CN1587198A - Low temperature sitering and prparing method for lithium blended strontium-barium titanate ceramics - Google Patents
Low temperature sitering and prparing method for lithium blended strontium-barium titanate ceramics Download PDFInfo
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- CN1587198A CN1587198A CN 200410053751 CN200410053751A CN1587198A CN 1587198 A CN1587198 A CN 1587198A CN 200410053751 CN200410053751 CN 200410053751 CN 200410053751 A CN200410053751 A CN 200410053751A CN 1587198 A CN1587198 A CN 1587198A
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Abstract
The present invention relates to the low temperature sintering process of functional strontium-barium titanate ceramic. The present invention features the Ba/Sr ratio range of 0.65-0.75 to 0.25-0.35; and sintering additive Li2CO3 in the amount of 0.2-1 wt% of strontium-barium titanate. The preparation process of the present invention has the strontium-barium titanate sintering temperature lowered by about 200 deg.c, final sintering temperature range up to about 30 deg.c, and temperature maintaining time shortened to 2 hr, while assuring the dielectric performance of the material to meet the requirement as infrared detector.
Description
Technical field
The present invention relates to a kind of strontium-barium titanate (Ba
(1-X)Sr
xTiO
3, be called for short BST) and the low-temperature sintering of function ceramics, or rather, by doping Quilonum Retard (Li
2CO
3) obviously reduce the low-temperature sintering method of BST material sintering temperature, belong to the function ceramics field.
Background technology
Strontium-barium titanate is the ferroelectrics of typical perovskite structure, this system material has high-k, low dielectric loss, and its Curie temperature can have huge market and use by regulating different variation of Ba/Sr ratio with dielectric properties at aspects such as electrical condenser, electro-optical device, ferroelectric memory and phase shifters.
The later stage nineties, in order to reduce the price of thermal infrared imager, open up the commercial market, the BST material begins to be subjected to people in the application aspect the no-refrigeration infrared focal plane thermal imaging system and pays close attention to.The pyroelectricity characteristic of BST material is to be embodied by the electric field enhancing and the temperature variation double effect that apply.BST material work temperature level near Curie temperature, its near Curie temperature the time specific inductivity can produce rapid variation with temperature; Under suitable bias field effect, the BST material can obtain bigger more stable detection efficiency.The adjustability of its excellent pyroelectric property of BST material and Curie temperature makes it can be widely used in the infrared acquisition aspect, as intrusion alarm, and fire alarm sensing, infrared imaging or the like.
Because BST material sintering temperature is very high, if use traditional ceramics preparation technology, final sintering temperature will be incubated 4 hours at 1380 ℃～1400 ℃, even after adopting chemical process to prepare powder, its sintering temperature is also more than 1300 ℃.When for example adopting sol-gel method to prepare the BST pottery, its sintering temperature is generally in (Ceng Huarong, Lin Shengwei etc., Journal of Inorganic Materials, 1999,14 (1): 101-106) more than 1320 ℃; As when using citric acid-nitrate combustion method preparation method, also need be in (Shen Cai etc., Journal of Inorganic Materials, 2004,19 (3): 681-685) more than 1300 ℃.Long-time high temperature sintering between 1300 ℃～1400 ℃, not only energy consumption causes environmental pollution greatly but also easily.Therefore, reducing sintering temperature is the realistic problem that presses for solution.
Goal of the invention
The object of the present invention is to provide a kind of strontium-barium titanate (Ba
(1-X)Sr
xTiO
3, 0.25≤X≤0.35 is called for short BST) and the low-temperature sintering method of function ceramics, can make sintering temperature reduce about 200 ℃, and the optimal sintering temperature scope can reach about 30 degree, soaking time shortens to 2 hours, keeps the dielectric properties of material simultaneously, satisfies the requirement of infrared eye.
Concrete implementation step
1) with commercially available analytical pure BaCO
3, SrCO
3And TiO
2Be starting raw material, the proportional range of Ba/Sr is 0.65～0.75/0.35～0.25;
2) low sintering additive is Li
2CO
3, addition 0.2～1Wt%, the recommendation addition is 0.3Wt%～0.5Wt%.(all being benchmark) with BST
3) preparation technology of employing conventional powder promptly synthesizes at 1150 ℃, is incubated 2 hours, and temperature rise rate is 2～4 ℃/minute.
4) adopt 1100 ℃～1150 ℃ of hot pressed sinterings, pressurize 2 hours, temperature rise rate is 2～4 ℃/minute, pressure is 10MPa.
Low-temperature sintering method advantage provided by the invention:
1) under the sinter additives effect, can make BST material (Ba/Sr=0.65～0.75/0.35～0.25) sintering temperature be reduced to 1100 ℃～1150 ℃, thereby save energy widely.
2) adopted hot-pressing sintering technique, made the BST ceramic density reach 99% of theoretical density; The physical strength of stupalith and processing characteristics thereby be greatly improved are expected to be applied to responsive element chip in the infrared focus plane thermal imaging system.
3) best hot pressing sintering range reaches about 30 degree than broad, and ceramic post sintering preparation technology becomes more readily available control.
4) behind the employing low-temperature sintering method, the grain-size of BST material is reduced.
Description of drawings
Fig. 1 Li doped
2CO
3Ba for 0.5wt%
0.70Sr
0.30TiO
3Concern between volume density and the sintering temperature, X-coordinate be sintering temperature (℃), ordinate zou is volume density (g/cm
3).
Fig. 2 Li doped
2CO
3Be Jie's temperature spectrum of 0.5wt%BST stupalith, X-coordinate be temperature (℃), ordinate zou is a relative permittivity.
Fig. 3 Li doped
2CO
3Be BST relative permittivity and the DC electric field relation of 0.5wt%, X-coordinate is DC electric field (V/mm), and ordinate zou is a relative permittivity.
Fig. 4 Li doped
2CO
3For concerning between the BST volume density of 0.5wt% and the sintering temperature, X-coordinate be sintering temperature (℃), ordinate zou is volume density (g/cm
3).
Fig. 5 Li doped
2CO
3Be Jie's temperature spectrum of 1.0wt%BST stupalith, X-coordinate be temperature (℃), ordinate zou is a relative permittivity.
Fig. 6 Li doped
2CO
3Be BST relative permittivity and the DC electric field relation of 1.0wt%, X-coordinate is DC electric field (V/mm), and ordinate zou is a relative permittivity.
Fig. 7 Li doped
2CO
3Be Jie's temperature spectrum of 0.5wt%BST stupalith, X-coordinate be temperature (℃), ordinate zou is a relative permittivity.
Embodiment
Below by concrete case study on implementation, further to illustrate substantive features of the present invention and obvious improvement:
Embodiment 1. low sintering additives are Li
2CO
3The BST pyroelectric ceramic material
Ba/Sr=70/30 in the BST material is with commercially available analytical pure BaCO
3, SrCO
3And TiO
2Be starting raw material, press Ba
0.70Sr
0.30TiO
3Batching, sintering additive Li
2CO
3Be 0.3Wt%.Adopt the preparation of conditional electronic ceramic process, synthesis condition is 1150 ℃ of insulations 2 hours; The hot pressed sintering temperature is respectively 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, 1150 ℃ insulations 2 hours, hot pressed sintering in logical oxygen atmosphere, and pressure is 10MPa.Its sintered density is respectively 5.594g/cm
3, 5.668g/cm
3, 5.687g/cm
3, 5.690g/cm
3, 5.684g/cm
3, 5.682g/cm
3The theoretical density of this system is 5.746g/cm
3Sample is coated with silver after being processed into needed size, measure its electrical property then.
Embodiment 2. low sintering additives are Li
2CO
3The BST pyroelectric ceramic material
Ba/Sr=70/30 in the BST material is with commercially available analytical pure BaCO
3, SrCO
3And TiO
2Be starting raw material, press Ba
0.70Sr
0.30TiO
3Batching, sintering additive Li
2CO
3Be 0.5Wt%.Adopt the preparation of conditional electronic ceramic process, synthesis condition is 1150 ℃ of insulations 2 hours; The hot pressed sintering temperature is respectively 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, 1150 ℃ insulations 2 hours, hot pressed sintering in logical oxygen atmosphere, and pressure is 10MPa.Its sintered density is respectively 5.694g/cm
3, 5.698g/cm
3, 5.707g/cm
3, 5.717g/cm
3, 5.726g/cm
3, 5.720g/cm
3The theoretical density of this system is 5.746g/cm
3Sample is coated with silver after being processed into needed size, measure its electrical property then.(seeing Fig. 1,2,3)
Embodiment 3. low sintering additives are Li
2CO
3BST pyroelectric ceramics material
Ba/Sr=70/30 in the BST material is with commercially available analytical pure BaCO
3, SrCO
3And TiO
2Be starting raw material, press Ba
0.70Sr
0.30TiO
3Batching, sintering additive Li
2CO
3Be 1Wt%.Adopt the preparation of conditional electronic ceramic process, synthesis condition is 1150 ℃ of insulations 2 hours; The hot pressed sintering temperature is 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, 1150 ℃ insulations 2 hours, hot pressed sintering in logical oxygen atmosphere, and pressure is 10MPa.Its sintered density is respectively 5.710g/cm
3, 5.721g/cm
3, 5.718g/cm
3, 5.709g/cm
3, 5.702g/cm
3, 5.694g/cm
3The theoretical density of this system is 5.746g/cm
3Sample is coated with silver after being processed into needed size, measure its electrical property then.(seeing Fig. 4,5,6)
Embodiment 4. low sintering additives are Li
2CO
3BST pyroelectric ceramics material
Ba/Sr=65/35 in the BST material is with commercially available analytical pure BaCO
3, SrCO
3And TiO
2Be starting raw material, press Ba
0.70Sr
0.30TiO
3Batching, sintering additive Li
2CO
3Be 0.5Wt%.Adopt the preparation of conditional electronic ceramic process, synthesis condition is 1150 ℃ of insulations 2 hours; The hot pressed sintering temperature is 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, 1150 ℃ insulations 2 hours, hot pressed sintering in logical oxygen atmosphere, and pressure is 10MPa.Its sintered density is respectively 5.594g/cm
3, 5.601g/cm
3, 5.627g/cm
3, 5.647g/cm
3, 5.666g/cm
3, 5.631g/cm
3The theoretical density of this system is 5.699g/cm
3Sample is coated with silver after being processed into needed size, measure its electrical property then.(see figure 7)
Claims (4)
1. the low-temperature melt producing method of a barium-strontium titanate ceramic comprises the synthetic and hot pressed sintering of batching, it is characterized in that:
(1) forming general formula is Ba
(1-x)Sr
xTiO
3, the proportional range of Ba/Sr is 0.65～0.75/0.35～0.25;
(2) the low-temperature sintering additive is LiCO
3, addition is 0.2～1Wt%, it is to be benchmark with the strontium-barium titanate;
(3) pre-synthesis temperature is 1150 ℃;
(4) the hot pressed sintering temperature is 1100～1150 ℃, and pressure is 5～15MPa.
2. by the low-temperature melt producing method of the described a kind of barium-strontium titanate ceramic of claim 1, it is characterized in that the addition of sinter additives is 0.3～0.5Wt%, is benchmark with the strontium-barium titanate.
3. by the low-temperature melt producing method of claim 1 or 2 described a kind of barium-strontium titanate ceramics, pressurize is 2 hours when it is characterized in that hot pressed sintering, 2～4 ℃/minute of temperature rise rates.
4. by the low-temperature melt producing method of claim 1 or 2 described a kind of barium-strontium titanate ceramics, it is characterized in that described sintering temperature is at 1120～1140 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404458C (en) * | 2005-11-23 | 2008-07-23 | 中国科学院上海硅酸盐研究所 | Zirconium dioxide mixed modified barium strontium phthalate-magnesium oxide base composite and preparation process thereof |
| CN100412030C (en) * | 2005-05-13 | 2008-08-20 | 中国科学院上海硅酸盐研究所 | Barium strontium titanate base electro-optical composite material and preparation method thereof |
| CN102850050A (en) * | 2012-08-31 | 2013-01-02 | 华中科技大学 | Low temperature sintering piezoelectric ceramic material and preparation method thereof |
| CN114477997A (en) * | 2020-05-20 | 2022-05-13 | 深圳市科思飞科技有限公司 | Ceramic powder and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2553757B1 (en) * | 1983-10-19 | 1991-07-26 | Haussonne Francois | CERAMIC COMPOSITIONS BASED ON TITANIUM OXIDE, THEIR PREPARATION AND THEIR USE AS DIELECTRICS IN ELECTRICAL CAPACITORS |
| CN1103328C (en) * | 2000-04-06 | 2003-03-19 | 中国科学院上海技术物理研究所 | Preparation of strontium-barium titanate film material |
| CN1250482C (en) * | 2003-05-08 | 2006-04-12 | 上海交通大学 | Prep. of strontium titanate barium ceramic target |
-
2004
- 2004-08-13 CN CNB2004100537516A patent/CN100344575C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100412030C (en) * | 2005-05-13 | 2008-08-20 | 中国科学院上海硅酸盐研究所 | Barium strontium titanate base electro-optical composite material and preparation method thereof |
| CN100404458C (en) * | 2005-11-23 | 2008-07-23 | 中国科学院上海硅酸盐研究所 | Zirconium dioxide mixed modified barium strontium phthalate-magnesium oxide base composite and preparation process thereof |
| CN102850050A (en) * | 2012-08-31 | 2013-01-02 | 华中科技大学 | Low temperature sintering piezoelectric ceramic material and preparation method thereof |
| CN114477997A (en) * | 2020-05-20 | 2022-05-13 | 深圳市科思飞科技有限公司 | Ceramic powder and application thereof |
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| CN100344575C (en) | 2007-10-24 |
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