CN104744032B - A kind of X8R type superfine ceramics capacitor dielectric material and preparation method thereof - Google Patents
A kind of X8R type superfine ceramics capacitor dielectric material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of X8R type Ba1‑xBixTiO3@(Nb2O5‑Co3O4) superfine ceramics capacitor dielectric material and preparation method thereof, its chemical composition formula meets：Ba1‑xBixTiO3+ n(aNb2O5+ bCo3O4), wherein, 0.002<X≤0.015, n=0.004 ~ 0.016, a=0.15～0.60 mol%, b=0.03～0.14 mol%.The present invention reaches following index using the powder body material that the sedimentation method and liquid phase coating method are obtained：Ba1‑xBixTiO3Powder dispersity is good, and the size controlling of granule is in 50 ~ 500 nm, and composite oxides coating thickness controls in 5 ~ 30 nm；Prepared ceramic medium material performance reaches following index：Ceramic disks sinter within the temperature range of 1100～1300 DEG C, and the crystal grain of pottery controls in 100 ~ 550 nm, room temperature dielectric constant<2600, room temperature dielectric is lost ＜ 2.5%, in 55 DEG C ~ 150 DEG C temperature ranges, C/C25℃＜ ± 15%.
Description
Technical field
The present invention relates to a kind of X8R type superfine ceramics capacitor dielectric material and preparation method thereof, belong to electronic ceramics electricity
Container material technical field.
Background technology
With multilayer ceramic capacitor（MLCC）Fast development, in order to meet its miniaturization, Large Copacity and in high temperature
In environment, application etc. requires, and ceramic medium material not only will possess high dielectric constant, and requires its temperature coefficient of capacitance relatively
The characteristic of smooth variation is assumed in wide temperature range.At present, X8R type ceramic dielectric material is because have within the scope of wider temperature
There is preferable temperature stability, be widely used in the fields such as oil exploration, car engine, shock resistance system.The EIA of X8R
(Electronic International Association) standard is as follows：8 and X represent respectively lower work temperature limit+
150 DEG C and -55 DEG C, the rate of temperature change that R represents electric capacity is less than ± 15 %, and room temperature dielectric is lost< 2.5%.
Electronic devices and components miniaturization, high performance development trend are that requirement MLCC sends out towards the direction of Large Copacity, superthin layer
Exhibition.At present, prepare BaTiO3The method of the dielectric material of base X8R type ceramic capacitor is mostly conventional solid-state method.But, due to
Solid-phase process preparation route is longer, and the powder granule prepared and ceramic crystalline grain larger, be unfavorable for the ultra-thin stratification of MLCC
Development.As United States Patent (USP)（US Patent No. 7727922）In, the basic composition of ceramic material is BaTiO3-ZrO2-
BaCO3-MnCO3-MoO3-MgO-Y2O3-SiO2, this composition meets X8R performance requirement, and room temperature dielectric constant is about 2000, but
Its composition is complicated, and the powder granule size prepared is more than 0.7 μm, and ceramic crystalline grain size is more than 2 μm；United States Patent (USP)（US
Patent No.5990029）, equally it is prepared for consisting of BaTiO using solid phase method3-Ta2O5-Nb2O5-ZnO-CaZrO3-MnO
X8R type ceramic material, room temperature dielectric constant is more than 2050, and the particle size of powder body is more than 0.8 μm, ceramic crystalline grain size
More than 5 μm；Chinese patent（Publication number 103011805A）, the basic composition of ceramic material is BaTiO3-K1/2Bi1/2TiO3-
BaNb2O6, meet X8R performance requirement, dielectric constant is about 1800.Therefore, how to optimize and simplify the composition of system, control pottery
The structure of ceramic dielectric material and obtain fine grain, epigranular and high performance X8R type BaTiO3Base MLCC material is to meet great Rong
Amount, ultra-thin stratification require to be problem to be solved by this invention.
Content of the invention
It is an object of the invention to provide a kind of form simple X8R type ceramic capacitor dielectric material and preparation method thereof.
Described X8R type superfine ceramics material has core shell structure, is expressed as Ba1-xBixTiO3@(Nb2O5-Co3O4), its change
Learning expression formula is：Ba1-xBixTiO3+ n(aNb2O5+ bCo3O4), wherein, 0.002<X≤0.015, n=0.004 ~ 0.016, a
Mol ratio with b is=10:1~1:1, preferably 3:1.
It is as follows that the present invention realizes process：
（1）At bath temperature is 30 ~ 50 DEG C, by a certain amount of TiCl4Solution is slowly dropped to 6 ~ 10 mol/L's
In NaOH solution, and it is sufficiently stirred for 0.5 ~ 1 h；
（2）It is respectively added slowly to the aqueous solution of configured good bismuth, barium ionss according to stoichiometric proportion, and constantly stir
Mix.Reaction temperature is 30 ~ 50 DEG C, and the response time is 0.5 ~ 1 h；
（3）Above-mentioned solution is continued stirring 2 ~ 6 h when bath temperature is 75 ~ 95 DEG C, washs, be dried, obtain Ba1- xBixTiO3Powder body；
（4）By step（3）Ba1-xBixTiO3Powder body ultrasonic disperse in deionized water, obtains the Ba of favorable dispersibility1- xBixTiO3Suspension；
（5）Niobium oxalate solution and cobalt nitrate solution are pressed the amount of material than mixing, obtains the inorganic mixed salt solution clarified；
（6）By step（5）Inorganic mixed salt solution be slowly dropped to Ba1-xBixTiO3In suspension, it is stirred vigorously, make
Its mix homogeneously；
（7）Add ammonia spirit, adjust pH in 9 ~ 11, by coprecipitation reaction so that Nb (OH)5、Co(OH)2And Co
(OH)3It is evenly coated at Ba1-xBixTiO3Particle surface；
（8）By gained suspension sucking filtration, drying, gained powder body is calcined 0.5 ~ 2 h in 600 ~ 850 DEG C, is obtained Ba1- xBixTiO3@(Nb2O5-Co3O4) ceramic capacitor dielectric powder body material；
（9）By step（8）The ceramic dielectric powder body obtaining, through pelletize, molding, burns in 1100～1300 DEG C of insulation 2～6 h
Knot makes ceramic medium material.
The present invention devises a kind of simple X8R type superfine ceramics capacitor dielectric material of composition.On the one hand, taken by bismuth
Part barium in generation " core " portion Barium metatitanate. obtains bismuth titanates barium it is therefore an objective to ceramic high temperature Curie temperature is shifted to high temperature direction,
And bismuth oxide fusing point itself is relatively low, sintering temperature can be reduced as sintering aid；On the other hand, will by chemical coprecipitation
Nb2O5And Co3O4It is uniformly wrapped on monodispersed Ba as " shell " composition1-xBixTiO3Micro-nano powder particle surface, prepared X8R
Type superfine ceramics material.This material can apply to make Large Copacity, superthin layer MLCC, therefore has wide answering in this field
Use prospect.
Beneficial effects of the present invention：
（1）It is 50 ~ 500 nm, the Ba of favorable dispersibility that the present invention has prepared granular size1-xBixTiO3Micro-nano rice flour
Body material, and there is the Ba of " core-shell " structure1-xBixTiO3@(Nb2O5-Co3O4) ceramic dielectric powder body material；
（2）It is obtained by the present invention and forms simple ceramic capacitor dielectric material, its upper limit has widened 150 using temperature
DEG C, room temperature dielectric constant can control between 2600 ~ 3000, and temperature coefficient of capacitance is little, and dielectric loss is little, and meeting X8R characteristic will
Ask；
（3）Ceramic crystalline grain size about 100 ~ 550 nm that the present invention obtains, epigranular, highly reliable, it is suitable for giving birth to
Produce Large Copacity, the MLCC of ultra-thin dielectric layer.
Brief description
Fig. 1 is the Ba of embodiment 1 preparation0.99Bi0.01TiO3The HR-SEM figure of powder body and its grain size distribution；
Fig. 2 is the TEM figure of embodiment 1-3 powder body different multiplying；
Fig. 3 is the HR-SEM figure of embodiment 1-3 ceramics sample and its grain size distribution of ceramic crystalline grain；
Fig. 4 is the performance diagram of the dielectric constant with temperature change of embodiment 1-1 to 1-4 ceramics sample；
The performance diagram that Fig. 5 varies with temperature for embodiment 1-1 to 1-4 ceramics sample temperature coefficient of capacitance.
Specific embodiment
The present invention will be further described by the following examples.
The present invention first passes through chemical precipitation method and prepares single dispersing Ba1-xBixTiO3Micro-nano powder, then passes through liquid phase bag
The method of covering prepares single dispersing Ba1-xBixTiO3@(Nb2O5-Co3O4) micro-nano powder, finally sinter and prepare X8R type superfine ceramics electricity
Vessel media material, this ceramic material crystal grain is by Ba1-xBixTiO3As " core " portion's material and Nb2O5-Co3O4Composite oxides bag
Coating forms as " shell " portion material.
Its preparation method comprises the following steps：
（1）At bath temperature is 30 ~ 50 DEG C, by a certain amount of TiCl4Solution is slowly dropped to 6 ~ 10 mol/L's
In NaOH solution, and it is sufficiently stirred for 0.5 ~ 1 h；
（2）The bismuth that is respectively added slowly to have prepared according to stoichiometric proportion, the aqueous solution of barium ionss, and constantly stir
Mix.Reaction temperature is 30 ~ 50 DEG C, and the response time is 0.5 ~ 1 h；
（3）Above-mentioned solution is continued stirring 2 ~ 6 h when bath temperature is 75 ~ 95 DEG C, washs, be dried, obtain Ba1- xBixTiO3Powder body；
（4）By step（3）Ba1-xBixTiO3Powder body ultrasonic disperse in deionized water, obtains the Ba of favorable dispersibility1- xBixTiO3Suspension；
（5）Niobium oxalate solution and cobalt nitrate solution are pressed the amount of material than mixing, obtains the inorganic mixed salt solution clarified；
（6）By step（5）Inorganic mixed salt solution be slowly dropped to Ba1-xBixTiO3In suspension, it is stirred vigorously, make
Its mix homogeneously；
（7）Add ammonia spirit, adjust pH in 9 ~ 11, by chemical coprecipitation, by Nb (OH)5、Co(OH)2And Co
(OH)3It is evenly coated at Ba1-xBixTiO3Particle surface；
（8）By gained suspension sucking filtration, drying, gained powder body is calcined 0.5 ~ 2 h in 600 ~ 850 DEG C, is obtained Ba1- xBixTiO3@(Nb2O5-Co3O4) ceramic capacitor dielectric powder body material；
（9）By step（8）The ceramic dielectric powder body obtaining, through pelletize, molding, burns in 1100～1300 DEG C of insulation 2～6 h
Knot makes ceramic medium material.
Embodiment 1
Preparation Ba1-xBixTiO3@(Nb2O5-Co3O4) powder body and its ceramic material, wherein, Ba1-xBixTiO3+ n
(aNb2O5+ bCo3O4) in x=0.010, a:b=3:1；N is respectively 0.004,0.008,0.012 and 0.016 (counter sample
Sequence number is designated as #1-1, #1-2, #1-3 and #1-4 successively).Liquid phase coating method of the present invention is adopted to prepare Ba0.99Bi0.01TiO3+ n
(3 mol% Nb2O5+ 1 mol% Co3O4) the comprising the following steps that of powder body and its ceramic medium material：
（1）Under the conditions of bath temperature is 30 DEG C, by the TiCl of 0.2014 g/mL of 50.00 mL4Solution is slowly added dropwise
To in the NaOH solution of 10.0 mol/L of 100.00 mL, and it is sufficiently stirred for 0.5 h, then according to stoichiometric proportion is delayed respectively
The slow aqueous solution adding bismuth, barium is in above-mentioned solution, and is stirred continuously 0.5 h, then by above-mentioned solution in bath temperature 90
Continue stirring 4 h in DEG C, finally scrubbed, it is dried, obtain monodispersity Ba0.99Bi0.01TiO3Powder body（Its FE-SEM figure is shown in figure
1）.
（2）The Ba that precise 1.0000 g is obtained0.99Bi0.01TiO3Powder body, by its ultrasonic disperse in deionized water,
Obtain Ba0.99Bi0.01TiO3Suspension；
（3）By a:b=3:1 measures the 5.94 × 10 of 20.00 mL respectively-3The niobium oxalate solution of mol/L and 20.0 mL's
2.97×10-3The cobalt nitrate solution mix homogeneously of mol/L, obtains the inorganic mixed salt solution clarified, then by above-mentioned inorganic salt
Mixed solution measures 5.78 mL, 11.55 mL, 17.32 mL and 23.10 mL respectively, parallel five groups, is slowly dropped to above-mentioned
Ba0.99Bi0.01TiO3In suspension.Through being stirred vigorously so as to mix homogeneously, it is subsequently adding ammonia spirit, adjust pH in ~ 9, lead to
Cross chemical coprecipitation, by Nb (OH)5、Co(OH)2、Co(OH)3It is evenly coated at Ba0.99Bi0.01TiO3Particle surface；
（4）By gained suspension sucking filtration, dry, gained powder body calcines 0.5 ~ 2 h in atmosphere in 600 ~ 850 DEG C, obtains
Ba0.99Bi0.01TiO3+ n(3 Nb2O5+1 Co3O4) ceramic dielectric powder body material；
（5）Ceramic dielectric powder body material, through pelletize, is pressed into diameter 8 mm and the base of thickness 1.5 mm under 6 MPa pressure
Body disk, makes disk ceramic medium material in 1180 DEG C of sintering.
The TEM figure of ceramic dielectric powder body 1-3 is shown in that Fig. 2, Fig. 3 give the FE-SEM figure of sample 1-3 ceramics sample, and Fig. 4 gives
Go out the characteristic curve of the dielectric constant with temperature change of ceramics sample 1-1 to 1-4, Fig. 5 gives ceramics sample 1-1 to 1-4
The performance diagram that varies with temperature of temperature coefficient of capacitance；Its dominant dielectric performance is shown in Table 1.
The performance parameter of table 1 ceramics sample #1-1 to #1-4
Embodiment 2
Liquid phase coating method technique using the present invention prepares Ba1-xBixTiO3@(Nb2O5-Co3O4) powder body and its ceramic material
Material, wherein, Ba1-xBixTiO3+ n(aNb2O5+ bCo3O4) in x=0.010 and n=0.012；a :B is respectively 6:Isosorbide-5-Nitrae .5:
1,3:1 and 1.5:1 (sequence number of counter sample is designated as #2-1, #2-2, #2-3 and #2-4 successively).Prepare
Ba0.99Bi0.01TiO3+ 0.012×(aNb2O5+ bCo3O4) the comprising the following steps that of powder body and its ceramic medium material：
（1）Under the conditions of bath temperature is 30 DEG C, by the TiCl of 0.2014 g/mL of 50.00 mL4Solution is slowly added dropwise
To in the NaOH solution of 10.0 mol/L of 100.00 mL, and it is sufficiently stirred for 0.5 h, then according to stoichiometric proportion is delayed respectively
The slow aqueous solution adding bismuth, barium is in above-mentioned solution, and is stirred continuously 0.5 h, then by above-mentioned solution in bath temperature 90
Continue stirring 4 h in DEG C, finally scrubbed, it is dried, obtain monodispersity Ba0.99Bi0.01TiO3Powder body；
（2）The Ba that precise 1.0000 g is obtained1-xBixTiO3Powder body, its ultrasonic disperse in deionized water obtains
Ba0.99Bi0.01TiO3Suspension；
（3）By a:B mol ratio is 6:Isosorbide-5-Nitrae .5:1,3:1 and 1.5:1 measure respectively 6.93 mL, 6.50mL, 5.78 mL and
The 5.94 × 10 of 4.33mL-3The niobium oxalate solution of mol/L and corresponding 3.47 mL, 3.25 mL, 2.89 mL and 2.17
The 2.97 × 10 of mL-3The cobalt nitrate solution of mol/L, mix homogeneously respectively；Then above-mentioned inorganic mixed salt solution is slowly added dropwise
To above-mentioned Ba0.99Bi0.01TiO3In suspension.Through being stirred vigorously so as to mix homogeneously, be subsequently adding ammonia spirit, adjust pH in
~ 9, by chemical coprecipitation, by Nb (OH)5、Co(OH)2、 Co(OH)3It is evenly coated at favorable dispersibility
Ba0.99Bi0.01TiO3Particle surface；
（4）By gained suspension sucking filtration, dry, gained powder body calcines 0.5 ~ 2 h in atmosphere in 600 ~ 850 DEG C, obtains
Ba0.99Bi0.01TiO3+ 0.012×(aNb2O5+ bCo3O4) ceramic dielectric powder body material；
（5）Ceramic dielectric powder body material, through pelletize, is pressed into diameter 8 mm and the base of thickness 1.5 mm under 6 MPa pressure
Body disk, makes disk ceramic medium material in 1180 DEG C of sintering.
The performance parameter of ceramics sample 2-1 to 2-5 is shown in Table 2.
The performance parameter of table 2 ceramics sample #2-1 to #2-4
Embodiment 3
Liquid phase coating method technique using the present invention prepares Ba1-xBixTiO3@(Nb2O5-Co3O4) powder body and its ceramic material
Material, wherein, Ba1-xBixTiO3+ n(aNb2O5+ bCo3O4) in n=0.012 and a:b=3:1；X is respectively 0.002,0.005 He
0.010（The sequence number of counter sample is designated as #3-1, #3-2 and #3-3 successively）.Synthesis Ba1-xBixTiO3+ 0.012×(3 Nb2O5
+1 Co3O4) the comprising the following steps that of powder body and its ceramic medium material：
（1）Under the conditions of bath temperature is 30 DEG C, by the TiCl of 0.2014 g/mL of 50.00 mL4Solution is slowly added dropwise
To in the NaOH solution of 10.0 mol/L of 100.0 0mL, and it is sufficiently stirred for 0.5 h, then according to x=0.002,0.005 He
0.010 measures the 1.06 × 10 of 1.89 mL, 4.72 mL and 9.43 mL respectively-3The bismuth nitrate solution of mol/L and corresponding to therewith
48.11 mL, 48.06 mL and 47.83 mL 2.07 × 10-2The barium acetate solution of mol/L, slow after mix homogeneously respectively
It is added drop-wise in above-mentioned solution, and be stirred continuously 0.5 h；Then above-mentioned solution is continued in 90 DEG C of bath temperature stirring 4
H, finally scrubbed, it is dried, obtain monodispersity Ba1-xBixTiO3Powder body；
（2）The Ba that precise 1.0000 g is obtained1-xBixTiO3Powder body, its ultrasonic disperse in deionized water obtains
Ba1-xBixTiO3Suspension；
（3）By a:b=3:1 measures the 5.94 × 10 of 5.78 mL-3The 2.97 of the niobium oxalate solution of mol/L and 2.89 mL ×
10-3The cobalt nitrate solution of mol/L, mix homogeneously；Then above-mentioned inorganic mixed salt solution is slowly dropped to above-mentioned Ba1- xBixTiO3In suspension.Through being stirred vigorously so as to mix homogeneously, it is subsequently adding ammonia spirit, adjust pH in ~ 9, by chemistry
Coprecipitation, by Nb (OH)5、Co(OH)2、Co(OH)3It is evenly coated at the Ba of favorable dispersibility1-xBixTiO3Particle surface；
（4）By gained suspension sucking filtration, dry, gained powder body calcines 0.5 ~ 2 h in atmosphere in 600 ~ 850 DEG C, obtains
Ba1-xBixTiO3+ 0.012×(3 Nb2O5+1Co3O4) ceramic dielectric powder body material；
（5）Ceramic dielectric powder body material, through pelletize, is pressed into diameter 8 mm and the base of thickness 1.5 mm under 6 MPa pressure
Body disk, makes disk ceramic medium material in 1180 DEG C of sintering.
The performance parameter of ceramics sample 3-1 to 3-3 is shown in Table 3.
The performance parameter of table 3 ceramics sample #3-1 to #3-3
Claims (9)
1. a kind of fine grain X8R type ceramic capacitor dielectric material it is characterised in that：" core " portion material of described dielectric ceramic material
For Ba1-xBixTiO3, " shell " portion material is Nb2O5-Co3O4, it is expressed as Ba1-xBixTiO3@(Nb2O5-Co3O4), its chemical composition
Expression formula is：Ba1-xBixTiO3+ n(aNb2O5+ bCo3O4), wherein, 0.002<X≤0.015, n=0.004 ~ 0.016, a with
The mol ratio of b is=10:1~1:1.
2. according to claim 1 X8R type ceramic capacitor dielectric material it is characterised in that：The mol ratio of a and b is=6:1~
3:1.
3. fine grain X8R type ceramic capacitor dielectric material described in claim 1 preparation method it is characterised in that：First pass through
Chemical precipitation method prepares single dispersing Ba1-xBixTiO3Micro-nano powder, then prepares single dispersing Ba by liquid phase coating method1- xBixTiO3@(Nb2O5-Co3O4) micro-nano powder, finally sinter and prepare X8R type superfine ceramics capacitor dielectric material.
4. the preparation method of fine grain X8R type ceramic capacitor dielectric material according to claim 3 is it is characterised in that include
Following steps：
（1）At 30～50 DEG C, by TiCl4Solution is added drop-wise in the NaOH solution of 6 ~ 10 mol/L, and is sufficiently stirred for；
（2）It is separately added into the aqueous solution of soluble bismuth and barium according to stoichiometric proportion；
（3）Above-mentioned solution is sufficiently stirred for, washs, being dried at 75 ~ 95 DEG C, obtains Ba1-xBixTiO3Powder body；
（4）By above-mentioned Ba1-xBixTiO3Powder body ultrasonic disperse in deionized water, obtains Ba1-xBixTiO3Suspension；
（5）Niobium oxalate solution and cobalt nitrate solution are stoichiometrically mixed to get inorganic mixed salt solution；
（6）By step（5）Inorganic mixed salt solution be added drop-wise to Ba1-xBixTiO3In suspension, stirring makes its mix homogeneously；
（7）Ammonia spirit is added to adjust pH to 9 ~ 11, by chemical coprecipitation, by Nb (OH)5、Co(OH)2、Co(OH)3Cladding
In Ba1-xBixTiO3Particle surface；
（8）Gained suspension is filtered, dries, gained powder body is calcined in atmosphere in 600 ~ 850 DEG C and obtained micro-nano Ba1- xBixTiO3@(Nb2O5-Co3O4) ceramic dielectric powder body；
（9）By step（8）Through pelletize, molding, sintering prepares ceramic capacitor dielectric material to the ceramic dielectric powder body obtaining.
5. according to claim 4 ceramic capacitor dielectric material preparation method it is characterised in that：Described Ba1-xBixTiO3
Powder body is single dispersing micro-nano powder, and diameter of particle is 50 ~ 500 nm.
6. according to claim 4 ceramic capacitor dielectric material preparation method it is characterised in that：Nb2O5And Co3O4Compound
Oxide is coated on Ba1-xBixTiO3Particle surface, coating thickness is 5 ~ 30 nm.
7. according to claim 4 ceramic capacitor dielectric material preparation method it is characterised in that：Step（8）In, described
Ba1-xBixTiO3@(Nb2O5-Co3O4) ceramic dielectric powder body particle size be 100 ~ 550 nm.
8. according to claim 4 ceramic capacitor dielectric material preparation method it is characterised in that：Step（9）In, pottery
Medium powder makes ceramic capacitor dielectric material in 1100～1300 DEG C of insulations 2～6 h sintering.
9. according to claim 8 ceramic capacitor dielectric material preparation method it is characterised in that：The pottery preparing
Capacitor dielectric material meets X8R standard.
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