CN108610040A - A method of reducing titanium barium stannate system dielectric loss under reducing atmosphere - Google Patents

A method of reducing titanium barium stannate system dielectric loss under reducing atmosphere Download PDF

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CN108610040A
CN108610040A CN201810393110.7A CN201810393110A CN108610040A CN 108610040 A CN108610040 A CN 108610040A CN 201810393110 A CN201810393110 A CN 201810393110A CN 108610040 A CN108610040 A CN 108610040A
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reducing atmosphere
under reducing
powder
dielectric loss
barium stannate
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李玲霞
王瑞杰
张宁
于仕辉
孙正
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Tianjin University
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Tianjin University
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    • 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
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention discloses a kind of methods of reduction titanium barium stannate dielectric loss under reducing atmosphere, first by raw material BaTiO3、SnO2、BaCO3By Ba (SnxTi1‑x)O3, wherein 0 chemical formulas of ＜ x≤0.3 weigh dispensing, calcined at 1050 DEG C after ball milling, drying, sieving, synthesize principal crystalline phase；Outer adding additives are granulated after secondary ball milling again；It will be granulated powder again and be pressed into green compact, after green compact dumping, under reducing atmosphere in 1350~1450 DEG C of sintering, low-loss titanium barium stannate dielectric material under reducing atmosphere is made.The present invention is by increasing secondary ball milling technique, and dielectric loss is down to 0.5%~4.0% by the 1.0%~5.0% of the prior art, to substantially increase the performance of multiple-layer sheet ceramic capacitor.

Description

A method of reducing titanium barium stannate system dielectric loss under reducing atmosphere
Technical field
The ceramic composition that the invention belongs to a kind of characterized by ingredient, more particularly to a kind of reduction titanium barium stannate dielectric damage The method of consumption.
Background technology
The manufacture craft of MLCC (multiple-layer sheet ceramic capacitor) requires interior electrode that must jointly be burnt with dielectric material Knot is to form monolithic structure, and common MLCC porcelains such as BaTiO3The sintering temperature of system porcelain is higher, for common sky For gas atmosphere sintering, only those fusing points are high, hardly possible aoxidizes, the metal with low-resistivity could be used as inner electrode, and one As select precious metals pt, Pd or Pd-Ag alloys as electrode in MLCC, in this way in the production cost of MLCC inner electrode at Originally larger proportion is accounted for, and the cost of MLCC was once being caused to remain high because of electrode material costliness, it is significantly limited and answers Use range.In addition, the big specific volumeization of MLCC requires the number of plies for reducing the thickness of dielectric layer and increasing ceramic dielectric, but with Jie The increase of the matter number of plies, inner electrode layer number also accordingly increase, and leading to MLCC, increased production cost.Therefore, MLCC's is cost effective Electrode base metal in an urgent demand.When selecting Ni electrodes as metal electrode, it is desirable to which dielectric material and electrode exist simultaneously Cofiring in reducing atmosphere, and then require the resistance to reduction of dielectric material.On the basis of realizing the anti-reduction of dielectric material, need The dielectric properties of dielectric material are optimized.Dielectric loss be refer to being converted electrical energy into unit time per unit volume The energy consumed for thermal energy.The energy expenditure of this part reduces the transformation efficiency of MLCC, therefore reduction dielectric loss has Beneficial to increasing the service efficiency of dielectric material.
Ba(SnxTi1-x)O3Dielectric material is a kind of critically important electron ceramic material.On the one hand, its application is very extensive, High dielectric container, dielectric amplifier, parametric device and switching circuit protector etc. can be used as.On the other hand, as Sn contains The increase of amount, Ba (SnxTi1-x)O3Ceramics can show the transition from typical ferroelectric to Relaxation Ferroelectrics, so, it is one Class is for the critically important material of the theoretical research of ferroelectric physics.
Invention content
The purpose of the present invention is to provide a kind of its Jie of raising under the process conditions being sintered under titanium barium stannate reducing atmosphere Electrical property, the method for reducing dielectric loss.
The present invention is achieved by following technical solution.
A method of titanium barium stannate dielectric loss under reducing atmosphere is reduced, there are following steps：
(1) by raw material BaTiO3、SnO2、BaCO3By Ba (SnxTi1-x)O3, wherein 0 chemical formulas of ＜ x≤0.3 weigh dispensing；
(2) powder that step (1) is prepared is put into ball grinder, zirconia ball and deionized water, ball milling 4 hours is added； The raw material after ball milling is placed in infrared drying oven again and is dried, 40 mesh sieve is crossed after drying, obtains evengranular powder；
(3) by step (2), treated that powder is calcined 3 hours at 1050 DEG C, synthesizes principal crystalline phase；
(4) by step (3) synthesize principal crystalline phase powder be put into ball grinder, secondary ball milling, be added zirconia ball and go from Sub- water, ball milling 4 hours；The raw material after ball milling is placed in infrared drying oven again and is dried, 40 mesh sieve is crossed after drying, it is equal to obtain particle Even powder；
(5) binder for being 7% in step (4) treated powder additional mass percent is crossed 80 mesh sub-sieves, is made Grain；
(6) the granulation powder of step (5) is pressed into green compact, after dumping, under reducing atmosphere, in 1350~1450 DEG C Sintering keeps the temperature 2~4 hours, and the dielectric material of low-loss titanium barium stannate under reducing atmosphere is made.
The step (2), (4) drying temperature be 100 DEG C.
The mass ratio of the step (2), the powder of (4) and zirconia ball, deionized water is 1: 1: 2.
The green body of the step (6) is the disk of Φ 10mm × 1mm.
The sintering temperature of the step (6) is 1400 DEG C.
The reducing atmosphere of the step (6) is H2:N2=1:20.
The present invention provides a kind of methods of reduction titanium barium stannate dielectric loss under reducing atmosphere, pass through and increase secondary ball Grinding process, Ba (Sn obtainedxTi1-x)O3The dielectric loss of dielectric material is down to 0.5% by the 1.0%~5.0% of the prior art ~4.0%.Due to the reduction of dielectric loss, the performance of multiple-layer sheet ceramic capacitor is substantially increased.
Specific implementation mode
Below by specific embodiment, the invention will be further described, and raw materials used in example is the commercially available pure examination of analysis Agent, specific embodiment are as follows.
Embodiment 1
(1) by raw material BaTiO3、SnO2、BaCO3By Ba (Sn0.05Ti0.95)O3Chemical formula weighs dispensing；
(2) powder by above-mentioned preparation is put into ball grinder, and zirconia ball and deionized water, ball milling 4 hours, powder is added Mass ratio with zirconia ball, deionized water is 1: 1: 2；The raw material after ball milling is placed in infrared drying oven at 100 DEG C again Drying crosses 40 mesh sieve, obtains evengranular powder after drying；
(3) by step (2), treated that powder is calcined 3 hours at 1050 DEG C, synthesizes principal crystalline phase；
(4) by step (3) synthesize principal crystalline phase powder be put into ball grinder, secondary ball milling, be added zirconia ball and go from The mass ratio of sub- water, ball milling 4 hours, powder and zirconia ball, deionized water is 1: 1: 2；The raw material after ball milling is placed in again red It is dried in outer drying box, 40 mesh sieve is crossed after drying, obtains evengranular powder；
(5) binder for being 7% in step (4) the powder additional mass percent that treated is crossed 80 mesh sub-sieves, is made Grain；
(6) the granulation powder of step (5) is pressed into powder compressing machine with the pressure of 6MPa to the green body of Φ 10mm × 1mm, After dumping, in H2:N2=1:Under 20 reducing atmosphere ratio, in 1350 DEG C of sintering, 3 hours are kept the temperature, is made under reducing atmosphere High-k low-loss low frequency titanium barium stannate dielectric material；
(7) TH2828S is used to test the dielectric loss of its sample, under 1KHz, tan δ=3.7%.
Embodiment 2~8
The main technologic parameters and its dielectric loss of embodiment 2~8 refer to table 1, remaining preparation process is complete with embodiment 1 It is identical.
Table 1
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 (6)

1. a kind of method reducing titanium barium stannate dielectric loss under reducing atmosphere, has following steps：
(1) by raw material BaTiO3、SnO2、BaCO3By Ba (SnxTi1-x)O3, wherein 0 chemical formulas of ＜ x≤0.3 weigh dispensing；
(2) powder that step (1) is prepared is put into ball grinder, zirconia ball and deionized water, ball milling 4 hours is added；Again will Raw material after ball milling, which is placed in infrared drying oven, dries, and 40 mesh sieve is crossed after drying, obtains evengranular powder；
(3) by step (2), treated that powder is calcined 3 hours at 1050 DEG C, synthesizes principal crystalline phase；
(4) powder that step (3) is synthesized to principal crystalline phase is put into ball grinder, and zirconia ball and deionized water is added in secondary ball milling, Ball milling 4 hours；The raw material after ball milling is placed in infrared drying oven again and is dried, 40 mesh sieve is crossed after drying, is obtained evengranular Powder；
(5) binder for being 7% in step (4) treated powder additional mass percent crosses 80 mesh sub-sieves, is granulated；
(6) the granulation powder of step (5) is pressed into green compact, after dumping, under reducing atmosphere, in 1350~1450 DEG C of burnings Knot keeps the temperature 2~4 hours, and low-loss titanium barium stannate dielectric material under reducing atmosphere is made.
2. a kind of method reducing titanium barium stannate system dielectric loss under reducing atmosphere according to claim 1, special Sign is, the step (2), (4) drying temperature be 100 DEG C.
3. a kind of method reducing titanium barium stannate system dielectric loss under reducing atmosphere according to claim 1, special Sign is that the mass ratio of the step (2), the powder of (4) and zirconia ball, deionized water is 1: 1: 2.
4. a kind of method reducing titanium barium stannate system dielectric loss under reducing atmosphere according to claim 1, special Sign is that the green body of the step (6) is the disk of Φ 10mm × 1mm.
5. a kind of method reducing titanium barium stannate system dielectric loss under reducing atmosphere according to claim 1, special Sign is that the sintering temperature of the step (6) is 1400 DEG C.
6. a kind of method reducing titanium barium stannate system dielectric loss under reducing atmosphere according to claim 1, special Sign is that the reducing atmosphere of the step (6) is H2:N2=1:20.
CN201810393110.7A 2018-04-27 2018-04-27 A method of reducing titanium barium stannate system dielectric loss under reducing atmosphere Pending CN108610040A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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CN106495687A (en) * 2016-10-27 2017-03-15 西安交通大学 A kind of existing fringing field, dielectric ceramic of high-energy-density and preparation method thereof
CN107382308A (en) * 2017-07-17 2017-11-24 天津大学 A kind of anti-reduced form dielectric material of high-k

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CN103073281A (en) * 2013-01-31 2013-05-01 天津大学 Lithium-zinc-titanium-tin series microwave dielectric ceramics material and preparation method thereof
CN106495687A (en) * 2016-10-27 2017-03-15 西安交通大学 A kind of existing fringing field, dielectric ceramic of high-energy-density and preparation method thereof
CN107382308A (en) * 2017-07-17 2017-11-24 天津大学 A kind of anti-reduced form dielectric material of high-k

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