CN103787415B - Solvent-thermal method is adopted to prepare the method for lithium tantalate nano powder - Google Patents
Solvent-thermal method is adopted to prepare the method for lithium tantalate nano powder Download PDFInfo
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- CN103787415B CN103787415B CN201410031457.9A CN201410031457A CN103787415B CN 103787415 B CN103787415 B CN 103787415B CN 201410031457 A CN201410031457 A CN 201410031457A CN 103787415 B CN103787415 B CN 103787415B
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- deionized water
- lithium tantalate
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Abstract
The invention discloses a kind of method adopting solvent-thermal method to prepare lithium tantalate nano powder, the method comprises following concrete steps: with the mixed solvent of deionized water and ethylene glycol for reaction solvent, with Li
2cO
3and Ta
2o
5for reaction raw materials, temperature of reaction is 240 DEG C, reaction times 12h, obtained lithium tantalate nano powder; Wherein, raw material is with molar ratio computing Ta:Li=1:4.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.Nano-powder crystal grain prepared by the present invention tiny complete, regular shape, purity are higher, soilless sticking or few to reunite and without the need to high-temperature calcination process.
Description
Technical field
What the present invention relates to is that one prepares 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 ratio and ethylene glycol as reaction solvent, adopt that solvent-thermal method prepares uniform crystal particles, purity is high, reunite few LiTaO
3powder, belongs to ceramic powder synthesis field.
Background technology
LiTaO
3be a kind of important ferroelectric material, the research and development of Lead-free ferroelectric ceramics were increasingly competitive in recent years, LiTaO
3the premium properties of pottery receives the extensive concern of numerous scholars.Preparation LiTaO
3usually have the methods such as molten-salt growth method, coprecipitation method, sol-gel method and hydrothermal method, but main in generation and synthesis technology exist three problems: (1) current synthetic technology is difficult to synthesize the tiny nano particle of size uniform crystal grain; (2) due to cost intensive, most nano-powder synthetic technology is made not realize industrialization; (3) cannot effectively being solved from agglomeration traits of nano-powder.Above problem limits LiTaO to a great extent
3widespread use.
Through finding the literature search of prior art, publication number is the LiTaO that the Chinese patent of CN103011839A discloses 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 " molten-salt growth method synthesis LiTaO at " Chinese Journal of Inorganic Chemistry " (in August, 2006, the 8th phase, 1491-1494 page)
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 without the wet mixing of deionized water ethanol again, powder is fully mixed, dry, at 650 ~ 900 DEG C, react 3 h in air atmosphere, furnace cooling, repeatedly clean for several times, until filtrate can't detect Cl with Silver Nitrate reagent with the deionization deionized water of heat
-till, at 120 DEG C, dry obtained LiTaO
3, owing to requiring that temperature is 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 preparation LiTaO of powder grain fine uniform
3the method of nano-powder.
For achieving the above object, the invention provides a kind of method adopting solvent-thermal method to prepare lithium tantalate nano powder, the method comprises following concrete steps: with the mixed solvent of deionized water and ethylene glycol for reaction solvent, with Li
2cO
3and Ta
2o
5for reaction raw materials, temperature of reaction is 240 DEG C, reaction times 12h, obtained lithium tantalate nano powder; Wherein, raw material is with molar ratio computing Ta:Li=1:4.
Above-mentioned method, wherein, in described mixed solvent, with volume basis, deionized water: ethylene glycol=1 ~ 4:1.
More preferably, in described mixed solvent, with volume basis, deionized water: ethylene glycol=1:1.
Because the present invention's mixing deionized water and ethylene glycol are organic solvent, by test different ratio, developing best organic solvent volume proportioning is deionized water: ethylene glycol=1:1.Nano-powder crystal grain prepared by the present invention tiny complete, regular shape, purity are higher, soilless sticking or few to reunite and without the need to high-temperature calcination process.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 DEG C, reaction 12h.After reaction terminates, filter, and priority is washed three times with deionized water respectively and dehydrated alcohol washes twice, guarantees 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
3containing a small amount of Ta in powder
2o
5.unreacted is complete, there is 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 selection volume ratio is deionized water and the ethylene glycol of 1:1, and temperature of reaction is 240 DEG C, reaction 12h.After reaction terminates, filter, and priority is washed three times with deionized water respectively and dehydrated alcohol washes twice, guarantees 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, as shown in Figure 1 (b wherein represents the spectrogram of embodiment 2).Observe through scanning electron microscope (SEM), size of microcrystal scope is 100-150nm, and degree of crystallinity is better, and crystal is cubic cylindricality, basic soilless sticking phenomenon.
Embodiment 3
According to mol ratio Ta:Li=1:4, Li
2cO
3for 2g, Ta
2o
5for 2.99g, solvent volume is than the deionized water and the ethylene glycol that are 2:1, and temperature of reaction is 240 DEG C, reaction 12h.After reaction terminates, filter, and priority is washed three times with deionized water respectively and dehydrated alcohol washes twice, guarantees 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 comparatively embodiment 2 is poor, as shown in Figure 1 (c wherein represents the spectrogram of embodiment 3), there is micro-dephasign.Observe through scanning electron microscope (SEM), size of microcrystal scope is 200-250nm, and degree of crystallinity is better, and partial crystals 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 the deionized water and the ethylene glycol that are 4:1, and temperature of reaction is 240 DEG C, reaction 12h.After reaction terminates, filter, and priority is washed three times with deionized water respectively and dehydrated alcohol washes twice, guarantees 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 containing a small amount of impurity, but comparatively embodiment 1 slightly well, comparatively embodiment 3 is slightly poor, as shown in Figure 1 (d wherein represents the spectrogram of embodiment 4), there is micro-dephasign.Observe through scanning electron microscope (SEM), size of microcrystal scope is 250-300nm, and degree of crystallinity is poor, and crystal is many in irregular shape, and part has agglomeration.
Although content of the present invention has done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple amendment 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: with the mixed solvent of deionized water and ethylene glycol for reaction solvent, with Li
2cO
3and Ta
2o
5for reaction raw materials, temperature of reaction is 240 DEG C, reaction times 12h, obtained 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, with volume basis, and deionized water: ethylene glycol=1 ~ 4:1.
3. method as claimed in claim 2, is characterized in that, in described mixed solvent, with volume basis, and 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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| 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 true CN103787415B (en) | 2015-08-19 |
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| 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 |
| CN104163454B (en) * | 2014-09-01 | 2016-01-20 | 中山大学 | A kind of preparation method of lithium tantalate |
| 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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