CN103787415A - Method for preparing lithium tantalate nano-powder by adopting solvothermal method - Google Patents
Method for preparing lithium tantalate nano-powder by adopting solvothermal method Download PDFInfo
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- CN103787415A CN103787415A CN201410031457.9A CN201410031457A CN103787415A CN 103787415 A CN103787415 A CN 103787415A CN 201410031457 A CN201410031457 A CN 201410031457A CN 103787415 A CN103787415 A CN 103787415A
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Abstract
The invention discloses a method for preparing lithium tantalate nano-powder by adopting a solvothermal method. The method comprises the following specific step: preparing the lithium tantalite nano-powder by taking a mixed solvent of deionized water and ethylene glycol as a reaction solvent, taking Li2CO3 and Ta2O5 as reaction raw materials and reacting at the temperature of 240 DEG C for 12 hours, wherein the molar ratio of Ta to Li as the raw materials is 1:4. The process method has the advantages of low reaction temperature, complete reaction, small quantity of impurities, high purity, easiness and convenience in operating and suitability for batch production. The prepared nano-powder is fine and complete in crystalline grains, regular in shape, high in purity, and free from of aggregation or slight in aggregation, and does not need high-temperature calcination treatment.
Description
Technical field
What the present invention relates to is that one is prepared lithium tantalate
(liTaO
3 )the method of powder, specifically with Quilonum Retard
(li
2cO
3 )and tantalum pentoxide
(ta
2o
5 )for main raw material, utilize the deionized water of different proportionings and ethylene glycol as reaction solvent, adopt that solvent-thermal method is prepared uniform crystal particles, purity is high, few LiTaO reunites
3powder, belongs to the synthetic field of ceramic powder.
Background technology
LiTaO
3be a kind of important ferroelectric material, the research and development of Lead-free ferroelectric ceramics are in recent years increasingly competitive, LiTaO
3the premium properties of pottery has been subject to numerous scholars' extensive concern.Preparation LiTaO
3conventionally there are the methods such as molten-salt growth method, coprecipitation method, sol-gel method and hydrothermal method, still, three problems of main existence in preparation and synthetic technology: (1) current synthetic technology is difficult to the synthetic tiny nano particle of size uniform crystal grain; (2), due to cost costliness, make most nano-powder synthetic technology can not realize industrialization; (3) cannot effectively being solved from agglomeration traits of nano-powder.Above problem has limited LiTaO to a great extent
3widespread use.
Through the literature search of prior art is found, the Chinese patent that publication number is CN103011839A discloses the LiTaO of the standby cube bulk of a kind of deionization hydro-thermal legal system and the granular mixed structure of bead
3the method of lead-free piezoelectric ceramic powder, the method deficiency is: the reaction times is longer, cannot obtain highly purified LiTaO
3nano-powder.Also find by literature search, Li Lihong etc. have delivered at " Chinese Journal of Inorganic Chemistry " (in August, 2006, the 8th phase, 1491-1494 page) that " molten-salt growth method is synthesized LiTaO
3powder ", concrete grammar is: with LiCl, Li
2cO
3, Ta
2o
5for raw material, raw materials weighing according to a certain ratio, then it is ground with agate mortar, add again without the wet mixing of deionized water ethanol, make powder fully mix, be dried, under air atmosphere, at 650 ~ 900 ℃, react 3 h, furnace cooling, repeatedly clean for several times with hot deionization deionized water, until filtrate can't detect Cl with Silver Nitrate reagent
-till, at 120 ℃, dry and make LiTaO
3, owing to requiring temperature higher, be not suitable for batch production.
By retrieving existing patent and document, do not find to use solvent-thermal method to prepare LiTaO
3the report of nano-powder.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of production method simple, the tiny uniform preparation LiTaO of powder crystal grain
3the method of nano-powder.
For achieving the above object, the invention provides a kind of method that adopts solvent-thermal method to prepare lithium tantalate nano powder, the method comprises following concrete steps: take the mixed solvent of deionized water and ethylene glycol as reaction solvent, with Li
2cO
3and Ta
2o
5for reaction raw materials, temperature of reaction is 240 ℃, and reaction times 12h, makes lithium tantalate nano powder; Wherein, raw material is with molar ratio computing Ta:Li=1:4.
Above-mentioned method, wherein, in described mixed solvent, in volume ratio, deionized water: ethylene glycol=1 ~ 4:1.
More preferably, in described mixed solvent, in volume ratio, deionized water: ethylene glycol=1:1.
Because the present invention's mixing deionized water and ethylene glycol are organic solvent, by testing different proportionings, developing best organic solvent volume proportion is deionized water: ethylene glycol=1:1.Tiny complete, the regular shape of nano-powder crystal grain prepared by the present invention, purity be higher, without reuniting or few reunite and without high-temperature calcination processing.Processing method of the present invention, temperature of reaction is lower, reacts completely, and impurity is few, and purity is high, easy and simple to handle, is applicable to batch production.
Accompanying drawing explanation
Fig. 1 is the spectrogram of the X-ray diffraction detected result of embodiment 1-4.
Embodiment
Below in conjunction with embodiment and accompanying drawing, technical scheme of the present invention is further described.
Embodiment 1
According to mol ratio Ta:Li=1:4, Li
2cO
3for 2g, Ta
2o
5for 2.99g, solvent only has deionized water, and temperature of reaction is 240 ℃, reaction 12h.After reaction finishes, filter, and successively wash three times with deionized water respectively and wash twice with dehydrated alcohol, guarantee unnecessary Li
2cO
3wash LiTaO
3be insoluble to deionized water, ethylene glycol and dehydrated alcohol, remain as throw out.
The LiTaO that the present embodiment obtains
3in powder, contain a small amount of Ta
2o
5.unreacted is complete, has dephasign, as shown in Figure 1 (a wherein represents the spectrogram of embodiment 1).Observe through scanning electron microscope (SEM), size of microcrystal scope is 250-300nm, and degree of crystallinity is poor, and crystal is irregular shape, has agglomeration.
Embodiment 2
According to mol ratio Ta:Li=1:4, Li
2cO
3for 2g, Ta
2o
5for 2.99g, solvent is selected deionized water and the ethylene glycol that volume ratio is 1:1, and temperature of reaction is 240 ℃, reaction 12h.After reaction finishes, filter, and successively wash three times with deionized water respectively and wash twice with dehydrated alcohol, guarantee unnecessary Li
2cO
3wash LiTaO
3be insoluble to deionized water, ethylene glycol and dehydrated alcohol, remain as throw out.
The LiTaO that the present embodiment obtains
3powder inclusion-free, reacts completely, without dephasign, and (b wherein represents the spectrogram of embodiment 2) as shown in Figure 1.Observe through scanning electron microscope (SEM), size of microcrystal scope is 100-150nm, and degree of crystallinity is better, and crystal is cubic cylindricality, substantially without agglomeration.
Embodiment 3
According to mol ratio Ta:Li=1:4, Li
2cO
3for 2g, Ta
2o
5for 2.99g, solvent volume is than deionized water and ethylene glycol for 2:1, and temperature of reaction is 240 ℃, reaction 12h.After reaction finishes, filter, and successively wash three times with deionized water respectively and wash twice with dehydrated alcohol, guarantee unnecessary Li
2cO
3wash LiTaO
3be insoluble to deionized water, ethylene glycol and dehydrated alcohol, remain as throw out.
The LiTaO that the present embodiment obtains
3powder is containing trace impurity, and poor compared with embodiment 2, (c wherein represents the spectrogram of embodiment 3), exists micro-dephasign as shown in Figure 1.Observe through scanning electron microscope (SEM), size of microcrystal scope is 200-250nm, and degree of crystallinity is better, and part crystal is cubic cylindricality, has a small amount of agglomeration.
Embodiment 4
According to mol ratio Ta:Li=1:4, Li
2cO
3for 2g, Ta
2o
5for 2.99g, solvent volume is than deionized water and ethylene glycol for 4:1, and temperature of reaction is 240 ℃, reaction 12h.After reaction finishes, filter, and successively wash three times with deionized water respectively and wash twice with dehydrated alcohol, guarantee unnecessary Li
2cO
3wash LiTaO
3be insoluble to deionized water, ethylene glycol and dehydrated alcohol, remain as throw out.
The LiTaO that the present embodiment obtains
3powder is containing a small amount of impurity, but compared with embodiment 1 slightly well, slightly poor compared with embodiment 3, (d wherein represents the spectrogram of embodiment 4), exists micro-dephasign as shown in Figure 1.Observe through scanning electron microscope (SEM), size of microcrystal scope is 250-300nm, and degree of crystallinity is poor, and crystal is irregular shape more, and part has agglomeration.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.Read after foregoing those skilled in the art, for multiple modification of the present invention and substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (3)
1. adopt solvent-thermal method to prepare a method for lithium tantalate nano powder, it is characterized in that, the method comprises following concrete steps: take the mixed solvent of deionized water and ethylene glycol as reaction solvent, with Li
2cO
3and Ta
2o
5for reaction raw materials, temperature of reaction is 240 ℃, and reaction times 12h, makes lithium tantalate nano powder; Wherein, raw material is with molar ratio computing Ta:Li=1:4.
2. the method for claim 1, is characterized in that, in described mixed solvent, and in volume ratio, deionized water: ethylene glycol=1 ~ 4:1.
3. method as claimed in claim 2, is characterized in that, in described mixed solvent, and in volume ratio, deionized water: ethylene glycol=1:1.
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| CN201410031457.9A CN103787415B (en) | 2014-01-23 | 2014-01-23 | Solvent-thermal method is adopted to prepare the method for lithium tantalate nano powder |
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| CN103787415B CN103787415B (en) | 2015-08-19 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833079A (en) * | 2014-02-14 | 2014-06-04 | 上海海事大学 | Method for preparation of lithium tantalate nano-powder by hydrothermal process |
| CN104163454A (en) * | 2014-09-01 | 2014-11-26 | 中山大学 | Preparing method of lithium tantalate crystal |
| CN113716533A (en) * | 2021-08-04 | 2021-11-30 | 杭州赛聚科技有限公司 | Preparation method of intelligent material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090286702A1 (en) * | 2008-05-19 | 2009-11-19 | Baker Hughes Incorporated | Using Nanoparticles for Water Flow Control in Subterranean Formations |
| CN101602596A (en) * | 2009-07-24 | 2009-12-16 | 中国地质大学（北京） | A kind of lithium tantalate nano powder and preparation method thereof |
-
2014
- 2014-01-23 CN CN201410031457.9A patent/CN103787415B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090286702A1 (en) * | 2008-05-19 | 2009-11-19 | Baker Hughes Incorporated | Using Nanoparticles for Water Flow Control in Subterranean Formations |
| CN101602596A (en) * | 2009-07-24 | 2009-12-16 | 中国地质大学（北京） | A kind of lithium tantalate nano powder and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 马守涛: "水热合成钽酸锂纳米粉及其介电性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833079A (en) * | 2014-02-14 | 2014-06-04 | 上海海事大学 | Method for preparation of lithium tantalate nano-powder by hydrothermal process |
| CN104163454A (en) * | 2014-09-01 | 2014-11-26 | 中山大学 | Preparing method of lithium tantalate crystal |
| CN104163454B (en) * | 2014-09-01 | 2016-01-20 | 中山大学 | A kind of preparation method of lithium tantalate |
| CN113716533A (en) * | 2021-08-04 | 2021-11-30 | 杭州赛聚科技有限公司 | Preparation method of intelligent material |
| CN113716533B (en) * | 2021-08-04 | 2022-11-18 | 杭州赛聚科技有限公司 | Preparation method of intelligent material |
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| CN103787415B (en) | 2015-08-19 |
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