CN102963928A - Barium zirconate titanate based Y5V powder material and preparation method thereof - Google Patents

Barium zirconate titanate based Y5V powder material and preparation method thereof Download PDF

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CN102963928A
CN102963928A CN2012104469014A CN201210446901A CN102963928A CN 102963928 A CN102963928 A CN 102963928A CN 2012104469014 A CN2012104469014 A CN 2012104469014A CN 201210446901 A CN201210446901 A CN 201210446901A CN 102963928 A CN102963928 A CN 102963928A
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powder
zirconate titanate
barium zirconate
niobium
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崔斌
张璐琭
马蓉
王艳
湛新星
畅柱国
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Northwest University
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Abstract

The invention discloses a barium zirconate titanate based Y5V powder material Ba (Ti[1-x]Zrx) O3+A which is sintered at the temperature of 1200-1320 DEG C to form a Y5V type ceramic material with ultrahigh dielectric constant and low dielectric loss. The ceramic material disclosed by the invention has the characteristics that the dielectric constant is maximally up to more than 22000; the temperature change rate of capacitance is between -82% and 22%; the room temperature dielectric loss is less than 0.8%; the powder particle size is between 20nm and 60 nm; and the ceramic grain size is less than 5 micrometers. The powder material disclosed by the invention is suitable for manufacturing multilayer ceramic capacitors or energy storage batteries with high capacity, small volume, high pressure resistance and high performance and has broad industrial application prospect.

Description

Barium zirconate titanate-based Y5V powder body material and preparation method thereof
Technical field
The present invention relates to a kind of barium zirconate titanate-based Y5V powder body material and preparation method thereof.
Background technology
BaTiO 3Series ceramic material is as a kind of important electron ceramic material, has high-k, ferroelectric, piezoelectricity, the good electric property such as withstand voltage, applies to widely the large miniature capacitor of volume low capacity.Y5V type ceramic condenser is widely used in electronic circuit as the representative of a class ceramic condenser of high dielectric property, particularly the mobile phone in high-grade electronic machine such as mobile computing, the mobile communication, automobile telephone etc.Velocity of variation when Y5V refers to that electrical capacity in-30-85 ℃ scope is with respect to 25 ℃ of room temperatures satisfies-82%≤(C-C 25)/C 25≤ 22%; C is-electrical capacity of certain temperature spot in the 30-85 ℃ scope.
At present, prepare barium zirconate titanate-based Y5V type ceramic condenser and mostly use solid phase method with dielectric material.The major advantage of solid phase method is that its preparation technology is simple ripe, raw material is cheap etc.But because its preparation technology is longer, thermal treatment temp is high, and mixture homogeneity is poor, causes easily powder granule larger, and component easily departs from, and needs the shortcomings such as the consumption of sintering agent is more, thus so that the mis-behave of pottery.Such as complicated process of preparation as described in the US Patent No. 005361187, the particle size of powder is more than 1 μ m, and the ceramic crystalline grain size has limited the reduction of ceramic layer thickness among the MLCC greater than 10 μ m, and the ceramic particle that medium layer comprises very little, can cause the reliability variation of electrical condenser.
The thin brilliant barium zirconate titanate-based Y5V type pottery of Liquid preparation methods mainly contains the precipitator method and hydrothermal method with medium powder.At present, the people such as Wang Sheng (Journal of Inorganic Materials, 2005,20:119-126) go out the powder median size less than 0.3 μ m with the hydro-thermal legal system is standby, ceramic granularity is 4 μ m, and room temperature dielectric constant is greater than 18000, dielectric loss is less than 0.7 %, and meets (the Ba of Y5V standard 0.97Ca 0.03) 1.001(Ti 0.80Zr 0.20) O 3Pottery.But hydrothermal method is usually for the having relatively high expectations of equipment, and temperature, pressure must strict control, and cost is high, and yields poorly.Although and the precipitator method have been simplified the preparation process of Y5V powder, the shortcoming that it still exists complex process, the easy segregation of component etc. to overcome, and specific inductivity only is 14000.
Compare with above two kinds of wet chemistry methods, the material of sol-gel method single stage method preparation can be calcined synthetic at a lower temperature, thereby has avoided material contaminated, finally obtains material high-purity, homogeneous; It has realized the even mixing of element at atomic level, and the concentration of controlled doping element more accurately, thereby obtains the powder of strict stoichiometric ratio; It can reach the effective control to powder granularity and pattern, obtains thin brilliant nano-powder.Chinese patent 200910254653.1 uses once through method in Sol Gel process to make diameter of particle less than the powder of 100 nm, but its gained ceramic dielectric constant lower (16000), the complicated [(Ba of phosphor composing 0.87Sr 0.04Ca 0.09) (Ti 0.86Zr 0.08Sn 0.06) O 3].
Summary of the invention
The purpose of this invention is to provide a kind of ultra-high dielectric coefficient low-dielectric loss ceramic condenser with barium zirconate titanate-based Y5V powder, its specific inductivity maximum can reach 24000, dielectric loss (25 ℃)≤0.8%.
Another object of the present invention provides an one step preparation method of above-mentioned barium zirconate titanate-based Y5V powder.
For achieving the above object, implementation procedure of the present invention is as follows:
Formula B a (Ti 1-xZr x) O 3The barium zirconate titanate-based Y5V powder that+A represents, 0.05＜x＜0.20 wherein, A is MnO 2, CuO, Nb 2O 5And rare earth oxide, principal crystalline phase Ba (Ti 1-xZr x) O 3Weight percent be 98.5-99.7wt%, the weight percent of each component is among the A: MnO 2Be 0.01-0.05%, CuO is 0.09-0.4%, Nb 2O 5Be 0.1-0.5%, rare earth oxide is 0.1-0.6%, and described rare earth oxide is the oxide compound of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium.
The preparation method of above-mentioned barium zirconate titanate-based Y5V powder may further comprise the steps:
(1) titanic acid ester is dissolved in Glacial acetic acid and the alcoholic solvent;
(2) add barium, zirconium, manganese, copper, rare earth salt aqueous solution according to stoichiometric ratio, the water-soluble complexes of niobium or pure niobium stir to get colloidal sol;
(3) colloidal sol further stirs and obtains gel, 30 ~ 90 ℃ of dry dry gel powders that get;
(4) dry gel powder got barium zirconate titanate-based Y5V powder in 0.5 ~ 8.0 hour in 750 ~ 1200 ℃ of lower calcinings.
Described titanic acid ester general formula is Ti (OR) 4, wherein R is butyl, sec.-propyl, octyl group or n-propyl.
Described alcoholic solvent is selected from ethanol, n-propyl alcohol, Virahol, n-butyl alcohol, 2-butanols.
Barium, manganese, copper, rare-earth salts add with the form of nitrate, nitrite or acetate, and zirconium adds with the form of zirconium nitrate or Zircosol ZN, and the water-soluble complexes of niobium or pure niobium are Nb 2O 5Superoxol, niobium hydroxide, ethanol niobium, n-propyl alcohol niobium, amylalcohol niobium.
Use powder that above-mentioned barium zirconate titanate-based Y5V powder preparation method obtains through granulation, compressing tablet, obtain the Y5V pottery at 1200-1320 ℃ of sintering 1 ~ 6 h.
The high dielectric constant and low dielectric loss ceramic condenser that the present invention prepares reaches following index with the dielectric material performance: the ceramic disks sintering temperature is between 1200-1320 ℃, grain-size is at 2-7 μ m, in-30 ℃ to+85 ℃ temperature range, temperature coefficient of capacitance (TCC) is in+22% ~-82% scope, the room temperature dielectric constant of material is at 15000-22000, room temperature dielectric loss＜0.8%.
The present invention adopts once through method in Sol Gel process, compositing formula by further optimization material and control preparation condition can obtain particle diameter little, be evenly distributed and barium zirconate titanate-based Y5V type pottery medium powder that purity is higher, thereby provide a new approach for the MLCC for preparing high-performance, thin layer, miniaturization; The additives such as zirconium barium titanate major ingredient, doping component and sintering agent all adopt the sol-gel method single stage method to add among the present invention, carry out causing when secondary mixes the composition mixing inhomogeneous to avoid major ingredient and additive etc., and the new problems such as impurity are advanced in blending; The median size of the powder of the present invention preparation is little, good dispersity, active high, purity is high; Raw material of the present invention is easy to get, and equipment is simple, and simple process, system component are controlled.
Description of drawings
Fig. 1 is the powder XRD spectra of embodiment 1 preparation;
Fig. 2 is the powder TEM photo of embodiment 1 preparation;
Fig. 3 is the SEM photo of the powder sintering pottery of embodiment 1 preparation;
Fig. 4 is the dielectric properties of the pottery of embodiment 1 preparation;
Fig. 5 is the SEM photo of the powder sintering pottery of embodiment 2 preparations;
Fig. 6 is the dielectric properties of the pottery of embodiment 2 preparations.
Embodiment
Embodiment 1
Press 1.00mol Ba (Ti 1-xZr x) O 3+ A, ZrO in the powder 2Content (x) be respectively 5.1 mol%, 5.4 mol%, 5.7 mol%, A is for forming fixing MnO 2, CuO, Nb 2O 5And rare earth oxide.Adopt the synthetic BaTiO of once through method in Sol Gel process 3Based Y 5 V nano-powder.Concrete steps are as follows:
A) take by weighing tetrabutyl titanate 50.00 g by stoichiometric ratio, stir Glacial acetic acid and the 29 ml dehydrated alcohols of lower 45 ml of adding, fully stir; Add barium acetate 43.70 g, holmium nitrate 0.4931 g, manganese acetate 0.0848 g, neutralized verdigris 0.2762 g, niobium oxides 0.1838g(Nb according to stoichiometric ratio 2O 5The adding form be Nb 2O 5Superoxol C Nb5+=0.01141 g/ml, 16.11ml), the quality of zirconium nitrate is 8.4427 g, constantly stirs, and temperature of reaction is room temperature, and the reaction times is 2 hours, obtains the blue-greenish colour vitreosol; Fully stir the barium phthalate base presoma that obtains homogeneous transparent, overnight leaving standstill, 80 ℃ of dry dry gel powders that get.
B) xerogel got nano-powder in 2 hours 900 ℃ of calcinings, and its XRD figure is composed as shown in Figure 1, and the TEM photo is seen Fig. 2.
C) powder adds water formation slurry, carries out ball milling take zirconia ball as mill is situated between, and Ball-milling Time is 6 ~ 48 h.The dried sample of ball milling through granulation, is pressed into the base substrate disk of diameter 8 mm and thickness 1.5 mm under 6 MPa pressure, carries out sintering and be incubated 2 h in 1300 ℃, make the disk stupalith, the SEM photo is seen Fig. 3.
The dielectric properties of ceramics sample are seen Fig. 4 and table 1, and as seen from Table 1, prepared material meets the requirement of EIA-Y5V standard.
Figure 356137DEST_PATH_IMAGE001
Embodiment 2
Press 1.00mol Ba (Ti 1-xZr x) O 3+ A, ZrO in the powder 2Content (x) be 5.4 mol%, A is for forming fixing MnO 2, CuO, Nb 2O 5And rare earth oxide.Adopt the synthetic barium zirconate titanate-based Y5V powder of once through method in Sol Gel process, the sintering temperature of pottery is respectively 1300 ℃, 1260 ℃ and 1240 ℃ (being designated as successively #2-1, #2-2 and #2-3), and concrete steps are as follows:
A) take by weighing tetrabutyl titanate 50.00 g by stoichiometric ratio, stir lower add an amount of Glacial acetic acid and dehydrated alcohol, fully stir; Add barium acetate 43.70 g, holmium nitrate 0.4931 g, zirconium nitrate 8.4427 g, manganese acetate 0.0848 g, neutralized verdigris 0.2762 g, Nb according to stoichiometric ratio 2O 50.1838g(Nb 2O 5The adding form be Nb 2O 5Superoxol C Nb5+=0.01141 g/ml, 16.11ml), and constantly stir, temperature of reaction is room temperature, and the reaction times is 2 hours, obtains the blue-greenish colour vitreosol; Fully stir the barium zirconate titanate-based presoma that obtains homogeneous transparent, overnight leaving standstill, 80 ℃ of dry dry gel powders that get.
B) xerogel got powder in 2 hours 900 ℃ of calcinings.
C) powder adds water formation slurry, carries out ball milling take zirconia ball as mill is situated between, and Ball-milling Time is 6 ~ 48 h.The dried sample of ball milling through granulation, is pressed into the base substrate disk of diameter 8 mm and thickness 1.5 mm under 6 MPa pressure, in 1300 ℃, carries out respectively sintering and be incubated 2 h under 1260 ℃ and 1240 ℃, make the disk stupalith, the SEM photo is seen Fig. 5.
Fig. 6 and table 2 are the dielectric properties of the ceramics sample of sintering under the differing temps.As seen from Table 2, prepared material meets the requirement of EIA-Y5V standard.
Figure 273277DEST_PATH_IMAGE002
Embodiment 3
Press 1.00mol Ba (Ti 1-xZr x) O 3+ A, ZrO in the powder 2Content (x) be 5.4 mol%, A is for forming fixing MnO 2, CuO, Nb 2O 5And rare earth oxide.Adopt the synthetic barium zirconate titanate-based Y5V powder of once through method in Sol Gel process, change MnO among the A 2, CuO, Nb 2O 5Or one or several quality of rare earth oxide, concrete steps are as follows:
A) take by weighing tetrabutyl titanate 50.00 g by stoichiometric ratio, stir lower add an amount of Glacial acetic acid and dehydrated alcohol, fully stir; Add barium acetate 43.70 g, zirconium nitrate 8.4427 g and the MnO that changes respectively different amounts according to stoichiometric ratio 2, CuO, Nb 2O 5Or one or several of rare earth oxide, parameter sees Table 3(and is followed successively by #3-1 in detail, #3-2 ..., #3-18), and constantly stirring, temperature of reaction is room temperature, the reaction times is 2 hours, obtains the blue-greenish colour vitreosol; Fully stir the barium zirconate titanate-based presoma that obtains homogeneous transparent, overnight leaving standstill, 80 ℃ of dry dry gel powders that get.
B) xerogel got nano-powder in 2 hours 900 ℃ of calcinings.
C) powder adds water formation slurry, carries out ball milling take zirconia ball as mill is situated between, and Ball-milling Time is 6 ~ 48 h.The dried sample of ball milling through granulation, is pressed into the base substrate disk of diameter 8 mm and thickness 1.5 mm under 6 MPa pressure, carries out sintering and be incubated 2 h in 1300 ℃, make the disk stupalith.
Table 3 is doping different mass A(MnO 2, CuO, Nb 2O 5And rare earth oxide) ceramic powder forms.Table 4 is the dielectric properties of the made pottery of corresponding different powders in the table 3.As seen from Table 4, prepared material meets the requirement of EIA-Y5V standard.
Figure 383046DEST_PATH_IMAGE003

Claims (8)

1. Formula B a (Ti 1-xZr x) O 3The barium zirconate titanate-based Y5V powder that+A represents, 0.05＜x＜0.20 wherein, A is MnO 2, CuO, Nb 2O 5And rare earth oxide, principal crystalline phase Ba (Ti 1-xZr x) O 3Weight percent be 98.5-99.7wt%,
The weight percent of each component is among the A: MnO 2Be 0.01-0.05%, CuO is 0.09-0.4%, Nb 2O 5Be 0.1-0.5%, rare earth oxide is 0.1-0.6%.
2. barium zirconate titanate-based Y5V powder according to claim 1, it is characterized in that: described rare earth oxide is the oxide compound of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, yttrium.
3. the preparation method of the described barium zirconate titanate-based Y5V powder of claim 1 may further comprise the steps:
(1) titanic acid ester is dissolved in Glacial acetic acid and the alcoholic solvent;
(2) add barium, zirconium, manganese, copper, rare earth salt aqueous solution according to stoichiometric ratio, the water-soluble complexes of niobium or pure niobium stir to get colloidal sol;
(3) colloidal sol further stirs and obtains gel, 30 ~ 90 ℃ of dry dry gel powders that get of gel;
(4) dry gel powder got barium zirconate titanate-based Y5V powder in 0.5 ~ 8.0 hour in 750 ~ 1200 ℃ of lower calcinings.
4. the preparation method of described barium zirconate titanate-based Y5V powder according to claim 3, it is characterized in that: described titanic acid ester general formula is Ti (OR) 4, wherein R is butyl, sec.-propyl, octyl group or n-propyl.
5. the preparation method of described barium zirconate titanate-based Y5V powder according to claim 3, it is characterized in that: described alcoholic solvent is selected from ethanol, n-propyl alcohol, Virahol, n-butyl alcohol, 2-butanols.
6. the preparation method of described barium zirconate titanate-based Y5V powder according to claim 3, it is characterized in that: barium, manganese, copper, rare-earth salts add with the form of nitrate, nitrite or acetate, and zirconium adds with the form of zirconium nitrate or Zircosol ZN.
7. the preparation method of described barium zirconate titanate-based Y5V powder according to claim 3, it is characterized in that: the water-soluble complexes of described niobium or pure niobium are Nb 2O 5Superoxol, niobium hydroxide, ethanol niobium, n-propyl alcohol niobium, amylalcohol niobium.
8. Y5V pottery is characterized in that right to use requires powder that 3 to 7 one of any described barium zirconate titanate-based Y5V powder preparing methods obtain through granulation, compressing tablet, obtains at 1200-1320 ℃ of sintering 1 ~ 6 h.
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CN106587992A (en) * 2016-12-08 2017-04-26 苏州艾博迈尔新材料有限公司 High-performance piezoceramic material and preparation method thereof
CN108558399A (en) * 2018-06-01 2018-09-21 西北大学 A kind of low-temperature sintering high dielectric property Y5V type ceramic capacitor dielectric materials and preparation method thereof
CN110642620A (en) * 2019-10-15 2020-01-03 宝鸡文理学院 Low-sintering high-dielectric ceramic material and preparation method thereof
CN112225559A (en) * 2020-09-25 2021-01-15 陕西科技大学 Zr-doped high-entropy perovskite oxide ceramic material with high energy storage and high efficiency, and preparation method and application thereof
CN114409402A (en) * 2022-02-24 2022-04-29 江苏科技大学 Capacitor dielectric porcelain and preparation method thereof

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CN106587992A (en) * 2016-12-08 2017-04-26 苏州艾博迈尔新材料有限公司 High-performance piezoceramic material and preparation method thereof
CN108558399A (en) * 2018-06-01 2018-09-21 西北大学 A kind of low-temperature sintering high dielectric property Y5V type ceramic capacitor dielectric materials and preparation method thereof
CN110642620A (en) * 2019-10-15 2020-01-03 宝鸡文理学院 Low-sintering high-dielectric ceramic material and preparation method thereof
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