The invention has the beneficial effects that:
(1) The high-temperature ceramic capacitor dielectric material has high and stable dielectric constant (1892 +/-15%) and low dielectric loss (less than or equal to 0.05) in a wide high-temperature range (83-382 ℃), has nontoxic raw materials, and can be used for high-temperature chip multilayer ceramic capacitors.
(2) The preparation method of the high-temperature ceramic capacitor dielectric material has the advantages of low cost, simple process, lower sintering temperature (1150 ℃), environmental friendliness and the like, and has good industrialization prospect.
Drawings
FIG. 1 shows 0.985 (K) obtained in example 1 of the present invention 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 The dielectric constant, dielectric loss and the change rate of the dielectric constant of the high-temperature ceramic capacitor dielectric material are plotted along with the change of temperature.
FIG. 2 shows 0.99 (K) obtained in comparative example 1 of the present invention 0.5 Na 0.5 )NbO 3 -0.01La(Zn 0.5 Zr 0.5 )O 3 The dielectric constant and dielectric loss of the dielectric material are plotted as a function of temperature.
FIG. 3 is 0.98 (K) of comparative example 2 of the present invention 0.5 Na 0.5 )NbO 3 -0.02La(Zn 0.5 Zr 0.5 )O 3 The dielectric constant and dielectric loss of the dielectric material are plotted as a function of temperature.
Detailed Description
In order to express the present invention more clearly, the present invention will be further illustrated by the following specific examples and comparative examples.
Example 1
The invention provides a wide-temperature-zone high-temperature ceramic capacitor dielectric material, which has the chemical composition formula as follows: 0.985 (K) 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 。
The preparation method of the wide-temperature-zone high-temperature ceramic capacitor dielectric material comprises the following steps:
(1) High-purity powder K with the purity of more than 99 percent 2 CO 3 、Na 2 CO 3 、Nb 2 O 5 、La 2 O 3 ZnO and ZrO 2 Oven drying at 120 deg.C for 24 hr, and mixing the dried powder with a weight ratio of 0.985 (K) 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 The stoichiometric ratio of (c) is accurately weighed (to 4 decimal places);
(2) Putting the precisely weighed powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill with the rotating speed of 360 revolutions per minute by taking zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry A;
(3) Putting the uniformly mixed slurry A into a thermostat at 120 ℃ for drying for 4 hours, grinding the dried slurry into powder by using an agate mortar, pressing the powder into a cylinder with the diameter of 20mm by using a press machine under the pressure of 150Mpa, heating the pressed cylinder to 900 ℃ in a high-temperature furnace at the speed of 5 ℃/min, and preserving heat for 2 hours for pre-sintering;
(4) Grinding the pre-sintered cylinder into uniform powder by using an agate mortar, putting the ground powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill at the rotating speed of 360 revolutions per minute by using zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry B;
(5) Putting the uniformly mixed slurry B into a thermostat at 120 ℃ for drying for 4 hours, grinding the slurry B into powder by using an agate mortar after drying, sieving the powder by using a 60-mesh sieve by using 5wt% of polyvinyl alcohol (PVA) aqueous solution as a binder for granulation, and pressing the granulated powder into a cylindrical sample with the diameter of 10mm and the thickness of 1mm by using a press machine under the pressure of 350 MPa;
(6) Heating the cylindrical sample to 550 ℃ at the speed of 1.5 ℃/min in a high-temperature furnace, preserving heat for 2 hours, discharging glue, putting the sample into an alumina crucible after discharging glue, covering granulated powder, heating to 1150 ℃ at the speed of 5 ℃/min, preserving heat for 4 hours, and naturally cooling to room temperature along with the furnace.
Comparative example 1
For comparison of dielectric properties, 0.99 (K) was prepared as follows 0.5 Na 0.5 )NbO 3 -0.01La(Zn 0.5 Zr 0.5 )O 3 The dielectric material of (2):
(1) High-purity powder K with the purity of more than 99 percent 2 CO 3 、Na 2 CO 3 、Nb 2 O 5 、La 2 O 3 ZnO and ZrO 2 Oven drying at 120 deg.C for 24 hr, and mixing the dried powder with a weight ratio of 0.99 (K) 0.5 Na 0.5 )NbO 3 -0.01La(Zn 0.5 Zr 0.5 )O 3 Precisely weighing (to 4 decimal places);
(2) Putting the precisely weighed powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill with the rotating speed of 360 revolutions per minute by taking zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry A;
(3) Putting the uniformly mixed slurry A into a thermostat at 120 ℃ for drying for 4 hours, grinding the dried slurry into powder by using an agate mortar, pressing the powder into a cylinder with the diameter of 20mm under the pressure of 150Mpa by using a press machine, heating the pressed cylinder to 900 ℃ in a high-temperature furnace at the speed of 5 ℃/min, and preserving heat for 2 hours for pre-sintering;
(4) Grinding the pre-sintered cylinder into uniform powder by using an agate mortar, putting the ground powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill at the rotating speed of 360 revolutions per minute by using zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry B;
(5) Putting the uniformly mixed slurry B into a thermostat at 120 ℃ for drying for 4 hours, grinding the slurry B into powder by using an agate mortar after drying, sieving the powder by using a 60-mesh sieve by using 5wt% of polyvinyl alcohol (PVA) aqueous solution as a binder for granulation, and pressing the granulated powder into a cylindrical sample with the diameter of 10mm and the thickness of 1mm by using a press machine under the pressure of 350 MPa;
(6) Heating the cylindrical sample to 550 ℃ at the speed of 1.5 ℃/min in a high-temperature furnace, preserving heat for 2 hours, discharging glue, putting the sample into an alumina crucible after discharging glue, covering granulated powder, heating to 1150 ℃ at the speed of 5 ℃/min, preserving heat for 4 hours, and naturally cooling to room temperature along with the furnace.
Comparative example 2
For comparison of dielectric properties, 0.98 (K) was prepared as follows 0.5 Na 0.5 )NbO 3 -0.02La(Zn 0.5 Zr 0.5 )O 3 The dielectric material of (2):
(1) High-purity powder K with the purity of more than 99 percent 2 CO 3 、Na 2 CO 3 、Nb 2 O 5 、La 2 O 3 ZnO and ZrO 2 Drying in a constant temperature oven at 120 deg.C for 24 hr, and mixing the dried powder with a weight ratio of 0.98 (K) 0.5 Na 0.5 )NbO 3 -0.02La(Zn 0.5 Zr 0.5 )O 3 The stoichiometric ratio of (c) is accurately weighed (to 4 decimal places);
(2) Putting the precisely weighed powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill with the rotating speed of 360 revolutions per minute by taking zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry A;
(3) Putting the uniformly mixed slurry A into a thermostat at 120 ℃ for drying for 4 hours, grinding the dried slurry into powder by using an agate mortar, pressing the powder into a cylinder with the diameter of 20mm under the pressure of 150Mpa by using a press machine, heating the pressed cylinder to 900 ℃ in a high-temperature furnace at the speed of 5 ℃/min, and preserving heat for 2 hours for pre-sintering;
(4) Grinding the pre-sintered cylinder into uniform powder by using an agate mortar, putting the ground powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill with the rotation speed of 360 revolutions per minute by using zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry B;
(5) Putting the uniformly mixed slurry B into a thermostat at 120 ℃ for drying for 4 hours, grinding the slurry B into powder by using an agate mortar after drying, sieving the powder by using 5wt% of polyvinyl alcohol (PVA) aqueous solution as a binder through a 60-mesh sieve for granulation, and pressing the granulated powder into a cylindrical sample with the diameter of 10mm and the thickness of 1mm by using a press machine under the pressure of 350 Mpa;
(6) Heating the cylindrical sample to 550 ℃ at the speed of 1.5 ℃/min in a high-temperature furnace, preserving heat for 2 hours, discharging glue, putting the sample into an alumina crucible after discharging glue, covering granulated powder, heating to 1150 ℃ at the speed of 5 ℃/min, preserving heat for 4 hours, and naturally cooling to room temperature along with the furnace.
The dielectric materials prepared in the above example 1, comparative example 1 and comparative example 2 were polished on the upper and lower surfaces and silver-coated to prepare a chip capacitor, and the relationship between the dielectric constant and dielectric loss at 100kHz and the change with temperature of these three dielectric materials was measured by a precision impedance analyzer.
The dielectric constant and dielectric loss of the materials prepared in example 1, comparative example 1 and comparative example 2 are shown in the accompanying drawings 1, 2 and 3 respectively. As can be seen from FIGS. 1-3, the temperature stability of the dielectric constant is strongly dependent on the chemical composition, and the temperature stability of the dielectric constant of the dielectric material in FIG. 1 is significantly higher than that of the dielectric materials in FIGS. 2 and 3. Further, the chemical composition formula in example 1 was calculated to be 0.985 (K) 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 The dielectric constant change rate of the dielectric material is related to the change of temperature, as shown in the insert diagram in the attached figure 1, the dielectric material has high and stable dielectric constant (-1892 +/-15%) and low dielectric loss (less than or equal to 0.05) in a wide high-temperature range (83 ℃ -382 ℃), and the dielectric material has great application potential in high-temperature chip multilayer ceramic capacitors.
Claims (2)
1. A wide temperature zone high-temperature ceramic capacitor dielectric material is characterized in that: the chemical composition formula of the dielectric material is 0.985 (K) 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 。
2. The preparation method of the wide-temperature-zone high-temperature ceramic capacitor dielectric material according to claim 1, characterized by comprising the following steps:
(1) High-purity powder K with the purity of more than 99 percent 2 CO 3 、Na 2 CO 3 、Nb 2 O 5 、La 2 O 3 ZnO and ZrO 2 Drying in a constant temperature oven at 120 deg.C for 24 hr, and mixing the dried powder with a weight ratio of 0.985 (K) 0.5 Na 0.5 )NbO 3 -0.015La(Zn 0.5 Zr 0.5 )O 3 The stoichiometric ratio of (c) is accurately weighed (to 4 decimal places);
(2) Putting the precisely weighed powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill with the rotating speed of 360 revolutions per minute by taking zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry A;
(3) Putting the uniformly mixed slurry A into a thermostat at 120 ℃ for drying for 4 hours, grinding the dried slurry into powder by using an agate mortar, pressing the powder into a cylinder with the diameter of 20mm under the pressure of 150Mpa by using a press machine, heating the pressed cylinder to 900 ℃ in a high-temperature furnace at the speed of 5 ℃/min, and preserving heat for 2 hours for pre-sintering;
(4) Grinding the pre-sintered cylinder into uniform powder by using an agate mortar, putting the ground powder into a nylon ball milling tank, and ball milling for 8 hours on a planetary ball mill with the rotation speed of 360 revolutions per minute by using zirconia balls and absolute ethyl alcohol as ball milling media to obtain uniformly mixed slurry B;
(5) Putting the uniformly mixed slurry B into a thermostat at 120 ℃ for drying for 4 hours, grinding the slurry B into powder by using an agate mortar after drying, sieving the powder by using 5wt% of polyvinyl alcohol (PVA) aqueous solution as a binder through a 60-mesh sieve for granulation, and pressing the granulated powder into a cylindrical sample with the diameter of 10mm and the thickness of 1mm by using a press machine under the pressure of 350 Mpa;
(6) Heating the cylindrical sample to 550 ℃ at the speed of 1.5 ℃/min in a high-temperature furnace, preserving heat for 2 hours for glue discharging, putting the sample into an alumina crucible after the glue discharging, covering granulated powder, heating to 1150 ℃ at the speed of 5 ℃/min, preserving heat for 4 hours, and naturally cooling to room temperature along with the furnace.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080239627A1 (en) * | 2007-03-27 | 2008-10-02 | Keith Bridger | High-Temperature Dielectric Materials and Capacitors Made Therefrom |
| CN104291821A (en) * | 2014-09-26 | 2015-01-21 | 天津大学 | Preparation method of potassium-sodium niobate-based multilayer ceramic capacitor dielectric material |
| CN107602115A (en) * | 2017-08-31 | 2018-01-19 | 陕西科技大学 | A kind of unleaded high energy storage density and the stable ceramic material of wide temperature and preparation method thereof |
| CN110498682A (en) * | 2019-09-12 | 2019-11-26 | 桂林理工大学 | A kind of temperature-stable high-temperature ceramic capacitor dielectric material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080239627A1 (en) * | 2007-03-27 | 2008-10-02 | Keith Bridger | High-Temperature Dielectric Materials and Capacitors Made Therefrom |
| CN104291821A (en) * | 2014-09-26 | 2015-01-21 | 天津大学 | Preparation method of potassium-sodium niobate-based multilayer ceramic capacitor dielectric material |
| CN107602115A (en) * | 2017-08-31 | 2018-01-19 | 陕西科技大学 | A kind of unleaded high energy storage density and the stable ceramic material of wide temperature and preparation method thereof |
| CN110498682A (en) * | 2019-09-12 | 2019-11-26 | 桂林理工大学 | A kind of temperature-stable high-temperature ceramic capacitor dielectric material and preparation method thereof |
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