CN104876565A - Lead-free high-dielectric-constant energy-storage dielectric ceramic material and preparation method thereof - Google Patents
Lead-free high-dielectric-constant energy-storage dielectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a lead-free high-dielectric-constant energy-storage dielectric ceramic material and a preparation method thereof. The chemical formula of the dielectric material is (1-x)BaTiO[3-x]CaSnO3, wherein x=0.11-0.15. The preparation method comprises the following steps: 1) proportioning raw materials BaCO3, CaCO3, SnO2 and TiO2 according to the chemical formula stoichiometric ratio; 2) uniformly mixing the raw materials by ball milling, drying, presintering in a muffle furnace, and naturally cooling in the furnace to obtain ceramic powder; 3) carrying out ball milling on the ceramic powder, granulating, screening, aging and carrying out single-surface extrusion forming to obtain a ceramic disk biscuit; and 4) carrying out high-temperature sintering on the ceramic disk biscuit. The method has the advantages of simple technique and low cost, and is lead-free and environment-friendly. The prepared energy-storage dielectric ceramic material has high relative dielectric constant (epsilon r is greater than 10000), and the energy storage density is 0.41-1.17 J/cm<3>.
Description
Technical field
The present invention relates to energy-storing dielectric ceramic technical field, be specifically related to a kind of unleaded high-k energy-storing dielectric ceramic material and preparation method thereof.
Background technology
Along with the development of modern science and technology, people have higher requirement to high voltage ceramic capacitor, not only to there is high compressive strength, also require that there is the features such as high relative dielectric constant, low-loss, high energy storage density, be beneficial to realize the miniaturization of electron device and integrated.
Although some plumbum-based material various aspects of performance for high voltage ceramic capacitor are superior, the toxicity of lead is comparatively large, can cause certain harm in production, use procedure to human body, environment, and simultaneously plumbous volatilization also can cause capacitor performance unstable.European Union and China have promulgated relevant law and regulations all, come into effect the unleaded control of electronic ceramics.Therefore, realize the greenization of capacitor ceramics, become the inexorable trend complying with social sustainable development.
BaTiO
3a kind of energy-accumulating medium material with high-k, the BaTiO prepared by liquid phase synthesizing method
3the height that specific inductivity is prepared compared with solid phase method, but under its room temperature, the specific inductivity of (25 DEG C) is still lower than 6000, and and technique is more complicated, poor repeatability.In addition, BaTiO
3the disruptive strength of pottery is 50 ~ 80kV/cm, and be at room temperature in ferroelectric phase, ferroelectric hysteresis loop is wider, and energy storage density is lower, thus limits its practical application.
Therefore, BaTiO be widened
3the use range of ceramic dielectic, needs to carry out doping vario-property, by BaTiO to it
3curie peak move near room temperature, to increase its specific inductivity; On the other hand, energy-accumulating medium material also needs compressive strength high as far as possible and low dielectric loss, to improve energy storage density.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, provides energy-storing dielectric ceramic material that a kind of specific inductivity is high, energy storage density is large and preparation method thereof.
For solving the problems of the technologies described above, technical scheme provided by the invention is:
There is provided a kind of unleaded high-k energy-storing dielectric ceramic material, its chemical formula is (1-x) BaTiO
3-xCaSnO
3, wherein x=0.11 ~ 0.15.
The present invention also provides the preparation method of above-mentioned unleaded high-k energy-storing dielectric ceramic material, and its step is as follows:
1) with BaCO
3, CaCO
3, SnO
2and TiO
2for raw material, according to chemical formula (1-x) BaTiO
3-xCaSnO
3middle metallic element stoichiometric ratio batching, wherein x=0.11 ~ 0.15;
2) by step 1) BaCO that takes
3, CaCO
3, SnO
2and TiO
2raw material ball milling mixes, and dries, is placed in retort furnace from room temperature, is warming up to 1000 ~ 1100 DEG C of pre-burning 2 ~ 3h, obtain ceramic powder with stove naturally cooling;
3) by step 2) gained ceramic powder ball milling post-drying, mix with binding agent and grind granulation, ageing 12h after sieving, one side extrusion forming obtains ceramic disks biscuit;
4) by step 3) gained ceramic disks biscuit in 600 ~ 650 DEG C of isothermal holding 2h, be then warming up to 1350 ~ 1400 DEG C sintering 2 ~ 3h, finally obtain unleaded high-k energy-storing dielectric ceramic material with stove naturally cooling.
By such scheme, step 2) and step 3) described ball milling is for adopting zirconia ball, take dehydrated alcohol as medium, the mixing and ball milling time is 12 ~ 26h.
By such scheme, step 2) described temperature rise rate is 2 ~ 4 DEG C/min.
By such scheme, step 3) described binding agent is polyvinyl alcohol water solution, concentration is 2.5wt%, and binding agent add-on is 1 ~ 3% of ceramic powder quality.
By such scheme, step 3) described extrusion forming pressure is 150 ~ 200MPa.
By such scheme, step 4) described temperature rise rate is 2 DEG C/min.
At (1-x) BaTiO
3-xCaSnO
3in the preparation of (x=0.11 ~ 0.15) energy-storing dielectric ceramic, our experimental result is: work as CaSnO
3solid solution doping lower than 11mol% or more than 15mol% time, media ceramic relative permittivity is at room temperature less than 10000, and works as CaSnO
3content lower than 11mol% time, the disruptive strength of media ceramic and energy storage density are compared to BaTiO
3not be improved significantly.When sintering temperature is lower than 1350 DEG C, media ceramic density can significantly decline, and material internal void content is larger; When sintering temperature is higher than 1450 DEG C, there is more liquid phase in material internal, causes the compressive strength of media ceramic and dielectric properties to worsen.
By the scope of control x, present invention obtains and there is high-k, low-dielectric loss and the energy-storing dielectric ceramic compared with high breakdown strength, relative to BaTiO
3pottery energy storage density is higher.
Beneficial effect of the present invention is: 1, preparation technology of the present invention is simple, reproducible, and not containing precious metal element in raw materials used, cost is lower, and not leaded, achieves porcelain greenization; 2, the present invention is by using Ca and Sn to BaTiO
3a position, B position simultaneously substitution, at room temperature (25 DEG C) significantly improve the specific inductivity (ε of material
r> 10000), resulting materials has relatively low dielectric loss (tan δ≤0.03) simultaneously, and disruptive strength is between 90 ~ 175kV/cm, and energy storage density improves (reaches 1.17J/cm
3), be conducive to the miniaturization realizing ceramic condenser.
Accompanying drawing explanation
The XRD figure of the energy-storing dielectric ceramic material of Fig. 1 prepared by comparative example 1 and embodiment 1 ~ 5 is composed;
The SEM figure of the energy-storing dielectric ceramic material of Fig. 2 prepared by comparative example 1;
The SEM figure of the energy-storing dielectric ceramic material of Fig. 3 prepared by embodiment 1;
The SEM figure of the energy-storing dielectric ceramic material of Fig. 4 prepared by embodiment 2;
The SEM figure of the energy-storing dielectric ceramic material of Fig. 5 prepared by embodiment 3;
The SEM figure of the energy-storing dielectric ceramic material of Fig. 6 prepared by embodiment 4;
The SEM figure of the energy-storing dielectric ceramic material of Fig. 7 prepared by embodiment 5;
The relative permittivity of the energy-storing dielectric ceramic material of Fig. 8 prepared by comparative example 1 and embodiment 1 ~ 5 and the temperature variant graph of relation of dielectric loss;
The ferroelectric hysteresis loop figure recorded under the test frequency of 10Hz under the energy-storing dielectric ceramic element room temperature of Fig. 9 prepared by comparative example 1 and embodiment 1 ~ 5.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing, the present invention is described in further detail.
Comparative example 1
Prepare unleaded energy-storing dielectric ceramic material B aTiO
3, step is as follows:
(1) be BaCO according to mol ratio
3: TiO
2the ratio batching of=1:1 (x=0);
(2) be medium by the raw material prepared with dehydrated alcohol, ball milling 24h in the nylon tank adding zirconia ball, dries, is placed in retort furnace and is warming up to 1000 DEG C with 2 DEG C/min temperature rise rate from room temperature, and insulation 2h, furnace cooling obtains BaTiO
3powder;
(3) be medium by the powder obtained in step (2) with dehydrated alcohol, ball milling 12h in the nylon tank adding zirconia ball, dry, in ceramic powder, drip binding agent (2.5wt% polyvinyl alcohol solution) mix granulation, binding agent add-on is 1% of ceramic powder quality, crosses 100 mesh sieves, ageing, dry-pressing formed under 150MPa forming pressure, obtain biscuit of ceramics;
(4) biscuit of ceramics sheet is incubated 2h binder removals in 600 DEG C, be incubated 2h at being then warming up to 1350 DEG C, temperature rise rate 2 DEG C/min, obtains ceramic medium material.
Energy-storing dielectric ceramic comparative example obtained carries out X-ray diffraction (XRD) and scanning electronic microscope (SEM) test.Be illustrated in figure 1 the XRD figure spectrum of this comparative example stupalith, can find out for typical perovskite structure, be Tetragonal under room temperature; Be illustrated in figure 2 the SEM figure of this comparative example stupalith, can find out that ceramic structure is fine and close, average grain size is about 0.9 μm.
The surface rubbing of media ceramic prepared by this comparative example, by after silver electrode, is tested its dielectric properties and ferroelectric properties at polishing.Be illustrated in figure 8 this energy-storing dielectric ceramic specific inductivity and dielectric loss variation with temperature curve under 1kHz frequency, test result shows: the Curie peak of this ceramics sample is at about 135 DEG C, and room temperature dielectric constant is about 3080, and dielectric loss is about 0.022.Be illustrated in figure 9 the ferroelectric hysteresis loop (x=0) of the present embodiment stupalith.Result shows: ferroelectric hysteresis loop is wider fat, and back-shaped area is large, and remnant polarization is large, and disruptive strength is low, is only 78kV/cm.According to energy storage density calculation formula
(wherein) W represents energy storage density, E
brepresent disruptive strength, E represents strength of electric field, and P represents polarizability) to calculate energy storage density be 0.32J/cm
3.
Embodiment 1
Prepare the energy-storing dielectric ceramic material of unleaded high-k, chemical formula is 0.89BaTiO
3-0.11CaSnO
3, step is as follows:
1) be BaCO according to mol ratio
3: CaCO
3: TiO
2: SnO
2the ratio batching of=0.89:0.11:0.89:0.11 (x=0.11);
2) be medium by the raw material prepared with dehydrated alcohol, ball milling 24h in the nylon tank adding zirconia ball, dries, is placed in retort furnace and is warming up to 1000 DEG C with 4 DEG C/min temperature rise rate from room temperature, insulation 2h, and furnace cooling obtains ceramic powder;
3) by step 2) in the powder that obtains take dehydrated alcohol as medium, ball milling 12h in the nylon tank adding zirconia ball, dry, in ceramic powder, drip binding agent (2.5wt% polyvinyl alcohol solution) mix granulation, binding agent add-on is 1% of ceramic powder quality, crosses 100 mesh sieves, ageing 12h, dry-pressing formed under 150MPa forming pressure, obtain ceramic disks biscuit;
4) ceramic disks biscuit is incubated 2h binder removals in 600 DEG C, be incubated 3h at being then warming up to 1350 DEG C, temperature rise rate 2 DEG C/min, obtains ceramic medium material.
The method identical with comparative example 1 is adopted to test the energy-storing dielectric ceramic prepared by the present embodiment.The XRD figure spectrum of the Ceramics Ceramic sample prepared by the present embodiment as shown in fig. 1, known sample is single phase perovskite structure sosoloid, in counterfeit Emission in Cubic, as shown in Figure 3, visible ceramic crystalline grain physically well develops SEM figure, and microtexture is finer and close, Jie's temperature spectrum under 1kHz is as Fig. 8, the Curie peak of sample is at about 40 DEG C, and room temperature dielectric constant is about 10006, and dielectric loss is about 0.028.Be illustrated in figure 9 the ferroelectric hysteresis loop (x=0.11) of the present embodiment stupalith, result shows: compared with comparative example, and ferroelectric hysteresis loop attenuates, and back-shaped area reduces, and sample breakdown intensity is 100kV/cm, and energy storage density is 0.41J/cm
3.
Embodiment 2
Prepare the energy-storing dielectric ceramic material of unleaded high-k, chemical formula is 0.88BaTiO
3-0.12CaSnO
3, step is as follows:
1) be BaCO according to mol ratio
3: CaCO
3: TiO
2: SnO
2the ratio batching of=0.88:0.12:0.88:0.12 (x=0.12);
2) be medium by the raw material prepared with dehydrated alcohol, ball milling 24h in the nylon tank adding zirconia ball, dries, is placed in retort furnace and is warming up to 1000 DEG C with 4 DEG C/min temperature rise rate from room temperature, insulation 2h, and furnace cooling obtains ceramic powder;
3) by step 2) in the powder that obtains take dehydrated alcohol as medium, ball milling 12h in the nylon tank adding zirconia ball, dry, in ceramic powder, drip binding agent (2.5wt% polyvinyl alcohol solution) mix granulation, binding agent add-on is 1% of ceramic powder quality, crosses 100 mesh sieves, ageing 12h, dry-pressing formed under 150MPa forming pressure, obtain ceramic disks biscuit;
4) ceramic disks biscuit is incubated 2h binder removals in 600 DEG C, be incubated 3h at being then warming up to 1380 DEG C, temperature rise rate 2 DEG C/min, obtains ceramic medium material.
The method identical with comparative example 1 is adopted to test the energy-storing dielectric ceramic prepared by the present embodiment.The XRD figure spectrum of the Ceramics Ceramic sample prepared by the present embodiment as shown in fig. 1, known sample is single phase perovskite structure sosoloid, in counterfeit Emission in Cubic, as shown in Figure 4, visible ceramic crystalline grain physically well develops SEM figure, and microtexture is finer and close, Jie's temperature spectrum under 1kHz is as Fig. 8, the Curie peak of sample is at about 28 DEG C, and room temperature dielectric constant is about 11150, and dielectric loss is about 0.029.Be illustrated in figure 9 the ferroelectric hysteresis loop (x=0.12) of the present embodiment stupalith, result shows: compared with comparative example, and ferroelectric hysteresis loop attenuates, and back-shaped area reduces, and sample breakdown intensity is 92kV/cm, and energy storage density is 0.53J/cm
3.
Embodiment 3
Prepare the energy-storing dielectric ceramic material of unleaded high-k, chemical formula is 0.87BaTiO
3-0.13CaSnO
3, step is as follows:
1) be BaCO according to mol ratio
3: CaCO
3: TiO
2: SnO
2the ratio batching of=0.87:0.13:0.87:0.13 (x=0.13);
2) be medium by the raw material prepared with dehydrated alcohol, ball milling 26h in the nylon tank adding zirconia ball, dries, is placed in retort furnace and is warming up to 1100 DEG C with 2 DEG C/min temperature rise rate from room temperature, insulation 3h, and furnace cooling obtains ceramic powder;
3) by step 2) in the powder that obtains take dehydrated alcohol as medium, ball milling 16h in the nylon tank adding zirconia ball, dry, in ceramic powder, drip binding agent (2.5wt% polyvinyl alcohol solution) mix granulation, binding agent add-on is 3% of ceramic powder quality, crosses 100 mesh sieves, ageing 12h, dry-pressing formed under 150MPa forming pressure, obtain ceramic disks biscuit;
4) ceramic disks biscuit is incubated 2h binder removals in 650 DEG C, be incubated 3h at being then warming up to 1380 DEG C, temperature rise rate 2 DEG C/min, obtains ceramic medium material.
The method identical with comparative example 1 is adopted to test the energy-storing dielectric ceramic prepared by the present embodiment.The XRD figure spectrum of the Ceramics Ceramic sample prepared by the present embodiment as shown in fig. 1, known sample is single phase perovskite structure sosoloid, in Emission in Cubic, as shown in Figure 5, visible ceramic crystalline grain physically well develops SEM figure, dense micro-structure, Jie's temperature spectrum under 1kHz is as Fig. 8, the Curie peak of sample is at about 17 DEG C, and room temperature dielectric constant is about 13550, and dielectric loss is about 0.021.Be illustrated in figure 9 the ferroelectric hysteresis loop (x=0.13) of the present embodiment stupalith, result shows: compared with comparative example, ferroelectric hysteresis loop spindle, and back-shaped area reduces, and sample breakdown intensity is 96kV/cm, and energy storage density is 0.76J/cm
3.
Embodiment 4
Prepare the energy-storing dielectric ceramic material of unleaded high-k, chemical formula is 0.86BaTiO
3-0.14CaSnO
3, step is as follows:
1) be BaCO according to mol ratio
3: CaCO
3: TiO
2: SnO
2the ratio batching of=0.86:0.14:0.86:0.14 (x=0.14);
2) be medium by the raw material prepared with dehydrated alcohol, ball milling 26h in the nylon tank adding zirconia ball, dries, is placed in retort furnace and is warming up to 1100 DEG C with 2 DEG C/min temperature rise rate from room temperature, insulation 3h, and furnace cooling obtains ceramic powder;
3) by step 2) in the powder that obtains take dehydrated alcohol as medium, ball milling 16h in the nylon tank adding zirconia ball, dry, in ceramic powder, drip binding agent (2.5wt% polyvinyl alcohol solution) mix granulation, binding agent add-on is 3% of ceramic powder quality, crosses 100 mesh sieves, ageing 12h, dry-pressing formed under 200MPa forming pressure, obtain ceramic disks biscuit;
4) ceramic disks biscuit is incubated 2h binder removals in 650 DEG C, be incubated 2h at being then warming up to 1400 DEG C, temperature rise rate 2 DEG C/min, obtains ceramic medium material.
The method identical with comparative example 1 is adopted to test the energy-storing dielectric ceramic prepared by the present embodiment.The XRD figure spectrum of the Ceramics Ceramic sample prepared by the present embodiment as shown in fig. 1, known sample is single phase perovskite structure sosoloid, in Emission in Cubic, as shown in Figure 6, visible ceramic crystalline grain physically well develops SEM figure, dense micro-structure, Jie's temperature spectrum under 1kHz is as Fig. 8, the Curie peak of sample is at about-2 DEG C, and room temperature dielectric constant is about 11357, and dielectric loss is about 0.008.Be illustrated in figure 9 the ferroelectric hysteresis loop (x=0.14) of the present embodiment stupalith, result shows: compared with comparative example, ferroelectric hysteresis loop spindle, and back-shaped area reduces, and sample breakdown intensity is 125kV/cm, and energy storage density is 0.92J/cm
3.
Embodiment 5
Prepare the energy-storing dielectric ceramic material of unleaded high-k, chemical formula is 0.85BaTiO
3-0.15CaSnO
3, step is as follows:
1) be BaCO according to mol ratio
3: CaCO
3: TiO
2: SnO
2the ratio batching of=0.85:0.15:0.85:0.15 (x=0.15);
2) be medium by the raw material prepared with dehydrated alcohol, ball milling 26h in the nylon tank adding zirconia ball, dries, is placed in retort furnace and is warming up to 1100 DEG C with 2 DEG C/min temperature rise rate from room temperature, insulation 3h, and furnace cooling obtains ceramic powder;
3) by step 2) in the powder that obtains take dehydrated alcohol as medium, ball milling 16h in the nylon tank adding zirconia ball, dry, in ceramic powder, drip binding agent (2.5wt% polyvinyl alcohol solution) mix granulation, binding agent add-on is 3% of ceramic powder quality, crosses 100 mesh sieves, ageing 12h, dry-pressing formed under 200MPa forming pressure, obtain ceramic disks biscuit;
4) ceramic disks biscuit is incubated 2h binder removals in 650 DEG C, be incubated 2h at being then warming up to 1400 DEG C, temperature rise rate 2 DEG C/min, obtains ceramic medium material.
The method identical with comparative example 1 is adopted to test the energy-storing dielectric ceramic prepared by the present embodiment.The XRD figure spectrum of the Ceramics Ceramic sample prepared by the present embodiment as shown in fig. 1, known sample is single phase perovskite structure sosoloid, in Emission in Cubic, as shown in Figure 7, visible ceramic crystalline grain physically well develops SEM figure, dense micro-structure, Jie's temperature spectrum under 1kHz is as Fig. 8, the Curie peak of sample is at about 3 DEG C, and room temperature dielectric constant is about 10100, and dielectric loss is about 0.009.Be illustrated in figure 9 the ferroelectric hysteresis loop (x=0.15) of this comparative example stupalith, result shows: compared with comparative example, the obvious spindle of ferroelectric hysteresis loop, and back-shaped area is little, and sample breakdown intensity is 175kV/cm, and energy storage density is 1.17J/cm
3.The performance index of the energy-storing dielectric ceramic material of table 1 prepared by comparative example 1 and embodiment 1 ~ 5.
Table 1
By the above detailed description to the embodiment of the present invention, can understand and the invention solves pure BaTiO
3the problem that under pottery room temperature, relative permittivity is not high enough, energy storage density is low.Adopt CaSnO
3the component dielectric loss that relative permittivity under material room temperature is increased to more than 10000, x=0.14 and 0.15 by media ceramic prepared by the method for solid solution modification effectively significantly reduces; The disruptive strength of material increases simultaneously, and has elongated ferroelectric hysteresis loop, and the stupalith that these two aspects reason makes the present invention prepare improves BaTiO
3the energy storage density of pottery, reaches 0.41 ~ 1.17J/cm
3.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (7)
1. a unleaded high-k energy-storing dielectric ceramic material, is characterized in that, its chemical formula is (1-x) BaTiO
3-xCaSnO
3, wherein x=0.11 ~ 0.15.
2. a preparation method for unleaded high-k energy-storing dielectric ceramic material, is characterized in that step is as follows:
1) with BaCO
3, CaCO
3, SnO
2and TiO
2for raw material, according to chemical formula (1-x) BaTiO
3-xCaSnO
3middle metallic element stoichiometric ratio batching, wherein x=0.11 ~ 0.15;
2) by step 1) BaCO that takes
3, CaCO
3, SnO
2and TiO
2raw material ball milling mixes, and dries, is placed in retort furnace from room temperature, is warming up to 1000 ~ 1100 DEG C of pre-burning 2 ~ 3h, obtain ceramic powder with stove naturally cooling;
3) by step 2) gained ceramic powder ball milling post-drying, mix with binding agent and grind granulation, ageing 12h after sieving, one side extrusion forming obtains ceramic disks biscuit;
4) by step 3) gained ceramic disks biscuit in 600 ~ 650 DEG C of isothermal holding 2h, be then warming up to 1350 ~ 1400 DEG C sintering 2 ~ 3h, finally obtain unleaded high-k energy-storing dielectric ceramic material with stove naturally cooling.
3. the preparation method of unleaded high-k energy-storing dielectric ceramic material according to claim 2, is characterized in that step 2) and step 3) described ball milling is for adopting zirconia ball, take dehydrated alcohol as medium, the mixing and ball milling time is 12 ~ 26h.
4. the preparation method of unleaded high-k energy-storing dielectric ceramic material according to claim 2, is characterized in that step 2) described temperature rise rate is 2 ~ 4 DEG C/min.
5. the preparation method of unleaded high-k energy-storing dielectric ceramic material according to claim 2, is characterized in that step 3) described binding agent is polyvinyl alcohol water solution, concentration is 2.5wt%, and binding agent add-on is 1 ~ 3% of ceramic powder quality.
6. the preparation method of unleaded high-k energy-storing dielectric ceramic material according to claim 2, is characterized in that step 3) described extrusion forming pressure is 150 ~ 200MPa.
7. the preparation method of unleaded high-k energy-storing dielectric ceramic material according to claim 2, is characterized in that step 4) described temperature rise rate is 2 DEG C/min.
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