CN103833079A - Method for preparation of lithium tantalate nano-powder by hydrothermal process - Google Patents

Method for preparation of lithium tantalate nano-powder by hydrothermal process Download PDF

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Publication number
CN103833079A
CN103833079A CN201410050490.6A CN201410050490A CN103833079A CN 103833079 A CN103833079 A CN 103833079A CN 201410050490 A CN201410050490 A CN 201410050490A CN 103833079 A CN103833079 A CN 103833079A
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lithium tantalate
reaction
nano powder
powder
lithium
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高林强
陈海
邹鑫
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Shanghai Maritime University
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Shanghai Maritime University
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Abstract

The invention discloses a method for preparation of lithium tantalate nano-powder by a hydrothermal process. The method includes: using deionized water as a reaction solvent, adding a lithium source and a tantalum source, ensuring the mole ratio of tantalum ions to lithium ions at 1:(1-8), carrying out reaction for 8-24h in an autoclave, keeping the reaction temperature at 200-260DEG C, and at the end of the reaction, firstly conducting washing by deionized water, and then performing washing by an alcohol solvent, thus obtaining the lithium tantalate nano-powder. The lithium source is LiOH or Li2CO3, and the tantalum source is Ta(OH)5 or Ta2O5. The method provided by the invention adopts different lithium sources and different tantalum sources as the raw materials, and takes deionized water as a reaction solvent to synthesize the LiTaO3 nano-powder. The prepared LiTaO3 powder has a regular shape, fine, complete and uniform grains, high purity, no aggregation or less agglomeration, and has no need for high-temperature calcination treatment. The method provided by the invention has the advantages of fewer steps, simple preparation, short reaction time, low reaction temperature, and is suitable for mass production.

Description

Hydrothermal method is prepared lithium tantalate nano powder
Technical field
The present invention relates to lithium tantalate nano powder preparation field, specifically, is that hydrothermal method is prepared lithium tantalate nano powder.
Background technology
Lithium tantalate (LiTaO 3) be a kind of important ferroelectric piezoelectric, the research and development of leadless piezoelectric 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 deionization hydro-thermal 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, in air, at 650～900 DEG C, react 3 h, furnace cooling, repeatedly clean for several times with hot deionized water, until filtrate can't detect Cl with Silver Nitrate reagent -till, at 120 DEG C, dry and make LiTaO 3, owing to requiring temperature higher, be not suitable for batch production.
Summary of the invention
The object of the invention is, for deficiency of the prior art, provides hydrothermal method to prepare lithium tantalate nano powder, and this production method is simple, the LiTaO of preparation 3nano-powder crystal grain is tiny evenly.
For achieving the above object, the technical scheme that the present invention takes is:
Hydrothermal method is prepared lithium tantalate nano powder, utilize deionized water for reaction solvent, add He Tan source, lithium source, the mol ratio that ensures tantalum ion and lithium ion is 1: (1～8), in autoclave, to react 8～24 hours, temperature of reaction is 200～260 DEG C, after reaction finishes, first use deionized water wash, then with alcoholic solvent washing, obtain lithium tantalate nano powder;
Described lithium source is LiOH or Li 2cO 3, described tantalum source is Ta (OH) 5or Ta 2o 5.
Preferably, described lithium source is Li 2cO 3, described tantalum source is Ta (OH) 5.
Wherein, described alcoholic solvent is selected from any in ethanol, methyl alcohol, Virahol or n-propyl alcohol.
Preferably, described alcoholic solvent is ethanol.
Preferably, the mol ratio of described tantalum ion and lithium ion is 1: (1.5～3.5).
The most preferred mol ratio of described tantalum ion and lithium ion is 1: 2.
Preferably, the described reaction times is 10～14 hours, most preferably 12 hours.
Preferably, described temperature of reaction is 230～250 DEG C, most preferably 240 DEG C.
Further, described autoclave is magnetic force rotary stirring high-pressure kettle.
The size of microcrystal of lithium tantalate nano powder prepared by employing the inventive method is 100～500 nanometers.
The invention has the advantages that:
1, the inventive method is with different lithium source (LiOH, Li 2cO 3) and different tantalums source (Ta (OH) 5, Ta 2o 5) for raw material, taking deionized water as reaction solvent synthetic LiTaO 3nano-powder, the LiTaO making 3powder regular shape, crystal grain is tiny complete and even, and purity is higher, without reuniting or few reunite and without high-temperature calcination processing;
2, the inventive method step is few, and preparation is simple, and the reaction times is short, and temperature of reaction is lower, is applicable to large-scale mass production.
Brief description of the drawings
Accompanying drawing 1 is the scanning electron microscope (SEM) photograph of lithium tantalate nano powder in embodiment 1.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below embodiment provided by the invention is elaborated; The present embodiment is implemented under taking technical solution of the present invention as prerequisite, has provided detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment.
embodiment 1
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 150mL, then add 1g Li 2cO 3with 3.59g Ta (OH) 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 2, to react 12 hours, temperature of reaction is 240 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washing with alcohol 2 times, obtains lithium tantalate nano powder.The scanning electron microscope (SEM) photograph of lithium tantalate nano powder is shown in accompanying drawing 1, and size of microcrystal is 100～150nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, crystal is cubic cylindricality, without agglomeration.
embodiment 2
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 180mL, then add 1g Li 2cO 3with 2.983g Ta 2o 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 2, to react 12 hours, temperature of reaction is 240 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washing with alcohol 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 200～250nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 3
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 200mL, then add 1g LiOH and 2.63g Ta 2o 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 3.5, to react 12 hours, temperature of reaction is 240 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washing with alcohol 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 250～300nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 4
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 170mL, then add 1g LiOH and 3.164g Ta (OH) 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 3.5, to react 12 hours, temperature of reaction is 240 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washing with alcohol 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 200～250nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 5
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 160mL, then add 1g Li 2cO 3with 3.987g Ta 2o 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 1.5, to react 18 hours, temperature of reaction is 200 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses methanol wash 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 150～200nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 6
In stirring-type autoclave, add reaction solvent deionized water 190mL, then add 1g LiOH and 2.3g Ta 2o 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 4, to react 20 hours, temperature of reaction is 250 DEG C, after reaction finishes, first uses deionized water wash 2 times, then with n-propyl alcohol washing 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 150～250nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 7
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 180mL, then add 1g LiOH and 2.22g Ta (OH) 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 5, to react 10 hours, temperature of reaction is 260 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washed with isopropyl alcohol 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 200～350nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 8
In stirring-type autoclave, add reaction solvent deionized water 150mL, then add 1g Li 2cO 3with 1.199g Ta (OH) 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 6, to react 15 hours, temperature of reaction is 245 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses methanol wash 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 200～250nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 9
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 180mL, then add 1g Li 2cO 3with 2.88g Ta (OH) 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 2.5, to react 24 hours, temperature of reaction is 220 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washing with alcohol 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 200～300nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 10
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 200mL, then add 1g LiOH and 3.7g Ta (OH) 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 3, to react 8 hours, temperature of reaction is 230 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washed with isopropyl alcohol 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 150～250nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 11
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 150mL, then add 1g Li 2cO 3with 7.19g Ta (OH) 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 1, to react 14 hours, temperature of reaction is 250 DEG C, after reaction finishes, first uses deionized water wash 2 times, then with n-propyl alcohol washing 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 100～200nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 12
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 150mL, then add 1g Li 2cO 3with 0.75g Ta 2o 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 8, to react 16 hours, temperature of reaction is 230 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washing with alcohol 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 200～500nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
embodiment 13
In magnetic force rotary stirring high-pressure kettle, add reaction solvent deionized water 150mL, then add 1g LiOH and 1.586g Ta (OH) 5, ensure that the mol ratio of tantalum ion and lithium ion is 1: 7, to react 9 hours, temperature of reaction is 240 DEG C, after reaction finishes, first uses deionized water wash 2 times, then uses washing with alcohol 2 times, obtains lithium tantalate nano powder.Lithium tantalate nano powder size of microcrystal is 150～400nm, powder inclusion-free, and degree of crystallinity is better and without dephasign, regular shape.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (10)

1. hydrothermal method is prepared lithium tantalate nano powder, it is characterized in that, utilize deionized water for reaction solvent, add He Tan source, lithium source, ensure that the mol ratio of tantalum ion and lithium ion is 1: (1～8), in autoclave, react 8～24 hours, temperature of reaction is 200～260 DEG C, after reaction finishes, first uses deionized water wash, with alcoholic solvent washing, obtain lithium tantalate nano powder again;
Described lithium source is LiOH or Li 2cO 3, described tantalum source is Ta (OH) 5or Ta 2o 5.
2. hydrothermal method according to claim 1 is prepared lithium tantalate nano powder, it is characterized in that, described lithium source is Li 2cO 3, described tantalum source is Ta (OH) 5.
3. hydrothermal method according to claim 1 is prepared lithium tantalate nano powder, it is characterized in that, described alcoholic solvent is selected from any in ethanol, methyl alcohol, Virahol or n-propyl alcohol.
4. hydrothermal method according to claim 3 is prepared lithium tantalate nano powder, it is characterized in that, described alcoholic solvent is ethanol.
5. hydrothermal method according to claim 1 is prepared lithium tantalate nano powder, it is characterized in that, described tantalum ion and the mol ratio of lithium ion are 1: (1.5～3.5).
6. hydrothermal method according to claim 5 is prepared lithium tantalate nano powder, it is characterized in that, described tantalum ion and the mol ratio of lithium ion are 1: 2.
7. hydrothermal method according to claim 1 is prepared lithium tantalate nano powder, it is characterized in that, the described reaction times is 10～14 hours.
8. hydrothermal method according to claim 1 is prepared lithium tantalate nano powder, it is characterized in that, described temperature of reaction is 230～250 DEG C.
9. hydrothermal method according to claim 1 is prepared lithium tantalate nano powder, it is characterized in that, described autoclave is magnetic force rotary stirring high-pressure kettle.
10. hydrothermal method according to claim 1 is prepared lithium tantalate nano powder, it is characterized in that, the size of microcrystal of described lithium tantalate nano powder is 100～500 nanometers.
CN201410050490.6A 2014-02-14 2014-02-14 Method for preparation of lithium tantalate nano-powder by hydrothermal process Pending CN103833079A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104163454A (en) * 2014-09-01 2014-11-26 中山大学 Preparing method of lithium tantalate crystal
CN109207000A (en) * 2018-06-07 2019-01-15 太仓萃励新能源科技有限公司 A kind of preparation method of nano-negative ion clear dope
CN111111645A (en) * 2019-12-27 2020-05-08 吉林大学 Enhanced LiTaO3Photocatalytic method

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CN1754014A (en) * 2003-03-06 2006-03-29 信越化学工业株式会社 Process for producing lithium tantalate crystal
CN1856597A (en) * 2003-10-16 2006-11-01 住友金属矿山株式会社 Lithium tantalate substrate and method for producing same
CN103787415A (en) * 2014-01-23 2014-05-14 上海海事大学 Method for preparing lithium tantalate nano-powder by adopting solvothermal method

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Publication number Priority date Publication date Assignee Title
CN1754014A (en) * 2003-03-06 2006-03-29 信越化学工业株式会社 Process for producing lithium tantalate crystal
CN1856597A (en) * 2003-10-16 2006-11-01 住友金属矿山株式会社 Lithium tantalate substrate and method for producing same
CN103787415A (en) * 2014-01-23 2014-05-14 上海海事大学 Method for preparing lithium tantalate nano-powder by adopting solvothermal method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109207000A (en) * 2018-06-07 2019-01-15 太仓萃励新能源科技有限公司 A kind of preparation method of nano-negative ion clear dope
CN111111645A (en) * 2019-12-27 2020-05-08 吉林大学 Enhanced LiTaO3Photocatalytic method

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Application publication date: 20140604