CN108975907A - The method for improving barium titanate dielectric material resistance to reduction is adulterated by transition-metal ions - Google Patents

The method for improving barium titanate dielectric material resistance to reduction is adulterated by transition-metal ions Download PDF

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CN108975907A
CN108975907A CN201811033254.8A CN201811033254A CN108975907A CN 108975907 A CN108975907 A CN 108975907A CN 201811033254 A CN201811033254 A CN 201811033254A CN 108975907 A CN108975907 A CN 108975907A
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transition
metal ions
dielectric material
batio
powder
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李玲霞
王瑞杰
毕越
于仕辉
王文波
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Tianjin University
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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
    • C04B35/462—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 based on titanates
    • C04B35/465—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 based on titanates based on alkaline earth metal titanates
    • C04B35/468—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 based on titanates based on alkaline earth metal titanates based on barium titanates
    • 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
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    • 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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
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    • 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
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • C04B2235/3267—MnO2
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    • 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
    • C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
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    • 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

Abstract

The method for improving barium titanate dielectric material resistance to reduction is adulterated by transition-metal ions the invention discloses a kind of, with BaTiO3Based on, the transition-metal ions compound X that additional mass percent content is 1~4% weighs ingredient, and the transition-metal ions compound X is SnO2、MnO2Or NH4VO3.It is calcined at 1000~1300 DEG C after ball milling, drying, sieving, synthesizes principal crystalline phase, then be granulated, be pressed into green compact, green compact are sintered in 1300~1450 DEG C, and BaTiO is made3Dielectric material.It is sintered close under dielectric constant of the present invention and air, dielectric loss is in 1.0%~4.0% range, insulation resistivity > 109, can be used for the preparation of multiple-layer sheet ceramic capacitor (MLCC).

Description

The method for improving barium titanate dielectric material resistance to reduction is adulterated by transition-metal ions
Technical field
The ceramic composition that the invention belongs to a kind of characterized by ingredient, in particular to it is a kind of to be mentioned by transition-metal ions doping High BaTiO3The method of dielectric material dielectric properties under reducing atmosphere.
Background technique
Traditional MLCC (multiple-layer sheet ceramic capacitor) generally selects precious metals pt, Pd or Pd-Ag alloy as MLCC Interior electrode, to meet the requirement of the high sintering temperature of dielectric material.But with being continuously increased for the MLCC number of plies, inner electrode Cost is gradually increased, and causes the high serious problem of MLCC cost.In order to realize the cost effective of manufacture craft, adopt Use the base metals such as Cu, Ni as electrode material.And this manufacture craft that will lead to MLCC needs to carry out under reducing atmosphere.Therefore Dielectric material is needed to meet and can meet MLCC performance after should being also sintered under reducing atmosphere under the matched requirement of interior electrode Requirement.Traditional BaTiO3Based dielectric material, under reducing atmosphere, since the generation of Lacking oxygen causes excessive freely electricity Son has the tendency that semiconducting, that is, loses the insulation performance of dielectric material.To inhibit BaTiO3Dielectric material semiconducting passes through this The consumption of free electron is realized in the transition-metal ions doping that patent illustrates, and then meets requirement of the base metal-MLCC to dielectric material.
Summary of the invention
The purpose of the present invention, be for realize MLCC manufacture craft it is cost effective, using base metal as electrode material, and To inhibit BaTiO3Dielectric material semiconducting under reducing atmosphere provides a kind of by doping transition-metal ions raising BaTiO3Medium The method of material resistance to reduction.
The present invention is achieved by following technical solution.
The method for improving barium titanate dielectric material resistance to reduction is adulterated by transition-metal ions, there are following steps:
(1) with BaTiO3Based on, the transition-metal ions compound X that additional mass percent content is 1~4%, weighing is matched Material；The transition-metal ions compound X is SnO2、MnO2Or NH4VO3；
(2) powder that step (1) is prepared is put into ball grinder, addition zirconia ball and deionized water, ball milling 4 hours； The raw material after ball milling is placed in infrared drying oven again and is dried, 40 meshes are crossed after drying, obtain evengranular powder；
(3) step (2) evengranular powder is calcined 3 hours at 1000~1300 DEG C, synthesizes principal crystalline phase；
(4) binder for being 7% in the powder additional mass percent of step (3) synthesis principal crystalline phase, crosses 80 mesh sub-sieves, It is granulated；
(5) the granulation powder of step (4) is pressed into green compact, after dumping, under reducing atmosphere, in 1300~1450 DEG C Sintering keeps the temperature 3 hours, and BaTiO is made3Dielectric material.
The drying temperature of the step (2) is 100 DEG C.
The powder and zirconia ball of the step (2), the mass ratio of deionized water are 1: 1: 2.
The green body of the step (5) is the disk of Φ 10mm × 1mm.
The sintering temperature of the step (5) is 1350 DEG C.
The present invention provides a kind of raising BaTiO3The method of dielectric material reproducibility, BaTiO obtained3Dielectric material is burnt Knot atmosphere is reducing atmosphere, and sintering temperature is 1300~1450 DEG C, is sintered under dielectric constant and air close, and dielectric loss exists In 1.0%~6.0% range, insulation resistivity > 109, can be used for the preparation of multiple-layer sheet ceramic capacitor (MLCC).
Specific embodiment
Below by specific embodiment, the invention will be further described, and raw materials used in embodiment is that commercially available analysis is pure Reagent, specific embodiment are as follows.
Embodiment 1
(1) by raw material BaTiO3、SnO2、BaCO3By Ba (Sn0.15Ti0.85)O3Chemical formula weighs ingredient；
(2) powder by above-mentioned preparation is put into ball grinder, addition zirconia ball and deionized water, and ball milling 4 hours, powder Mass ratio with zirconia ball, deionized water is 1: 1: 2；Raw material after ball milling is placed in infrared drying oven at 100 DEG C and is dried It is dry, 40 meshes are crossed after drying, obtain evengranular powder；
(3) step (2) evengranular powder is calcined 3 hours at 1050 DEG C, synthesizes principal crystalline phase；
(4) binder for being 7% in the powder additional mass percent of step (3) synthesis principal crystalline phase, crosses 80 mesh sub-sieves, It is granulated；
(5) the granulation powder of step (4) is pressed into powder compressing machine with the pressure of 6MPa to the green body of Φ 10mm × 1mm, It after dumping, is sintered in 1350 DEG C, keeps the temperature 3 hours, BaTiO is made3Resistance to reduction dielectric material.
(6) insulation resistance under the capacitance C and loss tan δ and 100V of its product is tested using TH2828S, and is counted The dielectric constant and insulation resistivity for calculating sample, under 1KHz, εr=8220, tan δ=1.908%, ρv=7.41 × 1010。
Embodiment 2
(1) BaTiO is weighed320g, by raw material MnO2Ingredient is weighed by with 1% doping ratio；
(2) powder by above-mentioned preparation is put into ball grinder, addition zirconia ball and deionized water, and ball milling 4 hours, powder Mass ratio with zirconia ball, deionized water is 1: 1: 2；Raw material after ball milling is placed in infrared drying oven at 100 DEG C and is dried It is dry, 40 meshes are crossed after drying, obtain evengranular powder；
(3) step (2) evengranular powder is calcined 3 hours at 1050 DEG C, synthesizes principal crystalline phase；
(4) binder for being 7% in the powder additional mass percent of step (3) synthesis principal crystalline phase, crosses 80 mesh sub-sieves, It is granulated；
(5) by the granulation powder of step (4) base for being pressed into Φ 10mm × 1mm with the pressure of 6MPa with powder compressing machine Body under reducing atmosphere ratio, is sintered in 1350 DEG C after dumping, keeps the temperature 3 hours, BaTiO is made3Resistance to reduction medium material Material.
(6) insulation resistance under the capacitance C and loss tan δ and 100V of its product is tested using TH2828S, and is counted The dielectric constant and insulation resistivity for calculating sample, under 1KHz, εr=2387, tan δ=1.0%, ρv=1.81 × 1012。
Embodiment 3
(1) BaTiO is weighed320g, by raw material NH4VO3Ingredient is weighed by with 1% doping ratio；
(2) powder by above-mentioned preparation is put into ball grinder, addition zirconia ball and deionized water, and ball milling 4 hours, powder Mass ratio with zirconia ball, deionized water is 1: 1: 2；Raw material after ball milling is placed in infrared drying oven at 100 DEG C and is dried It is dry, 40 meshes are crossed after drying, obtain evengranular powder；
(3) step (2) evengranular powder is calcined 3 hours at 1050 DEG C, synthesizes principal crystalline phase；
(4) binder for being 7% in the powder additional mass percent of step (3) synthesis principal crystalline phase, crosses 80 mesh sub-sieves, It is granulated；
(5) by the granulation powder of step (4) base for being pressed into Φ 10mm × 1mm with the pressure of 6MPa with powder compressing machine Body is sintered after dumping in 1350 DEG C, keeps the temperature 3 hours, and BaTiO is made3Resistance to reduction dielectric material.
(6) it using the insulation resistance under the capacitance C of TH2828S test article and loss tan δ and 100V, and calculates The dielectric constant and insulation resistivity of product out, under 1KHz, εr=2077, tan δ=5.181%, ρv=4.91 × 109。
The present invention is not limited to the above embodiment, and the variation of some details is possible, but therefore this does not violate this hair Bright scope and spirit.

Claims (5)

1. adulterating the method for improving barium titanate dielectric material resistance to reduction by transition-metal ions, there are following steps:
(1) with BaTiO3Based on, the transition-metal ions compound X that additional mass percent content is 1~4% weighs ingredient；Institute Stating transition-metal ions compound X is SnO2、MnO2Or NH4VO3；
(2) powder that step (1) is prepared is put into ball grinder, addition zirconia ball and deionized water, ball milling 4 hours；Again will Raw material after ball milling, which is placed in infrared drying oven, dries, and 40 meshes are crossed after drying, obtain evengranular powder；
(3) step (2) evengranular powder is calcined 3 hours at 1000~1300 DEG C, synthesizes principal crystalline phase；
(4) binder for being 7% in the powder additional mass percent of step (3) synthesis principal crystalline phase, crosses 80 mesh sub-sieves, makes Grain；
(5) the granulation powder of step (4) is pressed into green compact, after dumping, under reducing atmosphere, is burnt in 1300~1450 DEG C Knot keeps the temperature 3 hours, and BaTiO is made3Dielectric material.
2. according to claim 1 adulterated by transition-metal ions improves BaTiO3The method of dielectric material resistance to reduction, it is special Sign is that the drying temperature of the step (2) is 100 DEG C.
3. according to claim 1 adulterated by transition-metal ions improves BaTiO3The method of dielectric material resistance to reduction, it is special Sign is that the powder and zirconia ball of the step (2), the mass ratio of deionized water are 1: 1: 2.
4. according to claim 1 adulterated by transition-metal ions improves BaTiO3The method of dielectric material resistance to reduction, it is special Sign is that the green body of the step (5) is the disk of Φ 10mm × 1mm.
5. according to claim 1 adulterated by transition-metal ions improves BaTiO3The method of dielectric material resistance to reduction, it is special Sign is that the sintering temperature of the step (5) is 1350 DEG C.
CN201811033254.8A 2018-09-05 2018-09-05 The method for improving barium titanate dielectric material resistance to reduction is adulterated by transition-metal ions Pending CN108975907A (en)

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CN110183224A (en) * 2019-06-19 2019-08-30 天津大学 A kind of preparation method applied acceptor and be co-doped with high dielectric constant low consumption dielectric material
CN110256067A (en) * 2019-06-19 2019-09-20 天津大学 A kind of preparation method of the anti-reduced form dielectric substance of niobium additive Mn
CN112939597A (en) * 2021-04-06 2021-06-11 上海大学 PTCR thermal sensitive ceramic material and preparation method thereof
CN113860867A (en) * 2021-10-11 2021-12-31 天津大学 Barium titanate-based dielectric ceramic material with high tuning rate and preparation method thereof
CN114220659A (en) * 2021-11-26 2022-03-22 武汉理工大学 Oxide-reinforced inorganic dielectric amorphous composite film with high energy storage density and high breakdown strength and preparation method thereof
CN115819078A (en) * 2022-12-19 2023-03-21 江苏钧瓷科技有限公司 PTC thermistor ceramic material resisting reducing atmosphere and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110183224A (en) * 2019-06-19 2019-08-30 天津大学 A kind of preparation method applied acceptor and be co-doped with high dielectric constant low consumption dielectric material
CN110256067A (en) * 2019-06-19 2019-09-20 天津大学 A kind of preparation method of the anti-reduced form dielectric substance of niobium additive Mn
CN112939597A (en) * 2021-04-06 2021-06-11 上海大学 PTCR thermal sensitive ceramic material and preparation method thereof
CN113860867A (en) * 2021-10-11 2021-12-31 天津大学 Barium titanate-based dielectric ceramic material with high tuning rate and preparation method thereof
CN114220659A (en) * 2021-11-26 2022-03-22 武汉理工大学 Oxide-reinforced inorganic dielectric amorphous composite film with high energy storage density and high breakdown strength and preparation method thereof
CN115819078A (en) * 2022-12-19 2023-03-21 江苏钧瓷科技有限公司 PTC thermistor ceramic material resisting reducing atmosphere and preparation method thereof

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Application publication date: 20181211