CN101514103A - Method for preparing potassium-sodium niobate-sodium bismuth titanate nano ceramics - Google Patents
Method for preparing potassium-sodium niobate-sodium bismuth titanate nano ceramics Download PDFInfo
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- CN101514103A CN101514103A CNA2009100218320A CN200910021832A CN101514103A CN 101514103 A CN101514103 A CN 101514103A CN A2009100218320 A CNA2009100218320 A CN A2009100218320A CN 200910021832 A CN200910021832 A CN 200910021832A CN 101514103 A CN101514103 A CN 101514103A
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Abstract
The invention discloses a method for preparing potassium-sodium niobate-sodium bismuth titanate nano ceramics, comprising the following steps: analytically pure niobium pentaoxide, sodium carbonate, potassium carbonate, titanium dioxide and bismuth trioxide are mixed and subjected to the procedures of high-energy ball-milling mixing, presintering, cold isostatic pressing, high temperature sintering, and polishing as well as metallic electrode sputtering to finally prepare the potassium-sodium niobate-sodium bismuth titanate nano ceramics; the stoichiometric proportion of the components is (1-x)[(Na0.5Bi0.5)NbO3]-x[(Bi0.5Na0.5)TiO3], wherein x ranges from 0.005 to 0.9. As sosoloid system of the potassium-sodium niobate-sodium bismuth titanate undergoes high-energy ball milling and pressureless sintering, the nanoscale potassium-sodium niobate-sodium bismuth titanate ceramics are prepared; the grain size of the ceramic is reduced from 1-5mum in the prior art to 88-93 nanometers.
Description
Technical field
The present invention relates to a kind of preparation method's of potassium-sodium niobate-sodium bismuth titanate pottery, particularly potassium-sodium niobate-sodium bismuth titanate nano ceramics preparation method.
Background technology
Document " Ruzhong Zuo, Xusheng Fang, and Chun Ye, Phase structures and electrical properties ofnew lead-free Na
0.5K
0.5NbO
3-Bi
0.5Na
0.5TiO
3Ceramics, APPLIED PHYSICS LETTERS 90,092904 (2007) " a kind of preparation method of potassium-sodium niobate-sodium bismuth titanate pottery is disclosed; this method adopts traditional milling method to prepare the potassium-sodium niobate-sodium bismuth titanate pottery in conjunction with the pressureless sintering mode; common light ball alumina balls, zirconia ball and the agate ball ball milling raw material of employing; at the preparation powder initial stage, just be difficult to make original powder to reach nano level.In sintering subsequently, further the growing up of crystal grain makes the grain-size of pottery greatly between 1～5 micron, is difficult to obtain fine and close nano ceramics.
Summary of the invention
In order to overcome the prepared big deficiency of potassium-sodium niobate-sodium bismuth titanate ceramic crystalline grain size of prior art, the invention provides a kind of preparation method of potassium-sodium niobate-sodium bismuth titanate nano ceramics, potassium-sodium niobate-sodium bismuth titanate sosoloid system is carried out high-energy ball milling and pressureless sintering, can prepare the following potassium-sodium niobate-sodium bismuth titanate nano ceramics of 100 nanometers.
The technical solution adopted for the present invention to solve the technical problems: a kind of preparation method of potassium-sodium niobate-sodium bismuth titanate nano ceramics is characterized in comprising the steps:
A kind of preparation method of potassium-sodium niobate-sodium bismuth titanate nano ceramics is characterized in that comprising the steps:
(a), be (1-x) [(Na by stoichiometric ratio with analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide
0.5Bi
0.5) NbO
3]-x[(Bi
0.5Na
0.5) TiO
3] batching, wherein, 0.005＜x＜0.9;
(b) material that will prepare and steel ball are put into high energy ball mill, to add powder quality be 5～45% of steel ball quality; Raw material ball milling 4～16 hours in high energy ball mill, rotating speed is 150～550 rev/mins, does not add any ball-milling medium;
(c) will be through the material of step (b) ball milling 800～1000 ℃ of temperature lower calcinations 1～3 hour;
(d) take out the incinerating material and smash, high-energy ball milling is 1～3 hour again;
(e) the metal die pressing machine compression moulding of putting into diameter 5～15mm of the material powder behind the ball milling again, pressure is 50～150MPa, the base substrate of moulding is packed in the vacuum bag, exhaust vacuum, put into pressing machine, be pressurized to 300～650MPa, keep-uped pressure 3～10 minutes, and made biscuit of ceramics;
(f) biscuit of ceramics is put into sintering oven, 900～1200 ℃ of sintering temperatures 2～4 hours.
The invention has the beneficial effects as follows: because potassium-sodium niobate-sodium bismuth titanate sosoloid system is carried out high-energy ball milling and pressureless sintering, prepared nano level potassium-sodium niobate-sodium bismuth titanate nano ceramics, the grain-size of pottery is reduced to 88～93 nanometers by 1～5 micron of prior art.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is the microstructure photo of the embodiment of the invention 1 prepared potassium-sodium niobate-sodium bismuth titanate nano ceramics.
Fig. 2 is the microstructure photo of the embodiment of the invention 2 prepared potassium-sodium niobate-sodium bismuth titanate nano ceramics.
Embodiment
Embodiment 1, is raw material with analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide powder, and 120 ℃ of oven dry are after 24 hours, according to chemical formula 0.94Na
0.5K
0.5NbO
3-0.06Bi
0.5Na
0.5TiO
3Proportioning, raw materials weighing powder.The gained powder is directly put into the high energy ball mill that is added with steel ball without any special processing, to add powder quality be 5% of steel ball quality, carry out the mechanical alloying ball milling, do not add any ball-milling medium, the ball milling time is 8 hours, and rotating speed is 550 rev/mins; Powder after having ground was calcined 1 hour down at 850 ℃, made each material powder fully react; Take out the incinerating material and smash, high-energy ball milling is 1 hour again, and the niobate material powder behind the ball milling is put into the metal die pressing machine compression moulding of diameter 10mm again, and pressure is 100MPa.In order to improve green body quality, the base substrate of precompressed is packed in the vacuum bag, exhaust vacuum, to put in the oil press, pressure is 650MPa, keep-ups pressure 3 minutes, makes biscuit of ceramics.Then base substrate was carried out sintering 4 hours under 1090 ℃, to obtain the higher piezoelectric ceramics of density.The piezoelectric ceramics that sintering is later, through operation such as sanding and polishing, under the temperature that is lower than sintering temperature 100K, thermal etching half hour.Use scanning electronic microscope JEM-6460LV, observe the microtexture pattern (see figure 1) of piezoelectric ceramics.Use intercept method to calculate grain-size, obtaining its grain-size is 91 nanometers.
Embodiment 2, are raw material with analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide powder, and 120 ℃ of oven dry are after 24 hours, according to chemical formula 0.80Na
0.5K
0.5NbO
3-0.20Bi
0.5Na
0.5TiO
3Proportioning, the various material powders of weighing.The gained powder is directly put into the high energy ball mill that is added with steel ball without any special processing, to add powder quality be 25% of steel ball quality, carry out the mechanical alloying ball milling, do not add any ball-milling medium, the ball milling time is 4 hours, and rotating speed is 450 rev/mins; Powder after having ground was calcined 3 hours down at 800 ℃, made each material powder fully react; Take out the incinerating material and smash, high-energy ball milling is 2 hours again, and the niobate material powder behind the ball milling is put into the metal die pressing machine compression moulding of diameter 5mm again, and pressure is 100MPa.In order to improve green body quality, the base substrate of precompressed is packed in the vacuum bag, exhaust vacuum, to put in the oil press, pressure is 550MPa, keep-ups pressure 5 minutes, makes biscuit of ceramics.Then base substrate was carried out sintering 4 hours under 1090 ℃, to obtain the higher piezoelectric ceramics of density.The piezoelectric ceramics that sintering is later, through operation such as sanding and polishing, under the temperature that is lower than sintering temperature 100K, thermal etching half hour.Use scanning electronic microscope JEM-6460LV, observe the microtexture pattern (see figure 2) of piezoelectric ceramics.Use intercept method to calculate grain-size, obtaining its grain-size is 88 nanometers.
Embodiment 3, are raw material with analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide powder, and 120 ℃ of oven dry are after 24 hours, according to chemical formula 0.90Na
0.5K
0.5NbO
3-0.10Bi
0.5Na
0.5TiO
3Proportioning, the various material powders of weighing.The gained powder is directly put into the high energy ball mill that is added with steel ball without any special processing, to add powder quality be 35% of steel ball quality, carry out the mechanical alloying ball milling, do not add any ball-milling medium, the ball milling time is 12 hours, and rotating speed is 350 rev/mins; Powder after having ground was calcined 2 hours down at 900 ℃, made each material powder fully react; Take out the incinerating material and smash, high-energy ball milling is 2 hours again, and the niobate material powder behind the ball milling is put into the metal die pressing machine compression moulding of diameter 15mm again, and pressure is 50MPa.In order to improve green body quality, the base substrate of precompressed is packed in the vacuum bag, exhaust vacuum, to put in the oil press, pressure is 450MPa, keep-ups pressure 8 minutes, makes biscuit of ceramics.Then base substrate was carried out sintering 2 hours under 900 ℃, to obtain the higher piezoelectric ceramics piezoelectric ceramics of density.The piezoelectric ceramics that sintering is later, through operation such as sanding and polishing, under the temperature that is lower than sintering temperature 100K, thermal etching half hour.Use scanning electronic microscope JEM-6460LV, observe the microtexture pattern of piezoelectric ceramics, use intercept method to calculate grain-size, obtaining its grain-size is 93 nanometers.
Embodiment 4, are raw material with analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide, and 120 ℃ of oven dry are after 24 hours, according to chemical formula 0.50Na
0.5K
0.5NbO
3-0.50Bi
0.5Na
0.5TiO
3Proportioning, the various material powders of weighing.The gained powder is directly put into the high energy ball mill that is added with steel ball without any special processing, to add powder quality be 45% of steel ball quality, carry out the mechanical alloying ball milling, do not add any ball-milling medium, the ball milling time is 16 hours, and rotating speed is 150 rev/mins; Powder after having ground was calcined 2.5 hours down at 1000 ℃, made each material powder fully react; Take out the incinerating material and smash, high-energy ball milling is 3 hours again, and the niobate material powder behind the ball milling is put into the metal die pressing machine compression moulding of diameter 15mm again, and pressure is 150MPa.In order to improve green body quality, the base substrate of precompressed is packed in the vacuum bag, exhaust vacuum, to put in the oil press, pressure is 300MPa, keep-ups pressure 10 minutes, makes biscuit of ceramics.Then base substrate was carried out sintering 4 hours under 1200 ℃, to obtain the higher piezoelectric ceramics piezoelectric ceramics of density.The piezoelectric ceramics that sintering is later, through operation such as sanding and polishing, under the temperature that is lower than sintering temperature 100K, thermal etching half hour.Use scanning electronic microscope JEM-6460LV, observe the microtexture pattern of piezoelectric ceramics, use intercept method to calculate grain-size, obtaining its grain-size is 89 nanometers.
The present invention through repeatedly experiment, has all prepared the following potassium-sodium niobate-sodium bismuth titanate nano ceramics of 100 nanometers according to following steps.With analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide, be (1-x) [(Na by stoichiometric ratio
0.5Bi
0.5) NbO
3]-x[(Bi
0.5Na
0.5) TiO
3] batching, wherein, 0.005＜x＜0.9.The material and the steel ball that prepare are put into high energy ball mill, to add powder quality be 5～45% of steel ball quality.Raw material ball milling 4～16 hours in high energy ball mill, rotating speed is 150～550 rev/mins, does not add any ball-milling medium.The material that ball milling is crossed was 800～1000 ℃ of temperature lower calcinations 1～3 hour.Take out the incinerating material and smash, high-energy ball milling is 1～3 hour again.Material powder behind the ball milling is put into the metal die pressing machine compression moulding of diameter 5～15mm again, and pressure is 50～150MPa, and the base substrate of moulding is packed in the vacuum bag, exhaust vacuum, put into pressing machine, be pressurized to 300～650MPa, keep-uped pressure 3～10 minutes, and made biscuit of ceramics.Biscuit of ceramics is put into sintering oven,, make nano level potassium-sodium niobate-sodium bismuth titanate nano ceramics 900～1200 ℃ of sintering temperatures 2～4 hours.
Claims (1)
1, a kind of preparation method of potassium-sodium niobate-sodium bismuth titanate nano ceramics is characterized in that comprising the steps:
(a), be (1-x) [(Na by stoichiometric ratio with analytical pure level Niobium Pentxoxide, yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide
0.5Bi
0.5) NbO
3]-x[(Bi
0.5Na
0.5) TiO
3] batching, wherein, 0.005＜x＜0.9;
(b) material that will prepare and steel ball are put into high energy ball mill, to add powder quality be 5～45% of steel ball quality; Raw material ball milling 1～16 hour in high energy ball mill, rotating speed is 150～550 rev/mins, does not add any ball-milling medium;
(c) will be through the material of step (b) ball milling 800～1000 ℃ of temperature lower calcinations 1～3 hour;
(d) take out the incinerating material and smash, high-energy ball milling is after 1～3 hour again;
(e) the metal die pressing machine compression moulding of putting into diameter 5～15mm of the material powder behind the ball milling again, pressure is 50～150MPa, the base substrate of moulding is packed in the vacuum bag, exhaust vacuum, put into pressing machine, be pressurized to 300～650MPa, keep-uped pressure 3～10 minutes, and made biscuit of ceramics;
(f) biscuit of ceramics is put into sintering oven, 900～1200 ℃ of sintering temperatures 2～4 hours.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891475A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Preparation method of potassium-sodium niobate-potassium-bismuth titanate nano ceramics |
| CN101891474A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics and preparation method thereof |
| CN102234195A (en) * | 2010-04-23 | 2011-11-09 | 四川师范大学 | Potassium-sodium niobate and sodium lithium bismuth titanate-system lead-free piezoelectric ceramic composition |
| CN103360071A (en) * | 2013-07-18 | 2013-10-23 | 上海隆添新材料科技有限公司 | Production method of potassium sodium niobate/sodium bismuth titanate composite-phase piezoelectric ceramic |
| CN105523760A (en) * | 2015-11-27 | 2016-04-27 | 北京工业大学 | Preparation method for sodium columbate ceramic material with stable antiferroelectricity and low dielectric loss |
| CN110372372A (en) * | 2019-07-31 | 2019-10-25 | 贵州大学 | The preparation method of the bismuth-sodium titanate base lead-free piezoelectric ceramic of low-dielectric loss under high temperature |
| CN116477944A (en) * | 2022-12-02 | 2023-07-25 | 湖南大学 | Potassium sodium niobate-based leadless piezoelectric ceramic and preparation method and application thereof |
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2009
- 2009-04-03 CN CNA2009100218320A patent/CN101514103A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234195A (en) * | 2010-04-23 | 2011-11-09 | 四川师范大学 | Potassium-sodium niobate and sodium lithium bismuth titanate-system lead-free piezoelectric ceramic composition |
| CN101891475A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Preparation method of potassium-sodium niobate-potassium-bismuth titanate nano ceramics |
| CN101891474A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics and preparation method thereof |
| CN103360071A (en) * | 2013-07-18 | 2013-10-23 | 上海隆添新材料科技有限公司 | Production method of potassium sodium niobate/sodium bismuth titanate composite-phase piezoelectric ceramic |
| CN105523760A (en) * | 2015-11-27 | 2016-04-27 | 北京工业大学 | Preparation method for sodium columbate ceramic material with stable antiferroelectricity and low dielectric loss |
| CN105523760B (en) * | 2015-11-27 | 2018-08-28 | 北京工业大学 | A kind of preparation method of the sodium niobate ceramic material of the low-dielectric loss of stable anti-ferroelectricity |
| CN110372372A (en) * | 2019-07-31 | 2019-10-25 | 贵州大学 | The preparation method of the bismuth-sodium titanate base lead-free piezoelectric ceramic of low-dielectric loss under high temperature |
| CN110372372B (en) * | 2019-07-31 | 2021-12-17 | 贵州大学 | Preparation method of sodium bismuth titanate-based lead-free piezoelectric ceramic with low dielectric loss at high temperature |
| CN116477944A (en) * | 2022-12-02 | 2023-07-25 | 湖南大学 | Potassium sodium niobate-based leadless piezoelectric ceramic and preparation method and application thereof |
| CN116477944B (en) * | 2022-12-02 | 2024-07-16 | 湖南大学 | Potassium sodium niobate-based leadless piezoelectric ceramic and preparation method and application thereof |
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Open date: 20090826 |