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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Abstract
The invention discloses high-dielectric constant voltage-resistant rare earth-doped strontium titanate ceramic. The high-dielectric constant voltage-resistant rare earth-doped strontium titanate ceramic has a general chemical formula of NdxSr1-1.5xTiO3, wherein x represents the mole number of Nd and is greater than 0 and less than or equal to 0.2. The invention also discloses a preparation method of the high-dielectric constant voltage-resistant rare earth-doped strontium titanate ceramic. The preparation method obviously improves a relative dielectric constant of a strontium titanate ceramic product, guarantees and improves dielectric strength of the strontium titanate ceramic product, realizes the technical breakthrough of a strontium titanate ceramic system material, effectively improves energy storage density and comprehensive performances of the strontium titanate ceramic product, develops an application range of the strontium titanate ceramic system material as a high-voltage energy-storage dielectric material, and greatly improves popularization and application of the strontium titanate ceramic 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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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)
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| 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-base dielectric ceramic and preparation method thereof |
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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-base dielectric ceramic and preparation method thereof |
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 |