CN102515747A - High-dielectric constant voltage-resistant rare earth-doped strontium titanate ceramic and preparation method thereof - Google Patents
High-dielectric constant voltage-resistant rare earth-doped strontium titanate ceramic and preparation method thereof Download PDFInfo
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- CN102515747A CN102515747A CN2011104285637A CN201110428563A CN102515747A CN 102515747 A CN102515747 A CN 102515747A CN 2011104285637 A CN2011104285637 A CN 2011104285637A CN 201110428563 A CN201110428563 A CN 201110428563A CN 102515747 A CN102515747 A CN 102515747A
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- earth
- withstand voltage
- tio
- strontium titanate
- metatitanic acid
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- 239000000919 ceramic Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims description 22
- 229910052712 strontium Inorganic materials 0.000 claims description 21
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000011812 mixed powder Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000007908 dry granulation Methods 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 238000004146 energy storage Methods 0.000 abstract description 10
- 239000003989 dielectric material Substances 0.000 abstract description 4
- 229910052761 rare earth metal Inorganic materials 0.000 abstract 1
- 150000002910 rare earth metals Chemical class 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000013215 result calculation Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种高介耐压稀土掺杂钛酸锶陶瓷，以化学通式NdxSr1-1.5xTiO3表示，其中x为Nd的摩尔数，0＜x≤0.2。此外还公开了上述高介耐压稀土掺杂钛酸锶陶瓷的制备方法。本发明显著提高了钛酸锶陶瓷产品的相对介电常数，与此同时也保证并增加了耐电压强度，实现了钛酸锶陶瓷体系材料的技术突破，从而有效提高了钛酸锶陶瓷产品的储能密度及综合性能，拓展了其作为高压储能介电材料的应用领域，能够极大地促进该体系材料的推广和应用。
The invention discloses a rare-earth-doped strontium titanate ceramic with high medium and voltage resistance, which is represented by the general chemical formula Nd x Sr 1-1.5x TiO 3 , wherein x is the mole number of Nd, and 0<x≤0.2. In addition, a preparation method of the above-mentioned high-dielectric withstand voltage rare-earth doped strontium titanate ceramic is also disclosed. The invention significantly improves the relative permittivity of strontium titanate ceramic products, at the same time ensures and increases the withstand voltage strength, and realizes a technological breakthrough of strontium titanate ceramic system materials, thereby effectively improving the strontium titanate ceramic products. The energy storage density and comprehensive performance have expanded its application field as a high-voltage energy storage dielectric material, and can greatly promote the promotion and application of this system material.
Description
Technical field
The present invention relates to technical field of function materials, relate in particular to a kind of strontium titanate ceramics and preparation method thereof.
Background technology
Strontium titanate (SrTiO
3) pottery is a kind of important functional material, is widely used in fields such as electronics, mechanical industry.Strontium titanate ceramics is a cube phase structure under the room temperature, is paraelectrics, has higher relative permittivity (ε
r～300), and since its unlike ferroelectric bulk ceramic (like BaTiO
3) there is the instability of domain wall in such inside, so strontium titanate ceramics also has higher proof voltage intensity (E when thickness of sample is 1.0 ± 0.05mm
b～10kV/mm), have higher ε simultaneously thereby possess
rAnd E
bPeculiar property.For this reason in recent years, the strontium titanate base pottery is considered to one of solid-state energy-accumulating medium material system that has development potentiality.
Because strontium titanate ceramics can be similar to and think linear dielectric medium, so its energy storage density γ that uses as solid-state energy-accumulating medium material can express with following formula:
ε wherein
rBe relative permittivity, the strength of electric field of E for pottery is applied.
This shows, realize in the strontium titanate ceramics that more the key of high energy storage density is to obtain simultaneously higher relative permittivity and proof voltage intensity.Yet; Because the relative permittivity and the proof voltage intensity of dielectric material are the parameters of a pair of relative contradiction; Therefore the research of the strontium titanate base pottery energy storage material progress of making a breakthrough property never; Prior art is when obtaining more high relative dielectric constant, and its proof voltage intensity just significantly reduces; And under the situation that guarantees proof voltage intensity, relative permittivity can not be significantly improved again.Therefore, prior art strontium titanate base pottery energy storage density is difficult to effective raising, and its over-all properties has also received very big influence, thereby has limited the use range of strontium titanate base pottery, and its promotion and application have also received obstruction.For this reason, how to obtain to take into account simultaneously and have high-k and be to be badly in need of the technical problem that solves and break through at present than the strontium titanate ceramics of high withstand voltage intensity.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art; Provide a kind of taking into account simultaneously to have high-k and ceramic than the rear-earth-doped metatitanic acid strontium of high withstand voltage intensity; Thereby effectively improve the energy storage density of ceramic product, expand it in Application Areas as the high-voltage energy storage dielectric materials.Another object of the present invention is to provide the preparation method of the above-mentioned high withstand voltage rear-earth-doped metatitanic acid strontium pottery that is situated between.
The object of the invention is achieved through following technical scheme:
A kind of high Jie provided by the invention is withstand voltage, and rear-earth-doped metatitanic acid strontium is ceramic, with chemical general formula Nd
xSr
1-1.5xTiO
3Expression, wherein x is the mole number of Nd, 0＜x≤0.2, preferred 0.008≤x≤0.2.
Another object of the present invention is achieved through following technical scheme:
The preparation method of the above-mentioned high withstand voltage rear-earth-doped metatitanic acid strontium pottery that is situated between provided by the invention may further comprise the steps:
(1) with SrCO
3, Nd
2O
3And TiO
2Take by weighing batching as raw material according to said chemical general formula;
(2) said raw material ball mill mixing, the oven dry back obtains mixed powder;
(3) said mixed powder is incubated 3～5 hours synthetic Nd that obtain under 1050～1200 ℃ of temperature
xSr
1-1.5xTiO
3Powder;
(4) said Nd
xSr
1-1.5xTiO
3After powder carried out secondary ball milling, oven dry granulation, compression moulding obtained ceramic body;
(5) behind the said ceramic body intensification plastic removal, 1250～1380 ℃ of sintering temperature insulations 2～6 hours, making chemical constitution was Nd
xSr
1-1.5xTiO
3The height withstand voltage rear-earth-doped metatitanic acid strontium pottery that is situated between.
Further, in step according to the invention (2)/(4), be medium with water, by quality than raw material/powder: ball: water=1: 1.2: 1～1.2 ball millings 6～10 hours.
Further, in the step according to the invention (4), be that the polyvinyl alcohol water solution of 1.0～5.0wt% carries out granulation as sticker with concentration, its consumption is said Nd
xSr
1-1.5xTiO
35～15wt% of powder weight.
The present invention has following beneficial effect:
The rear-earth-doped metatitanic acid strontium ceramic formula system that the present invention adopted has significantly improved the relative permittivity of ceramic product; Meanwhile also guarantee and increased proof voltage intensity; Realized the technological breakthrough of strontium titanate ceramics system material; Thereby effectively improved the energy storage density and the over-all properties of ceramic product, expanded its Application Areas as the high-voltage energy storage dielectric materials.Simultaneously; Preparing method's technology of the present invention is simple, and the formula system that is adopted has increased the transmission course of material, has promptly quickened the diffusion process of material; Thereby greatly reduce sintering temperature; The preparation process is easy to control, and the ceramic product steady quality is reliable, can greatly promote the promotion and application of this system material.
Description of drawings
To combine embodiment and accompanying drawing that the present invention is made further detailed description below:
Fig. 1 be the high withstand voltage rear-earth-doped metatitanic acid strontium ceramics sample that is situated between of the embodiment of the invention the XRD figure spectrum.
Embodiment
The high withstand voltage rear-earth-doped metatitanic acid strontium pottery that is situated between of the embodiment of the invention, its chemical general formula is Nd
xSr
1-1.5xTiO
3, adopt analytical pure SrCO
3, Nd
2O
3And TiO
2For starting raw material prepares.Formulation parameter and the raw material consumption in the preparation process in its chemical general formula of each embodiment are as shown in table 1.
The formulation parameter and the raw material consumption of table 1 embodiment one～six rear-earth-doped metatitanic acid strontium pottery
Based on above-mentioned formulating of recipe, the preparation method of the high withstand voltage rear-earth-doped metatitanic acid strontium pottery that is situated between of the embodiment of the invention is following:
(1) with SrCO
3, Nd
2O
3And TiO
2Take by weighing batching as raw material according to consumption shown in the table 1;
(2) by quality than raw material: the agate ball mill: deionized water=1: 1.2: 1 planetary ball mill 6 hours, the oven dry back obtains mixed powder;
(3) mixed powder is incubated 3～5 hours synthetic Nd that obtain under 1050～1200 ℃ of temperature
xSr
1-1.5xTiO
3Powder;
(4) press mass ratio Nd
xSr
1-1.5xTiO
3Powder: agate ball mill: deionized water=1: 1.2: 1 planetary ball mill 8 hours, ball milling slurry are crossed oven dry under air atmosphere behind 120 mesh sieves; The polyvinyl alcohol water solution that in the oven dry powder, adds concentration then and be 2.5wt% carries out granulation as sticker, and its consumption is 8% of oven dry powder weight; Powder after the granulation obtains ceramic body in the moulding of 100～120Mpa pressure pressed after crossing 40 mesh sieves;
(5) behind the eliminating sticker that slowly heats up under 600～650 ℃ of temperature, 1250～1380 ℃ of sintering temperatures insulations 2～6 hours, make chemical constitution was Nd to ceramic body in air
xSr
1-1.5xTiO
3The height withstand voltage rear-earth-doped metatitanic acid strontium ceramics sample that is situated between.
Various embodiments of the present invention preparing method's processing parameter is seen table 2.
The preparation technology parameter of table 2 embodiment one～six rear-earth-doped metatitanic acid strontium pottery
The be situated between XRD figure spectrum of withstand voltage rear-earth-doped metatitanic acid strontium ceramics sample of the height that various embodiments of the present invention make is as shown in Figure 1, and tests in following condition: volume density adopts Archimedes's drainage to measure; Specific density is the ratio (theoretical density obtains according to the XRD test result calculations) of volume density and theoretical density; Relative permittivity is that frequency is that 1MHz measures down; (specimen thickness is 1.0 ± 0.05mm) to be to measure in the medium with insulating transformer oil to proof voltage intensity.Probe temperature is room temperature.The performance index of the ceramics sample that test obtains are as shown in table 3.
The performance index of table 3 embodiment one～six rear-earth-doped metatitanic acid strontium ceramics sample
Table 3 result shows that the high relative permittivity that is situated between withstand voltage rear-earth-doped metatitanic acid strontium ceramics sample of the embodiment of the invention has had significant raising, meanwhile also guarantees and has increased proof voltage intensity, has realized the technological breakthrough of strontium titanate ceramics system material.
Claims (5)
1. the withstand voltage rear-earth-doped metatitanic acid strontium pottery of high Jie is characterized in that: with chemical general formula Nd
xSr
1-1.5xTiO
3Expression, wherein x is the mole number of Nd, 0＜x≤0.2.
2. the high withstand voltage rear-earth-doped metatitanic acid strontium pottery that is situated between according to claim 1, it is characterized in that: said x is 0.008≤x≤0.2.
3. the preparation method of claim 1, one of the 2 said high withstand voltage rear-earth-doped metatitanic acid strontium potteries that are situated between may further comprise the steps:
(1) with SrCO
3, Nd
2O
3And TiO
2Take by weighing batching as raw material according to said chemical general formula;
(2) said raw material ball mill mixing, the oven dry back obtains mixed powder;
(3) said mixed powder is incubated 3～5 hours synthetic Nd that obtain under 1050～1200 ℃ of temperature
xSr
1-1.5xTiO
3Powder;
(4) said Nd
xSr
1-1.5xTiO
3After powder carried out secondary ball milling, oven dry granulation, compression moulding obtained ceramic body;
(5) behind the said ceramic body intensification plastic removal, 1250～1380 ℃ of sintering temperature insulations 2～6 hours, making chemical constitution was Nd
xSr
1-1.5xTiO
3The height withstand voltage rear-earth-doped metatitanic acid strontium pottery that is situated between.
4. the preparation method of the high withstand voltage rear-earth-doped metatitanic acid strontium pottery that is situated between according to claim 3 is characterized in that: in said step (2)/(4), be medium with water, by quality than raw material/powder: ball: water=1: 1.2: 1～1.2 ball millings 6～10 hours.
5. according to the preparing methods of claim 3 or the 4 described high withstand voltage rear-earth-doped metatitanic acid strontiums potteries that are situated between, it is characterized in that: in the said step (4), be that the polyvinyl alcohol water solution of 1.0～5.0wt% carries out granulation as sticker with concentration, its consumption is said Nd
xSr
1-1.5xTiO
35～15wt% of powder weight.
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|---|---|---|---|
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| CN2011104285637A CN102515747A (en) | 2011-12-20 | 2011-12-20 | High-dielectric constant voltage-resistant rare earth-doped strontium titanate ceramic and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174943A (en) * | 2015-09-22 | 2015-12-23 | 桂林电子科技大学 | Dielectric energy storage ceramic and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962540A (en) * | 2006-11-13 | 2007-05-16 | 武汉理工大学 | High-energy-storage density solid energy-storage medium ceramics and its preparing process |
| CN102219506A (en) * | 2011-04-13 | 2011-10-19 | 武汉理工大学 | Rare earth Nd and SiO2 doped SrTiO3 based dielectric ceramics and its preparation method |
-
2011
- 2011-12-20 CN CN2011104285637A patent/CN102515747A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962540A (en) * | 2006-11-13 | 2007-05-16 | 武汉理工大学 | High-energy-storage density solid energy-storage medium ceramics and its preparing process |
| CN102219506A (en) * | 2011-04-13 | 2011-10-19 | 武汉理工大学 | Rare earth Nd and SiO2 doped SrTiO3 based dielectric ceramics and its preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 沈宗洋: "稀土Nd掺杂SrTiO3基高储能介质陶瓷缺陷结构及介电性能研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174943A (en) * | 2015-09-22 | 2015-12-23 | 桂林电子科技大学 | Dielectric energy storage ceramic and preparation method thereof |
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Application publication date: 20120627 |