CN110963796A - Giant dielectric constant low-loss X8R type ceramic capacitor material and preparation method thereof - Google Patents
Giant dielectric constant low-loss X8R type ceramic capacitor material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 31
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000015895 biscuits Nutrition 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000000137 annealing Methods 0.000 claims abstract description 5
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 239000003292 glue Substances 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000012300 argon atmosphere Substances 0.000 claims abstract 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims description 2
- 238000009475 tablet pressing Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 19
- 239000004408 titanium dioxide Substances 0.000 description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 238000002083 X-ray spectrum Methods 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
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- 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
- C04B35/46—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 titanium oxides or titanates
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
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Abstract
The invention relates to a giant dielectric constant low-loss X8R type ceramic capacitor material, the nominal chemical formula of which is 95 mol% TiO2‑5mol％Ga2O3. The preparation method comprises the following steps: according to TiO2:Ga2O3Mixing materials according to the molar ratio of 95:5, taking absolute ethyl alcohol as a ball milling medium, uniformly mixing by ball milling, and drying; then presintering at 1000-1100 ℃ for 2.5-3.5h to obtain presintered powder, crushing, ball-milling and uniformly mixing by taking absolute ethyl alcohol as a ball-milling medium, drying and grinding into powder; adding PVA binder, granulating, tabletting and discharging glue to obtain a ceramic biscuit body; sintering at 1330-1370 deg.c for 3-5 hr to obtain ceramic block material; annealing for 1.5-2.5h in an argon atmosphere at 900-1000 ℃ to obtain the product. The invention has simple preparation process, low cost and ring alignmentThe environment is harmless, and the obtained X8R ceramic material has high dielectric constant, low loss, good frequency and thermal stability and good industrialization prospect.
Description
Technical Field
The invention belongs to the technical field of electronic ceramic material application, and particularly relates to a giant dielectric constant low-loss X8R type ceramic capacitor material and a preparation method thereof.
Background
In the present society, with the rapid development of electronic and microelectronic technologies and the demand for miniaturization, integration and multi-functionalization of electronic products, materials with high dielectric constants have received unprecedented attention. Compared with other high-dielectric-constant materials, the giant dielectric ceramic material has the advantages of extremely high dielectric constant, good mechanical strength, corrosion resistance, temperature stability and the like, and is considered as a potential material which can be widely applied to integrated circuits and high-energy-storage-density capacitors.
In the past decade of research on giant dielectric ceramic materials, researchers have discovered a range of environmentally friendly giant dielectric ceramic materials, such as perovskite, perovskite-like perovskite, barium titanate, strontium titanate, nickel oxide, and the like. By utilizing (In, Nb) acceptor-donor double-doped rutile titanium dioxide ceramic, a university Liu Yun professor team In Australian national university In 2013 successfully prepares the giant dielectric ceramic material with the dielectric constant as high as 50000 or more, the loss lower than 0.05 and excellent temperature and frequency stability. Therefore, modification of rutile titanium dioxide ceramic by doping becomes a research hotspot in the direction of giant dielectric ceramics at present.
Disclosure of Invention
The purpose of the invention is: provides a giant dielectric constant low-loss X8R type ceramic capacitor material and a preparation method thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
a giant dielectric constant low loss X8R type ceramic capacitor material has a nominal chemical formula of (95-97) mol% TiO2-(3～5)mol％Ga2O3。
A preparation method of a giant dielectric constant low-loss X8R type ceramic capacitor material comprises the following specific steps:
(1) adding TiO into the mixture2、Ga2O3As starting material, according to TiO2:Ga2O3Mixing (95-97) and (3-5) in a molar ratio, and then taking absolute ethyl alcohol as a ball milling medium, uniformly mixing by ball milling, and drying;
(2) pre-burning the dried powder prepared in the step (1) at the temperature of 1000-1100 ℃ for 2.5-3.5h to prepare pre-burned powder;
(3) crushing the pre-sintered powder prepared in the step (2), then ball-milling and mixing uniformly by taking absolute ethyl alcohol as a ball-milling medium, drying and grinding into micron-sized powder;
(4) adding the PVA binder into the powder prepared in the step (3), and performing granulation, tabletting and glue discharge to obtain a ceramic biscuit body;
(5) sintering the ceramic biscuit body at 1330-1370 ℃ for 3-5h to obtain a corresponding ceramic block material;
(6) annealing the ceramic block material in an argon-hydrogen atmosphere at the temperature of 900-1000 ℃ for 1.5-2.5h to obtain the giant dielectric constant low-loss X8R type ceramic capacitor material.
Preferably, TiO in step (1)2In the rutile form, TiO2The purity of (2) was 99.99%.
Preferably, the ball milling time in the step (1) is 11-13h, the drying temperature is 95-105 ℃, and the drying time is 11-13 h.
Preferably, the ball milling time in the step (3) is 11-13h, the drying temperature is 95-105 ℃, and the drying time is 11-13 h.
Preferably, the diameter of the tabletting mould in step (4) is 11-13mm, the pressure is 75-85MPa, and the dwell time is 2-4 minutes.
Preferably, the gel discharging temperature in the step (4) is 580- > 620 ℃, and the gel discharging time is 1.8-2.2 h.
Preferably, the mass ratio of the powder prepared in step (3) to the PVA binder in step (4) is 2: 1.
Preferably, the concentration of hydrogen in the argon-hydrogen atmosphere in step (6) is 4 to 6%.
The invention has the beneficial effects that:
the preparation method has the advantages of simple preparation process, low cost and no harm to the environment, and the obtained X8R ceramic material has the advantages of high dielectric constant, low loss and good frequency and thermal stability. The rutile titanium dioxide-based giant dielectric low-loss X8R ceramic material provided by the invention has a good industrialization prospect.
Drawings
FIG. 1 shows 95 mol% TiO prepared in example 1 of the present invention2-5 mol％Ga2O3The X-ray spectrum of the titanium dioxide-based giant dielectric constant low-loss X8R ceramic material.
FIG. 2 shows 95 mol% TiO prepared in example 1 of the present invention2-5 mol％Ga2O3A micrograph of a titanium dioxide-based giant dielectric constant low loss X8R ceramic material.
FIG. 3 shows 95 mol% TiO prepared in example 1 of the present invention2-5 mol％Ga2O3The dielectric constant and loss of the titanium dioxide-based giant dielectric constant low-loss X8R ceramic material are regularly shown along with the change of frequency under the room temperature condition.
FIG. 4 shows 95 mol% TiO prepared in example 1 of the present invention2-5 mol％Ga2O3The dielectric constant and loss of the titanium dioxide-based giant dielectric constant low-loss X8R ceramic material are in a regular graph with the change of temperature under different frequency conditions.
FIG. 5 shows 95 mol% TiO prepared in example 1 of the present invention2-5 mol％Ga2O3The change rate of the dielectric constant of the titanium dioxide-based giant dielectric constant low-loss X8R ceramic material under different frequency conditions is a regular graph along with the change of temperature.
Detailed Description
The invention adopts the traditional solid phase method to prepare the titanium dioxide-based ceramic material, and obtains the rutile titanium dioxide-based giant dielectric constant low-loss X8R ceramic material with thermal stability by utilizing the annealing process in the reducing atmosphere.
The present invention will be specifically described below with reference to examples. The following examples are illustrative and not intended to be limiting, and are not intended to limit the scope of the invention.
Example 1
A preparation method of a giant dielectric constant low-loss X8R type ceramic capacitor material comprises the following specific steps:
(1) TiO with the purity of 99.99 percent2(rutile type), Ga2O3Raw materials are TiO with the stoichiometric ratio of 95mol percent2-5 mol％Ga2O3The ingredients are put into a ball milling tank, zirconia balls and a nylon tank are selected, the mixing and ball milling time is 12 hours, the rotating speed is 300 r/min, and the ball milling medium is absolute ethyl alcohol. Drying the product obtained after ball milling at 100 DEG CAnd drying in the oven for 12 h.
(2) And (2) raising the temperature of the dried powder prepared in the step (1) to 1050 ℃ at a heating rate of 3 ℃/min for pre-sintering for 3 h.
(3) Taking out the pre-sintered powder, grinding, ball milling for 12h by using absolute ethyl alcohol as a ball milling medium, uniformly mixing, drying at 100 ℃ for 12h, and grinding into powder.
(4) Adding 10g of the powder into 5mL of PVA solution (5 wt% of PVA) and fully grinding; 0.7g of fully ground powder is taken and placed in a die with the diameter of 12mm, the pressure is maintained for 3 minutes under 80MPa, and the pressed block is glued for 2 hours at 600 ℃.
(5) And sintering the ceramic biscuit body obtained after the rubber is removed at 1350 ℃ for 4h to obtain the corresponding ceramic block material.
(6) And (3) annealing the ceramic block material in an argon-hydrogen atmosphere at 950 ℃ for 2h to obtain the rutile type titanium dioxide-based ceramic material, wherein the concentration of hydrogen in the argon-hydrogen atmosphere is 5%.
The rutile type titanium dioxide based ceramic material prepared in the example 1 was tested for the change of dielectric constant and loss under different frequency and temperature conditions, as shown in fig. 3, 4 and 5, the dielectric constant of the rutile type titanium dioxide based ceramic material can be maintained at 10 under 100-1M Hz5Nearby and the loss is only 0.04 at a frequency of 1k Hz. In addition, the change rate of the dielectric constant under a plurality of frequencies is in the range of-12.98 to 14.64 within the temperature range of-55 ℃ to 150 ℃. Obviously, the giant dielectric ceramic material has high temperature stability, meets the industrial standard of an X8R ceramic capacitor (the electrostatic capacity change rate is more than or equal to 15 percent and less than or equal to 15 percent), has strong practicability, and is expected to be applied to the electronic ceramic market.
Claims (9)
1. A giant dielectric constant low-loss X8R type ceramic capacitor material is characterized in that: the nominal chemical formula of the material is (95-97) mol% TiO2-(3～5)mol％Ga2O3。
2. A method for preparing the giant dielectric constant low loss X8R type ceramic capacitor material of claim 1, wherein: the method comprises the following specific steps:
(1) adding TiO into the mixture2、Ga2O3As starting material, according to TiO2:Ga2O3Mixing (95-97) and (3-5) in a molar ratio, and then taking absolute ethyl alcohol as a ball milling medium, uniformly mixing by ball milling, and drying;
(2) pre-burning the dried powder prepared in the step (1) at the temperature of 1000-1100 ℃ for 2.5-3.5h to prepare pre-burned powder;
(3) crushing the pre-sintered powder prepared in the step (2), then ball-milling and mixing uniformly by taking absolute ethyl alcohol as a ball-milling medium, drying and grinding into micron-sized powder;
(4) adding the PVA binder into the powder prepared in the step (3), and performing granulation, tabletting and glue discharge to obtain a ceramic biscuit body;
(5) sintering the ceramic biscuit body at 1330-1370 ℃ for 3-5h to obtain a corresponding ceramic block material;
(6) annealing the ceramic block material in an argon-hydrogen atmosphere at the temperature of 900-1000 ℃ for 1.5-2.5h to obtain the giant dielectric constant low-loss X8R type ceramic capacitor material.
3. The method for preparing giant dielectric constant low loss X8R type ceramic capacitor material as claimed in claim 2, wherein: TiO in step (1)2In the rutile form, TiO2The purity of (2) was 99.99%.
4. The method for preparing giant dielectric constant low loss X8R type ceramic capacitor material as claimed in claim 2, wherein: in the step (1), the ball milling time is 11-13h, the drying temperature is 95-105 ℃, and the drying time is 11-13 h.
5. The method for preparing giant dielectric constant low loss X8R type ceramic capacitor material as claimed in claim 2, wherein: in the step (3), the ball milling time is 11-13h, the drying temperature is 95-105 ℃, and the drying time is 11-13 h.
6. The method for preparing giant dielectric constant low loss X8R type ceramic capacitor material as claimed in claim 2, wherein: in the step (4), the diameter of the tablet pressing die is 11-13mm, the pressure is 75-85MPa, and the pressure maintaining time is 2-4 minutes.
7. The method for preparing giant dielectric constant low loss X8R type ceramic capacitor material as claimed in claim 2, wherein: the glue discharging temperature in the step (4) is 580-.
8. The method for preparing giant dielectric constant low loss X8R type ceramic capacitor material as claimed in claim 2, wherein: the mass ratio of the powder prepared in the step (3) to the PVA binder in the step (4) is 2: 1.
9. The method for preparing giant dielectric constant low loss X8R type ceramic capacitor material as claimed in claim 2, wherein: the concentration of hydrogen in the argon atmosphere in the step (6) is 4-6%.
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| CN113061025A (en) * | 2021-05-21 | 2021-07-02 | 安徽大学 | Lead-free bismuth sodium titanate-based X9R type ceramic capacitor material and preparation method thereof |
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