CN101851093B - Method for preparing barium titanate nano powder - Google Patents
Method for preparing barium titanate nano powder Download PDFInfo
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- CN101851093B CN101851093B CN2010102021818A CN201010202181A CN101851093B CN 101851093 B CN101851093 B CN 101851093B CN 2010102021818 A CN2010102021818 A CN 2010102021818A CN 201010202181 A CN201010202181 A CN 201010202181A CN 101851093 B CN101851093 B CN 101851093B
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Abstract
The invention discloses a method for preparing barium titanate nano powder for solving the technical problem that the conventional method for preparing the barium titanate nano powder has high calcining temperature. The invention adopts the technical scheme that the method comprises the following steps of: adding barium octahydrate and tetrabutyl titanate into a reaction container, sealing the reaction container, then putting the reaction container into a tube furnace introduced with nitrogen atmosphere, and calcining the mixture to obtain carbon-containing barium titanate powder; calcining the carbon-containing barium titanate powder in the air to remove carbon; washing the barium titanate powder after carbon removal by using hydrochloric acid, and repeatedly flushing and filtering the barium titanate powder by using deionized water till the pH value of the filtered deionized water is neutral; and drying the barium titanate powder in an oven. Because the pressure in the closed reaction container is improved by using the gas released in a tetrabutyl titanate cracking process, the calcining temperature of the barium titanate nano powder preparation process is reduced to about 650 to 750 DEG C from 900 DEG C of the background technology.
Description
Technical field
The present invention relates to a kind of preparing method's of nano-powder, particularly a kind of Barium Titanate nano-powder preparation method.
Background technology
Barium titanate is a kind of crucial electron ceramic material, in scientific research and Industrial products, is widely used.In order to adapt to the development trend of device miniatureization, the Barium Titanate nano-powder that processability is good becomes new developing direction.At present, prepare the Barium Titanate nano-powder complicated process of preparation through wet chemistry method, cost is higher.
Document " Li Xia, Li Zhenwen, coprecipitation method synthetic with research; piezoelectricity and acousto-optic, 31 (4), 2009; 528-534 " a kind of preparation method of Barium Titanate nano-powder is disclosed, document adopts coprecipitation method, to have made particle diameter be the barium carbonate powder of 60nm through optimizing other processing condition such as dispersant concentration, calcining temperature; But the preparation process is complicated, and influence factors such as temperature of reaction, additive concentration are more, and has just obtained the barium carbonate powder of pure phase 900 ℃ of calcinings; Calcining temperature is higher, from the XRD figure spectrum that document provides, finds out that the crystallinity of powder is bad.
Summary of the invention
In order to overcome the high deficiency of preparing method's calcination temperature of existing Barium Titanate nano-powder, the present invention provides a kind of preparation method of Barium Titanate nano-powder.This method is a raw material with barium hydroxide, tetra-n-butyl titanate, utilizes the gas that discharges in the tetra-n-butyl titanate cracking process to improve the pressure in the closed reaction vessel, can reduce the calcination temperature that Barium Titanate nano-powder prepares process.
The technical solution adopted for the present invention to solve the technical problems: a kind of preparation method of Barium Titanate nano-powder is characterized in comprising the steps:
(a) in reaction vessel, add barium hydroxide and tetra-n-butyl titanate respectively, wherein the mol ratio of barium hydroxide and tetra-n-butyl titanate is 1: 1～1.5: 1;
(b) be fired to 650～750 ℃ with putting into the tube furnace that is connected with nitrogen atmosphere after the reactor drum sealing, be incubated 2～4 hours, obtain containing the barium carbonate powder of carbon;
The barium carbonate powder that (c) will contain carbon is fired to 500～600 ℃ in air, be incubated decarburization in 20～40 minutes;
(d) with the barium titanate powder body and function hydrochloric acid after decarburization washing, with deionized water washing and filtering repeatedly, the pH value of the deionized water after filtering is a neutrality again;
(e) place baking oven to dry barium carbonate powder.
Useful result of the present invention is: owing to utilize the gas that discharges in the tetra-n-butyl titanate cracking process to improve the pressure in the closed reaction vessel, the calcination temperature that Barium Titanate nano-powder prepares process is reduced to about 650～750 ℃ by 900 ℃ of background technology.
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
Description of drawings
Fig. 1 is the X ray diffracting spectrums of the different barium titaniums of the inventive method than the barium carbonate powder for preparing under the condition.
Fig. 2 is the transmission electron microscope photo of the barium carbonate powder of embodiment 4 preparations.
Embodiment
Following examples are with reference to Fig. 1～2.
Embodiment 1, in reaction vessel, adds 1.3918g barium hydroxide and 1.5ml tetra-n-butyl titanate respectively, and wherein the mol ratio of barium hydroxide and tetra-n-butyl titanate is 1: 1; Reactor drum is tightened sealing, again reactor drum is put into the tube furnace that is connected with nitrogen atmosphere and be fired to 750 ℃, be incubated 2 hours, obtain containing the barium carbonate powder of carbon; The barium carbonate powder that will contain carbon is fired to 500 ℃ of decarburizations in air, be incubated 40 minutes; Powder after the decarburization is used the salt acid elution, and again with deionized water washing and filtering repeatedly, the pH value of the deionized water after filtering is a neutrality; Place baking oven to dry powder again.(a) is the barium titanium than being the X ray diffracting spectrum of 1 o'clock barium carbonate powder among Fig. 1; As can be seen from the figure; Use the barium titanium than still having anatase titania to exist in the prepared barium carbonate powder of the presoma that is 1, obtaining prepared barium carbonate powder tetragonality through the calculating lattice constant is 1.0026.
Embodiment 2, in reaction vessel, add 1.5310g barium hydroxide and 1.5ml tetra-n-butyl titanate respectively, and wherein the mol ratio of barium hydroxide and tetra-n-butyl titanate is 1.1: 1; Reactor drum is tightened sealing, again reactor drum is put into the tube furnace that is connected with nitrogen atmosphere and be fired to 700 ℃, be incubated 3.5 hours, obtain containing the barium carbonate powder of carbon; The barium carbonate powder that will contain carbon is fired to 520 ℃ of decarburizations in air, be incubated 35 minutes; Powder after the decarburization is used the salt acid elution, and again with deionized water washing and filtering repeatedly, the pH value of the deionized water after filtering is a neutrality; Place baking oven to dry powder again.(b) is that barium titanium ratio is the X ray diffracting spectrum of 1.1: 1 o'clock barium carbonate powders among Fig. 1; As can be seen from the figure; Use barium titanium ratio is to still have anatase titania to exist in the prepared barium carbonate powder of 1.1: 1 presoma, and obtaining prepared barium carbonate powder tetragonality through the calculating lattice constant is 1.0033.
Embodiment 3, in reaction vessel, add 1.8093g barium hydroxide and 1.5ml tetra-n-butyl titanate respectively, and wherein the mol ratio of barium hydroxide and tetra-n-butyl titanate is 1.3: 1; Reactor drum is tightened sealing, again reactor drum is put into the tube furnace that is connected with nitrogen atmosphere and be fired to 730 ℃, be incubated 3 hours, obtain containing the barium carbonate powder of carbon; The barium carbonate powder that will contain carbon is fired to 550 ℃ of decarburizations in air, be incubated half a hour; Powder after the decarburization is used the salt acid elution, and again with deionized water washing and filtering repeatedly, the pH value of the deionized water after filtering is a neutrality; Place baking oven to dry powder again.(c) is that barium titanium ratio is the X ray diffracting spectrum of 1.3: 1 o'clock barium carbonate powders among Fig. 1; As can be seen from the figure; Use barium titanium ratio is to still have anatase titania to exist in the prepared barium carbonate powder of 1.3: 1 presoma, and obtaining prepared barium carbonate powder tetragonality through the calculating lattice constant is 1.0077.
Embodiment 4, in reaction vessel, add 2.0877g barium hydroxide and 1.5ml tetra-n-butyl titanate respectively, and wherein the mol ratio of barium hydroxide and tetra-n-butyl titanate is 1.5: 1; Reactor drum is tightened sealing, again reactor drum is put into the tube furnace that is connected with nitrogen atmosphere and be fired to 650 ℃, be incubated 4 hours, obtain containing the barium carbonate powder of carbon; The barium carbonate powder that will contain carbon is fired to 600 ℃ of decarburizations in air, be incubated 20 minutes; Powder after the decarburization is used the salt acid elution, and again with deionized water washing and filtering repeatedly, the pH value of the deionized water after filtering is a neutrality; Place baking oven to dry powder again.(d) is that barium titanium ratio is the X ray diffracting spectrum of 1.5: 1 o'clock barium carbonate powders among Fig. 1; As can be seen from the figure; Using barium titanium ratio is that 1.5: 1 the prepared barium carbonate powder of presoma is tetragonal phase structure, does not have other dephasigns, and to obtain its tetragonality be 1.0058 through calculating lattice constant.Fig. 2 is that barium titanium ratio is the transmission electron microscope photo of 1.5: 1 o'clock prepared barium carbonate powders, and as can be seen from the figure, powder dispersity is good, and the average crystal grain size is about 100nm.
The barium carbonate powder purity that the present invention prepares is high, dispersiveness and good crystallinity, and particle diameter is approximately 100nm, and has tetragonal phase structure.
Claims (1)
1. the preparation method of a Barium Titanate nano-powder is characterized in that comprising the steps:
(a) in reaction vessel, add barium hydroxide and tetra-n-butyl titanate respectively, wherein the mol ratio of barium hydroxide and tetra-n-butyl titanate is 1: 1～1.5: 1;
(b) be fired to 650～750 ℃ with putting into the tube furnace that is connected with nitrogen atmosphere after the reactor drum sealing, be incubated 2～4 hours, obtain containing the barium carbonate powder of carbon;
The barium carbonate powder that (c) will contain carbon is fired to 500～600 ℃ in air, be incubated decarburization in 20～40 minutes;
(d) with the barium titanate powder body and function hydrochloric acid after decarburization washing, with deionized water washing and filtering repeatedly, the pH value of the deionized water after filtering is a neutrality again;
(e) place baking oven to dry barium carbonate powder.
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| CN106861669B (en) * | 2017-02-27 | 2019-06-04 | 陕西科技大学 | A kind of porous laminated structure metatitanic acid particle and preparation method thereof |
| CN111192763B (en) * | 2020-03-12 | 2021-11-30 | 东北大学秦皇岛分校 | Preparation method of barium titanate-based all-solid-state capacitor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1800030A (en) * | 2005-12-20 | 2006-07-12 | 湘潭大学 | Process for preparing barium titanate nano-rod |
| CN101045554A (en) * | 2007-03-12 | 2007-10-03 | 胜利油田华鑫石油材料有限公司 | Method for preparing uniform dispersion square phase barium titanate nanocrystal |
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| CN1800030A (en) * | 2005-12-20 | 2006-07-12 | 湘潭大学 | Process for preparing barium titanate nano-rod |
| CN101045554A (en) * | 2007-03-12 | 2007-10-03 | 胜利油田华鑫石油材料有限公司 | Method for preparing uniform dispersion square phase barium titanate nanocrystal |
Non-Patent Citations (1)
| Title |
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| 陈杰.《微波液相合成钛酸锶钡纳米粉体》.《压电与声光》.2009,第31卷(第4期),第523-524、527页. * |
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