CN101805007A - Preparation method of rare earth hydroxide nanorod - Google Patents
Preparation method of rare earth hydroxide nanorod Download PDFInfo
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- CN101805007A CN101805007A CN 201010136349 CN201010136349A CN101805007A CN 101805007 A CN101805007 A CN 101805007A CN 201010136349 CN201010136349 CN 201010136349 CN 201010136349 A CN201010136349 A CN 201010136349A CN 101805007 A CN101805007 A CN 101805007A
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Abstract
The invention relates to a preparation method of rare earth hydroxide nanorods, which belongs to the technical field of the inorganic nano material preparation process. The preparation method comprises the following steps carried out at room temperature: a, dissolving 0.006mol of cetyltrimethylammonium bromide into 40ml of deionized water to obtain CTAB solution with the concentration being 0.15M; b, placing 0.004mol of analytical pure chloride hexahydrate (LnCl3 . 6H2O) in a 100ml beaker, adding 10ml of deionized water, and magnetically mixing at a speed of 300r/m to obtain chloride solution with the concentration being 0.4M; c, dropping ammonia into the CTAB solution, and magnetically mixing at a speed of 300r/m to obtain mixed solution; dropping the prepared 10ml of LnCl3 solution into the mixed solution; and sealing the beaker; magnetically mixing for 2 hours at a speed of 300r/m and aging for 5 days at the room temperature; and d, washing sediments five times with distilled water to remove the CTAB and drying to obtain the rare earth hydroxide nanorods. The invention has the advantages of simple process, easy operation and low power consumption.
Description
Technical field:
The present invention relates to a kind of preparation method of rare earth hydroxide nanorod, belong to the inorganic nano material preparation process technology field.
Background technology:
Rare earth element has unique 4f electronic configuration, therefore has unique character such as electricity, optics and magnetics.Rare-earth hydroxide is a kind of compound in the high-tech area widespread use, mainly as raw material or additives such as electronic ceramics, laserable material, photoelectric material and glass-ceramic, also can be used as the thermo-stabilizer of PVC material etc.In addition, rare-earth hydroxide also is widely used in fields such as photoelectric device, phosphor material, transmitter, sorbing material, indicating meter, catalysis and bioprobe.
China is the first in the world rare earth big country, and rare-earth industry has become one of China's important chemical industry.Since carbon nanotube was found, the research to nano material had both at home and abroad become focus.When the size of material reaches Nano grade, the various character different with the body material appear through regular meeting, strengthen as catalytic effect enhancing, photoluminescence performance.Therefore, the preparation of novel rare-earth Nano material of hydrate and property research become the focus of broad research.
The domestic and international at present preparation method about the one dimension rare-earth hydroxide mainly contains traditional solvent-thermal method (B.TangNanotechnology, 2004,15,1273-1276.), hydrothermal method (Li Yadong etc., the method of synthesizing rare-earth oxyhydroxide or oxide nano thread and nano-powder thereof, Chinese invention patent, CN1403375A; The synthetic method of rare-earth hydroxide nanotube and serial rare-earth compound nano tube thereof, Chinese invention patent, CN1424257A; N.Zhang etc., MaterialsChemistry and Physics, 2009,114,160-167), hydro-thermal micro emulsion method (Y.D.Yin etc., Chinese ChemicalLetters, 2007,18,491-494.) and sol-gel method (I.Djer etc., Journal of Solid State Chemistry, 2007,180,2154-2165.).Occurred again afterwards the microwave promotion law (L.Ma etc., Materials Letters, 2007,61,1711-1714.) and template agent method (P.Bocchetta etc., Electrochemistry Communications, 2007,683-688.).Traditional hydrothermal method, solvent-thermal method, hydro-thermal-micro emulsion method, sol-gel method require High Temperature High Pressure (Teflon autoclave) condition, and new microwave promotion law requires microwave heating.These preparation method's costs are higher, and complex process.
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, and provide at ambient temperature a kind of, adopt the method for the cheap feedstock production rare earth hydroxide nanorod that is easy to get.
The preparation method's of rare earth hydroxide nanorod of the present invention whole process of preparation is carried out at ambient temperature, and concrete steps are as follows:
A. prepare the tensio-active agent settled solution: get the cetyl trimethylammonium bromide of 0.006mol, promptly analytical pure CTAB is dissolved in it fully and obtains transparent settled solution CTAB solution in the 40ml deionized water, and the CTAB strength of solution is 0.15M;
B. prepare rare earth chloride (LnCl
3) solution: get 0.004mol analytical pure six water muriate (LnCl
36H
2O) place the 100ml beaker, toward wherein adding 300 rev/mins of magnetic agitation of 10ml deionized water, be transparent settled solution until dissolving fully, the concentration of chloride soln is 0.4M;
C. in CTAB solution, drip wt% and be 25% ammoniacal liquor, and 300 rev/mins of magnetic agitation obtained uniform and transparent mixed solution after 30 minutes; 300 rev/mins of magnetic agitation then, and with the 10ml LnCl that configures
3Solution slowly is added drop-wise in the mixing solutions of CTAB and ammoniacal liquor; Beaker is sealed, continued in the room temperature ageing 5 days after 2 hours of 300 rev/mins of magnetic agitation;
D. after ageing finishes precipitation is filtered, removed CTAB 5 times with the distilled water centrifuge washing, obtain rare earth hydroxide nanorod more after drying.
Rare earth chloride of the present invention is that Lanthanum trichloride, samarium trichloride, Europium trichloride, chlorination roll, in the terbium chloride any.
The preparation method of rare earth hydroxide nanorod of the present invention, its chemical equation is:
Ln
3++3OH
-→Ln(OH)
3
Preparation method of the present invention compares with traditional technology, has whole process of preparation and carries out at ambient temperature; Technology is simple, and is easy to operate; Energy expenditure is low, can not introduce other pollutents in preparation process; The high advantage of rare-earth hydroxide purity that obtains.
Because rare-earth hydroxide has unique physical and chemical performances such as magnetics, electricity and optics, nanometer rod has special propertys such as anisotropy simultaneously, therefore is expected to have very vast market prospect and good prospects for application at display device, biomarker, optics and catalytic field.
Description of drawings:
Fig. 1 is lanthanum hydroxide nanometer rod X-ray powder diffraction figure.
Fig. 2 is lanthanum hydroxide nanometer rod transmission electron microscope figure.
Fig. 3 is samaric hydroxide nanometer rod X-ray powder diffraction figure.
Fig. 4 is samaric hydroxide nanometer rod transmission electron microscope figure.
Fig. 5 is europium hydroxide nanometer rod X-ray powder diffraction figure.
Fig. 6 is europium hydroxide nanometer rod transmission electron microscope figure.
Fig. 7 is gadolinium hydroxide nanometer rod X-ray powder diffraction figure.
Fig. 8 is gadolinium hydroxide nanometer rod transmission electron microscope figure.
Fig. 9 is terbium hydroxide nanometer rod X-ray powder diffraction figure.
Figure 10 is terbium hydroxide nanometer rod transmission electron microscope figure.
Embodiment:
Below be the example of the rare earth hydroxide nanorod that adopts the inventive method preparation, understand the present invention with further.
Embodiment 1:
1, takes by weighing 0.004mol analytical pure six water Lanthanum trichloride (LaCl
36H
2O) place the 100ml beaker, be the water white transparency settled solution until dissolving fully toward wherein adding the 10ml deionized water and stirring.Taking by weighing 0.006mol analytical pure CTAB is dissolved in it to obtain transparent settled solution in 40ml deionized water fully.
2, under 300 rev/mins of magnetic agitation conditions, in CTAB solution, drip 10ml (wt% is 25%) ammonia soln fast, stir and obtained even mixed solution in 30 minutes; 300 rev/mins of magnetic agitation then, and with the 10ml LaCl that configures
3Solution slowly is added drop-wise in the mixing solutions of CTAB and ammoniacal liquor; Beaker is sealed, continued 300 rev/mins of magnetic agitation 2 hours, afterwards ageing 5 days at ambient temperature.
3, after ageing finished, the elimination supernatant liquid carried out 5 centrifuge washings with distilled water to sample and removes CTAB, and at room temperature drying obtains white powder.Product is accredited as pure six side's phase lanthanum hydroxides through X-ray diffraction (Fig. 1); TEM Electronic Speculum (Fig. 2) testing product pattern: bar-shaped, length-to-diameter ratio is 15.
Embodiment 2:
1, takes by weighing 0.004mol analytical pure six water samarium trichloride (SmCl
36H
2O) place the 100ml beaker, be light yellow transparent settled solution until dissolving fully toward wherein adding the 10ml deionized water and stirring.Taking by weighing 0.006mol analytical pure CTAB is dissolved in it to obtain transparent settled solution in 40ml deionized water fully.
2, under 300 rev/mins of magnetic agitation conditions, in CTAB solution, drip 10ml (wt% is 25%) ammonia soln fast, stir and obtained even mixed solution in 30 minutes; 300 rev/mins of magnetic agitation then, and with the 10ml SmCl that configures
3Solution slowly is added drop-wise in the mixing solutions of CTAB and ammoniacal liquor; Beaker is sealed, continued 300 rev/mins of magnetic agitation 2 hours, afterwards ageing 5 days at ambient temperature.
3, after ageing finished, the elimination supernatant liquid carried out 5 centrifuge washings with distilled water to sample and removes CTAB, and at room temperature drying obtains buff powder.Product is accredited as pure six side's phase samaric hydroxides through X-ray diffraction (Fig. 3); TEM Electronic Speculum (Fig. 4) testing product pattern: bar-shaped, length-to-diameter ratio is 12.
Embodiment 3:
1, takes by weighing 0.004mol analytical pure six water Europium trichloride (EuCl
36H
2O) place the 100ml beaker, be the achromaticity and clarification clear solution until dissolving fully toward wherein adding the 10ml deionized water and stirring.Taking by weighing 0.006mol analytical pure CTAB is dissolved in it to obtain transparent settled solution in 40ml deionized water fully.
2, under 300 rev/mins of magnetic agitation conditions, in CTAB solution, drip 10ml (wt% is 25%) ammonia soln fast, stir and obtained even mixed solution in 30 minutes; 300 rev/mins of magnetic agitation then, and with the 10ml EuCl that configures
3Solution slowly is added drop-wise in the mixing solutions of CTAB and ammoniacal liquor; Beaker is sealed, continued 300 rev/mins of magnetic agitation 2 hours, afterwards ageing 5 days at ambient temperature.
3, after ageing finished, the elimination supernatant liquid carried out 5 centrifuge washings with distilled water to sample and removes CTAB, and at room temperature drying obtains white powder.Product is accredited as pure six side's phase europium hydroxides through X-ray diffraction (Fig. 5); TEM Electronic Speculum (Fig. 6) testing product pattern: bar-shaped, length-to-diameter ratio is 13.
Embodiment 4:
1, takes by weighing 0.004mol analytical pure six water Gadolinium trichloride (GdCl
36H
2O) place the 100ml beaker, be the achromaticity and clarification clear solution until dissolving fully toward wherein adding the 10ml deionized water and stirring.Taking by weighing 0.006mol analytical pure CTAB is dissolved in it to obtain transparent settled solution in 40ml deionized water fully.
2, under 300 rev/mins of magnetic agitation conditions, in CTAB solution, drip 10ml (wt% is 25%) ammonia soln fast, stir and obtained even mixed solution in 30 minutes; 300 rev/mins of magnetic agitation then, and with the 10ml GdCl that configures
3Solution slowly is added drop-wise in the mixing solutions of CTAB and ammoniacal liquor; Beaker is sealed, continued 300 rev/mins of magnetic agitation 2 hours, afterwards ageing 5 days at ambient temperature.
3, after ageing finished, the elimination supernatant liquid carried out 5 centrifuge washings with distilled water to sample and removes CTAB, and at room temperature drying obtains white powder.Product is accredited as pure six side's phase gadolinium hydroxides through X-ray diffraction (Fig. 7); TEM Electronic Speculum (Fig. 8) testing product pattern: bar-shaped, length-to-diameter ratio is 25.
Embodiment 5:
1, takes by weighing 0.004mol analytical pure six water terbium chloride (TbCl
36H
2O) place the 100ml beaker, be the achromaticity and clarification clear solution until dissolving fully toward wherein adding the 10ml deionized water and stirring.Taking by weighing 0.006mol analytical pure CTAB is dissolved in it to obtain transparent settled solution in 40ml deionized water fully.
2, under 300 rev/mins of magnetic agitation conditions, in CTAB solution, drip 10ml (wt% is 25%) ammonia soln fast, stir and obtained even mixed solution in 30 minutes; 300 rev/mins of magnetic agitation then, and with the 10ml TbCl that configures
3Solution slowly is added drop-wise in the mixing solutions of CTAB and ammoniacal liquor; Beaker is sealed, continued 300 rev/mins of magnetic agitation 2 hours, afterwards ageing 5 days at ambient temperature.
3, after ageing finished, the elimination supernatant liquid carried out 5 centrifuge washings with distilled water to sample and removes CTAB, and at room temperature drying obtains white powder.Product is accredited as pure six side's phase terbium hydroxides through X-ray diffraction (Fig. 9); TEM Electronic Speculum (Figure 10) testing product pattern: bar-shaped, length-to-diameter ratio is 20.
Claims (2)
1. the preparation method of a rare earth hydroxide nanorod is characterized in that whole process of preparation carries out at ambient temperature as follows:
A. prepare the tensio-active agent settled solution: get the cetyl trimethylammonium bromide of 0.006mol, promptly analytical pure CTAB is dissolved in it fully and obtains transparent settled solution CTAB solution in the 40ml deionized water, and the CTAB strength of solution is 0.15M;
B. prepare rare earth chloride (LnCl
3) solution: get 0.004mol analytical pure six water muriate (LnCl
36H
2O) place the 100ml beaker, toward wherein adding 300 rev/mins of magnetic agitation of 10ml deionized water, be transparent settled solution until dissolving fully, the concentration of chloride soln is 0.4M;
C. in CTAB solution, drip wt% and be 25% ammoniacal liquor, and 300 rev/mins of magnetic agitation obtained uniform and transparent mixed solution after 30 minutes; 300 rev/mins of magnetic agitation then, and with the 10ml LnCl that configures
3Solution slowly is added drop-wise in the mixing solutions of CTAB and ammoniacal liquor; Beaker is sealed, continued in the room temperature ageing 5 days after 2 hours of 300 rev/mins of magnetic agitation;
D. after ageing finishes precipitation is filtered, removed CTAB 5 times with the distilled water centrifuge washing, obtain rare earth hydroxide nanorod more after drying.
2. by the preparation method of the described rare earth hydroxide nanorod of claim 1, it is characterized in that described rare earth chloride is that Lanthanum trichloride, samarium trichloride, Europium trichloride, chlorination roll, in the terbium chloride any.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115146A (en) * | 2011-01-06 | 2011-07-06 | 云南大学 | Nano-structured cerium oxide with and application thereof |
| CN116409808A (en) * | 2022-01-05 | 2023-07-11 | 上海市地江建筑科技有限公司 | Samarium hydroxide nanorod-based hydrophobic film and preparation process thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403375A (en) * | 2002-10-11 | 2003-03-19 | 清华大学 | Synthesis process of nanostring and nanopowder of RE hydroxide or oxide |
| CN101234750A (en) * | 2008-02-28 | 2008-08-06 | 廖春生 | Method of preparing superfine micro-particle and nano granule |
| CN101407330A (en) * | 2008-10-30 | 2009-04-15 | 上海大学 | Method of preparing cerium oxide nano-rod |
-
2010
- 2010-03-31 CN CN 201010136349 patent/CN101805007A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403375A (en) * | 2002-10-11 | 2003-03-19 | 清华大学 | Synthesis process of nanostring and nanopowder of RE hydroxide or oxide |
| CN101234750A (en) * | 2008-02-28 | 2008-08-06 | 廖春生 | Method of preparing superfine micro-particle and nano granule |
| CN101407330A (en) * | 2008-10-30 | 2009-04-15 | 上海大学 | Method of preparing cerium oxide nano-rod |
Non-Patent Citations (1)
| Title |
|---|
| 《Nanotechnology》 20090804 Qiuying Mu et al. Synthesis, characterization and photoluminescence of lanthanum hydroxide nanorods by a simple route at room temperature 第2页 1，2 第20卷, 第34期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115146A (en) * | 2011-01-06 | 2011-07-06 | 云南大学 | Nano-structured cerium oxide with and application thereof |
| CN116409808A (en) * | 2022-01-05 | 2023-07-11 | 上海市地江建筑科技有限公司 | Samarium hydroxide nanorod-based hydrophobic film and preparation process thereof |
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Open date: 20100818 |