CN113004030A - High-dielectric-constant ceramic dielectric material and preparation method thereof - Google Patents
High-dielectric-constant ceramic dielectric material and preparation method thereof Download PDFInfo
- Publication number
- CN113004030A CN113004030A CN202110287412.8A CN202110287412A CN113004030A CN 113004030 A CN113004030 A CN 113004030A CN 202110287412 A CN202110287412 A CN 202110287412A CN 113004030 A CN113004030 A CN 113004030A
- Authority
- CN
- China
- Prior art keywords
- heating
- temperature
- basio
- dielectric
- hours
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 35
- 239000003989 dielectric material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 48
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000007873 sieving Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000004615 ingredient Substances 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 7
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 10
- 230000008859 change Effects 0.000 description 7
- 238000005245 sintering Methods 0.000 description 5
- 230000003247 decreasing effect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62665—Flame, plasma or melting treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3215—Barium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/36—Glass starting materials for making ceramics, e.g. silica glass
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Plasma & Fusion (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
- Ceramic Capacitors (AREA)
Abstract
The invention discloses a high dielectric constant ceramic dielectric material and a preparation method thereof; belongs to the technical field of ceramic dielectric materials; the material is prepared from 80-90% of BaO-5.75Fe by mass percent2O30.5NiO and 10-20% BaSiO3Forming microcrystalline glass; ball-milling, heating, mixing and blank-making raw materials, heating to 1100-1150 ℃ step by step according to a certain heating rate, preserving heat for 0.5-2 hours, and cooling to obtain a ceramic dielectric material; the problem that the capacitance temperature coefficient of the existing ceramic dielectric material has large variation range within the range of-55 ℃ to 150 ℃ is solved; has a dielectric constantHigh dielectric loss and stable temperature coefficient.
Description
Technical Field
The invention belongs to the technical field of ceramic dielectric materials, and relates to a high-dielectric-constant ceramic dielectric material and a preparation method thereof.
Background
At present, scientific and economic development is unprecedented, and with the change of science and technology, modern materials are developed towards functional materials, nano materials and the like. The functional material is a material which displays functions and effects of various properties such as current, light, heat, sound and the like, is inseparable from the development of modern science and technology, and has irreplaceable functions in high-tech fields such as sensing, national defense, aviation, exploration, energy, weapons and the like.
In recent years, with the rapid advance of electronic science and technology, the living habits of people have changed from turning to the ground. The popularization of smart phones and 4G communication technologies greatly shortens the distance between people; the development of wearable equipment greatly facilitates the life of people; the appearance of high-performance computers has become the most important tool in scientific work process of people, and all the high-performance computers benefit from the miniaturization and integration of circuit chips in electronic equipment, and as an indispensable passive device in a circuit, namely a multilayer ceramic capacitor, the high-performance computers have the characteristics of large specific volume, long service life, small volume, high reliability, suitability for surface assembly and the like besides the characteristic of blocking direct current and alternating current of the capacitor.
The dielectric material is an important material in functional materials, and is widely applied in the technical field of the current. The development of electronic components requires that the dielectric material has a high dielectric constant, low dielectric loss, a proper curie temperature, good frequency, temperature stability and the like. The modern electronic industry has higher and higher requirements on integration level, and electronic components as important components of the electronic components not only have good dielectric properties, but also need to be modified to make the electronic components smaller and lighter and well matched with use occasions. Therefore, the high dielectric materials with the above characteristics become the research focus at present, and there are many reports on the high dielectric materials, such as barium titanate, barium strontium titanate, and Pb1–xCax(Fe1/2,Nb1/2)O3And the like. However, these ceramic materials have problems such as high sintering temperature, low dielectric constant, and high loss.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a high-dielectric-constant ceramic dielectric material and a preparation method thereof. The ceramic dielectric material has high dielectric constant, low dielectric loss and stable capacitance temperature coefficient.
Specifically, the present invention is achieved by the following technical means in order to achieve the above object.
A high-dielectric-constant ceramic dielectric material is prepared from BaO-5.75Fe (80-90 wt.%)2O30.5NiO and 10-20% BaSiO3And (3) microcrystalline glass.
A preparation method of a high dielectric constant ceramic dielectric material comprises the following steps:
a) raw material Ba (NO)3)2、Fe(NO3)3And Ni (NO)3)2According to the chemical formula BaO-5.75Fe2O3Mixing and ball milling 0.5NiO, heating to 750-.
b) Mixing the raw material BaCO3And SiO2According to the chemical formula BaSiO3Ball milling the mixture, heating to 1300 ℃ to 1500 ℃, keeping the temperature for 1-3 hours, continuing heating to 1400 ℃ to 1700 ℃, keeping the temperature for 0.5-1 hour, and cooling to obtain BaSiO3Microcrystalline glass.
c) 10-20% of BaSiO by mass percent3And (3) mixing the microcrystalline glass and 80-90% of the frit A to obtain a mixture B.
d) And granulating the ingredient B, pressing into a green body, heating to 400-500 ℃ at the heating rate of 2-4 ℃/min, heating to 1100-1150 ℃ at the heating rate of 8-12 ℃/min, preserving the heat for 0.5-2 hours, and cooling to obtain the ceramic dielectric material.
Preferably, the temperature rise rate in step a is 5-10 ℃/min.
More preferably, the heating rate in the step a is 7 ℃/min.
Preferably, in both the step a and the step b, the ingredients after ball milling are dried and pass through 250 holes/cm of 120-2And sieving and then heating.
Preferably, the temperature reduction in the step b is to be reduced to 800 ℃ at 700-.
Preferably, in step d, the pressure for pressing into the green body is 8-9 MPa.
Preferably, the granulating of the ingredient B is to add water into the ingredient B, ball-mill the mixture, dry and sieve the mixture, and add a binding agent with the mass percent of 5-8% of the ingredient B for granulation.
Preferably, the adhesive is polyvinyl alcohol or paraffin.
Preferably, in step d, the temperature rising rate is to rise to 450 ℃ at a temperature rising rate of 2 ℃/min, and then to be heated to 1100 ℃ and 1150 ℃ at a temperature rising rate of 10 ℃/min, and the temperature is maintained for 1 hour.
Compared with the prior art, the invention has the following beneficial effects:
the invention solves the problem that the capacitance temperature coefficient of the existing ceramic dielectric material is positive, negative and continuously changed within the range of-55 to 150 ℃, and provides a high dielectric constant ceramic dielectric material and a preparation method thereof, wherein the high dielectric constant ceramic dielectric material is prepared from 80 to 90 mass percent of BaO-5.75Fe2O30.5NiO and 10-20% BaSiO3The material has the advantages that the dielectric constant of the material is increased and then reduced along with the increase of the temperature, and the change range is small; has the characteristics of high dielectric constant, low dielectric loss and stable temperature coefficient.
Drawings
In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention more clearly understood, the following drawings are taken for illustration:
FIG. 1 is a graph showing the results of temperature coefficient measurements of high dielectric constant ceramic dielectric materials prepared in examples 1, 2, 3 and 4.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solution of the present invention is described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
Example 1
A high-dielectric-constant ceramic dielectric material is prepared from 10% BaSiO3Microcrystalline glass and 90% BaO-5.75Fe2O3-0.5NiO composition.
The preparation method of the high dielectric constant ceramic dielectric material comprises the following steps: raw material Ba (NO)3)2、Fe(NO3)3And Ni (NO)3)2According to the chemical formula BaO-5.75Fe2O30.5NiO, ball milling for 6 hours in a ball mill with the rotating speed of 400r/min, drying for 4 hours in a common oven with the temperature of 100 ℃ of 3.3kw, and passing through 250 holes/cm2And (4) separating a sample, sieving, heating to 800 ℃ at the speed of 5 ℃/min, and preserving heat at 800 ℃ for 3 hours to obtain the frit A.
Mixing the raw material BaCO3And SiO2According to the chemical formula BaSiO3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C for 4 hr in a 3.3kw ordinary oven, and passing through 250 holes/cm2Separating the sample, sieving, heating to 1400 deg.C, holding for 2 hr, continuing heating to 1600 deg.C, holding for 0.5 hr, cooling to 800 deg.C, holding for 2 hr, and cooling to room temperature to obtain BaSiO3Microcrystalline glass.
The mixture is prepared according to 90 percent of frit A and 10 percent of BaSiO3Uniformly mixing the microcrystalline glass according to the mass relation, adding 70ml of deionized water, ball-milling for 8 hours on a ball mill with the rotating speed of 400r/min, drying for 4 hours at 120 ℃, and passing through 250 holes/cm2And (3) separating a sample, sieving, adding 8wt% of paraffin wax for granulation, pressing into a green blank with the pressure of 8MPa, heating to 450 ℃ at the heating rate of 2 ℃/min, heating to 1100 ℃ at the heating rate of 10 ℃/min for sintering, keeping the temperature for 1 hour, and cooling to obtain the ceramic medium. The dielectric property test results (test frequency is 1 KHz) of the prepared high dielectric constant ceramic dielectric material are shown in Table 1 and figure 1. In example 1, it can be seen from the graph that in the temperature range of-55 ℃ to 150 ℃, the dielectric constant is increased and then decreased with the increase of the temperature, and the change range is not large. As can be seen from the table, the dielectric constant of the sample was high and the loss was low at room temperature.
Example 2
A high-dielectric-constant ceramic dielectric material is prepared from 15% BaSiO3Microcrystalline glass and 85% BaO-5.75Fe2O3-0.5NiO composition.
Preparing the high mediumThe method for preparing the dielectric ceramic material with the electric constant comprises the following steps: raw material Ba (NO)3)2、Fe(NO3)3And Ni (NO)3)2According to the chemical formula BaO-5.75Fe2O30.5NiO, ball milling for 5 hours on a ball mill with the rotating speed of 400r/min, drying for 5 hours in a common oven with the temperature of 100 ℃ of 3.3kw, and passing through 200 holes/cm2And (4) separating a sample, sieving, heating to 800 ℃ at the speed of 7 ℃/min, and preserving heat at 800 ℃ for 2 hours to obtain the frit A.
Mixing the raw material BaCO3And SiO2According to the chemical formula BaSiO3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C for 4 hr in a 3.3kw ordinary oven, and passing through 250 holes/cm2Separating the sample, sieving, heating to 1400 deg.C, holding for 2 hr, continuing heating to 1600 deg.C, holding for 0.5 hr, cooling to 800 deg.C, holding for 2 hr, and cooling to room temperature to obtain BaSiO3Microcrystalline glass.
The mixture is prepared according to 85 percent of frit A and 15 percent of BaSiO3Uniformly mixing the microcrystalline glass according to the mass relation, adding 70ml of deionized water, ball-milling for 8 hours on a ball mill with the rotating speed of 400r/min, drying for 4 hours at 120 ℃, and passing through 200 holes/cm2And (3) separating a sample, sieving, adding 7wt% of paraffin wax for granulation, pressing into a green blank with the pressure of 8MPa, heating to 500 ℃ at the heating rate of 2 ℃/min, heating to 1110 ℃ at the heating rate of 10 ℃/min for sintering, keeping the temperature for 1 hour, and cooling to obtain the ceramic medium. The dielectric property test results (test frequency is 1 KHz) of the prepared high dielectric constant ceramic dielectric material are shown in Table 1 and figure 1. For example 2, it can be seen from the figure that in the temperature range of-55 ℃ to 150 ℃, the dielectric constant is increased and then decreased with the increase of the temperature, and the change range is not large. As can be seen from the table, the dielectric constant of the sample was high and the loss was low at room temperature.
Example 3
A high-dielectric-constant ceramic dielectric material is prepared from 20% BaSiO3Microcrystalline glass and 80% BaO-5.75Fe2O3-0.5NiO composition.
The preparation method of the high dielectric constant ceramic dielectric material comprises the following steps: raw material Ba (NO)3)2、Fe(NO3)3And Ni (NO)3)2According to the chemical formula BaO-5.75Fe2O30.5NiO, ball milling for 4 hours in a ball mill with the rotating speed of 400r/min, drying for 5 hours in a common oven with the temperature of 100 ℃ of 3.3kw, and passing through 120 holes/cm2And (4) screening, heating to 800 ℃ at the speed of 10 ℃/min, and preserving heat for 4 hours at the temperature of 800 ℃ to obtain the frit A.
Mixing the raw material BaCO3And SiO2According to the chemical formula BaSiO3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C for 4 hr in a 3.3kw ordinary oven, and passing through 200 holes/cm2Separating the sample, sieving, heating to 1400 deg.C, holding for 2 hr, continuing heating to 1600 deg.C, holding for 0.5 hr, cooling to 800 deg.C, holding for 2 hr, and cooling to room temperature to obtain BaSiO3Microcrystalline glass.
The mixture is prepared according to 80 percent of frit A and 20 percent of BaSiO3Uniformly mixing the microcrystalline glass according to the mass relation, adding 70ml of deionized water, ball-milling for 8 hours on a ball mill with the rotating speed of 400r/min, drying for 5 hours at 120 ℃, and passing through 120 holes/cm2And (3) separating a sample, sieving, adding 5wt% of paraffin wax for granulation, pressing into a green body with the pressure of 8MPa, heating to 400 ℃ at the heating rate of 2 ℃/min, heating to 1120 ℃ at the heating rate of 10 ℃/min for sintering, keeping the temperature for 1 hour, and cooling to obtain the ceramic medium. The dielectric property test results (test frequency is 1 KHz) of the prepared high dielectric constant ceramic dielectric material are shown in Table 1 and figure 1. For example 3, it can be seen from the figure that in the temperature range of-55 ℃ to 150 ℃, the dielectric constant is increased and then decreased with the increase of the temperature, and the change amplitude is not large. As can be seen from the table, the dielectric constant of the sample was high and the dielectric loss was low at room temperature.
Example 4
A high-dielectric-constant ceramic dielectric material is prepared from 11% of BaSiO3Microcrystalline glass and 89% BaO-5.75Fe2O3-0.5NiO composition.
The preparation method of the high dielectric constant ceramic dielectric material comprises the following steps: raw material Ba (NO)3)2、Fe(NO3)3And Ni (NO)3)2According to the chemical formula BaO-5.75Fe2O30.5NiO, ball milling for 6 hours in a ball mill with the rotating speed of 400r/min, drying for 5 hours in a common oven with the temperature of 100 ℃ of 3.3kw, and passing through 120 holes/cm2And (4) separating a sample, sieving, heating to 800 ℃ at the speed of 5 ℃/min, and preserving heat at 800 ℃ for 3 hours to obtain the frit A.
Mixing the raw material BaCO3And SiO2According to the chemical formula BaSiO3Mixing, ball milling for 6 hr in a ball mill at 400r/min, drying at 100 deg.C for 4 hr in a 3.3kw ordinary oven, and passing through 120 holes/cm2Separating the sample, sieving, heating to 1400 deg.C, holding for 2 hr, continuing heating to 1600 deg.C, holding for 0.5 hr, cooling to 800 deg.C, holding for 2 hr, and cooling to room temperature to obtain BaSiO3Microcrystalline glass.
The mixture was prepared according to 89% frit A and 11% BaSiO3Uniformly mixing the microcrystalline glass according to the mass relation, adding 70ml of deionized water, ball-milling for 8 hours on a ball mill with the rotating speed of 400r/min, drying for 5 hours at the temperature of 120 ℃, and passing through 250 holes/cm2And (3) separating a sample, sieving, adding 8wt% of paraffin wax for granulation, pressing into a green body with the pressure of 8MPa, heating to 450 ℃ at the heating rate of 2 ℃/min, heating to 1150 ℃ at the heating rate of 10 ℃/min for sintering, keeping the temperature for 1 hour, and cooling to obtain the ceramic medium. The dielectric property test results (test frequency is 1 KHz) of the prepared high dielectric constant ceramic dielectric material are shown in Table 1 and figure 1. For example 4, it can be seen from the graph that in the temperature range of-55 ℃ to 150 ℃, the dielectric constant is increased and then decreased with the increase of the temperature, and the change range is not large. As can be seen from the table, the dielectric constant of the sample was high and the dielectric loss was low at room temperature.
In combination with the four examples, it can be seen from Table 1 and FIG. 1 that the dielectric constant of the sample increases and decreases with increasing temperature in the temperature range of-55 ℃ to 150 ℃ without much change.
The test method and test equipment used in the present invention are as follows:
1. dielectric constantTesting of ε and loss tan δ: the capacitance C and the dielectric loss tan delta (test frequency 1 KHz) of the capacitor were measured using a HEWLETT PACKARD 4278A capacitance tester, and the dielectric constant ε was calculated by the following equation:
wherein: c is the capacitance of the sample, in pF; d is the thickness of the sample piece in cm; d is the diameter of the sintered sample piece in cm.
2. Temperature coefficient of capacitance
The formula for calculation (-55 ℃ to 150 ℃):
wherein: reference temperature t0The temperature is selected to be 25 ℃,
has a unit of 10-6/℃。
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A ceramic dielectric material with high dielectric constant is characterized by comprising 80-90% of BaO-5.75Fe by mass2O30.5NiO and 10-20% BaSiO3And (3) microcrystalline glass.
2. The method of claim 1, comprising the steps of:
a) will be provided withRaw material Ba (NO)3)2、Fe(NO3)3And Ni (NO)3)2According to the chemical formula BaO-5.75Fe2O3Carrying out material mixing and ball milling on-0.5 NiO, then heating to 750-;
b) mixing the raw material BaCO3And SiO2According to the chemical formula BaSiO3Ball milling the mixture, heating to 1300 ℃ to 1500 ℃, keeping the temperature for 1-3 hours, continuing heating to 1400 ℃ to 1700 ℃, keeping the temperature for 0.5-1 hour, and cooling to obtain BaSiO3Microcrystalline glass;
c) 10-20% of BaSiO by mass percent3Mixing the microcrystalline glass and 80-90% of the frit A to obtain a mixture B;
d) and granulating the ingredient B, pressing into a green body, heating to 400-500 ℃ at the heating rate of 2-4 ℃/min, heating to 1100-1150 ℃ at the heating rate of 8-12 ℃/min, preserving the heat for 0.5-2 hours, and cooling to obtain the ceramic dielectric material.
3. The method according to claim 2, wherein the temperature increase rate in step a is 5-10 ℃/min.
4. The method according to claim 3, wherein the temperature increase rate in step a is 7 ℃/min.
5. The method as claimed in claim 2, wherein the step a and the step b are performed by drying the ball-milled mixture and passing through 250 pores/cm of 120-2And sieving and then heating.
6. The method as claimed in claim 2, wherein the temperature reduction in step b is carried out at 800 ℃ and 700 ℃, and the temperature is maintained for 2-3 hours and then reduced to room temperature.
7. The method of claim 2, wherein the green compact is pressed at a pressure of 8-9 MPa in step d.
8. The method for preparing a ceramic dielectric material with a high dielectric constant according to claim 2 or 7, wherein the granulating of the ingredient B comprises adding water into the ingredient B, ball-milling, drying, sieving, and adding a binder in an amount of 5-8% by mass of the ingredient B for granulation.
9. The method according to claim 8, wherein the binder is polyvinyl alcohol or paraffin wax.
10. The method as claimed in claim 2, wherein in the step d, the temperature is raised to 450 ℃ at a rate of 2 ℃/min, and then heated to 1100 ℃ and 1150 ℃ at a rate of 10 ℃/min, and the temperature is maintained for 1 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110287412.8A CN113004030A (en) | 2021-03-17 | 2021-03-17 | High-dielectric-constant ceramic dielectric material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110287412.8A CN113004030A (en) | 2021-03-17 | 2021-03-17 | High-dielectric-constant ceramic dielectric material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113004030A true CN113004030A (en) | 2021-06-22 |
Family
ID=76409379
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110287412.8A Pending CN113004030A (en) | 2021-03-17 | 2021-03-17 | High-dielectric-constant ceramic dielectric material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113004030A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05217424A (en) * | 1991-09-25 | 1993-08-27 | Murata Mfg Co Ltd | Non-reducing dielectric ceramic composition |
| CN101492293A (en) * | 2009-03-09 | 2009-07-29 | 陕西科技大学 | Barium titanate based Y5P ceramic dielectric material and method of producing the same |
| CN106904956A (en) * | 2017-03-10 | 2017-06-30 | 浙江大学 | A kind of nickel doped barium ferrite ceramic material of the magnetic high that is situated between high and preparation method thereof |
| CN111943666A (en) * | 2020-06-23 | 2020-11-17 | 太原理工大学 | Temperature-stable ceramic dielectric material and preparation method thereof |
-
2021
- 2021-03-17 CN CN202110287412.8A patent/CN113004030A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05217424A (en) * | 1991-09-25 | 1993-08-27 | Murata Mfg Co Ltd | Non-reducing dielectric ceramic composition |
| CN101492293A (en) * | 2009-03-09 | 2009-07-29 | 陕西科技大学 | Barium titanate based Y5P ceramic dielectric material and method of producing the same |
| CN106904956A (en) * | 2017-03-10 | 2017-06-30 | 浙江大学 | A kind of nickel doped barium ferrite ceramic material of the magnetic high that is situated between high and preparation method thereof |
| CN111943666A (en) * | 2020-06-23 | 2020-11-17 | 太原理工大学 | Temperature-stable ceramic dielectric material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| MUHAMMAD ASIF RAFIQ ET AL.: "Effect of Ni2+ Substitution on the Structural, Magnetic, and Dielectric Properties of Barium Hexagonal Ferrites (BaFe12O19)", 《JOURNAL OF ELECTRONIC MATERIALS》 * |
| 文九巴等: "《材料科学与工程》", 31 August 2007 * |
| 黄新友等: "BaSiO3掺杂对BT基电容器陶瓷性能和结构的影响", 《2011中国功能材料科技与产业高层论坛论文集》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106927804B (en) | A kind of microwave-medium ceramics temperature frequency characteristic adjusting control agent and its LTCC material | |
| CN105777109B (en) | A kind of low sintering giant dielectric ceramic capacitor medium and preparation method thereof | |
| CN113004028B (en) | Silicon-based low-dielectric microwave dielectric ceramic and preparation method thereof | |
| CN105732020B (en) | A kind of preparation method of giant dielectric, low-loss titanium dioxide base composite ceramic | |
| CN106892659A (en) | A kind of anti-reduction huge dielectric constant medium material for multilayer ceramic capacitors | |
| CN107512906A (en) | A kind of anti-reduction X9R type ceramic capacitor dielectric materials and preparation method thereof | |
| CN106938928A (en) | A kind of anti-reduction huge dielectric constant low loss, high value ceramic capacitor dielectric material | |
| CN111943666A (en) | Temperature-stable ceramic dielectric material and preparation method thereof | |
| CN107640970B (en) | The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material and preparation method thereof | |
| CN108863348A (en) | A kind of dielectric ceramic material and preparation method thereof of ultra-wide temperature stability | |
| CN104446452B (en) | Lead-free medium-temperature stable dielectric electronic ceramic material and preparation method thereof | |
| CN106278261A (en) | A kind of low-temperature sintering low-loss high frequency medium ceramic material and preparation method thereof | |
| CN114773060A (en) | Mg-Ta-based dielectric ceramic for multilayer ceramic capacitor and low-temperature preparation method thereof | |
| CN109437896B (en) | Positive temperature coefficient X7R ceramic dielectric material and preparation method thereof | |
| CN112341192B (en) | High-energy-storage-density sodium bismuth titanate-based lead-free dielectric material and preparation method thereof | |
| CN109626999B (en) | Negative temperature coefficient ceramic dielectric material and preparation method thereof | |
| CN106915964B (en) | Lead-free high-energy-storage-density ceramic material and preparation method thereof | |
| CN101030478B (en) | High-dielectric metal-electric medium composite ceramic capacitance and its production | |
| CN107226696A (en) | X7R types BaTiO3Based capacitor ceramic material and preparation method thereof | |
| CN113004030A (en) | High-dielectric-constant ceramic dielectric material and preparation method thereof | |
| CN109081693B (en) | High-dielectric X8R ceramic dielectric material and preparation method thereof | |
| CN105272192B (en) | A kind of low-k AG characteristic multilayer ceramic capacitor porcelains and preparation method thereof | |
| CN107746271B (en) | AgTa co-doped titanium dioxide-based dielectric ceramic material with low frequency and low dielectric loss and preparation method thereof | |
| CN100434394C (en) | B-position precursor doped with modified Barium titanate metal composite ceramic and preparation method thereof | |
| CN102531576A (en) | Dielectric material for capacitor with positive temperature coefficient change and positive voltage property and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210622 |
|
| RJ01 | Rejection of invention patent application after publication |