CN1872696A - Method for preparing Nano tube of lanthanum hydroxide, and Nano tube of lanthanum oxide - Google Patents
Method for preparing Nano tube of lanthanum hydroxide, and Nano tube of lanthanum oxide Download PDFInfo
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- CN1872696A CN1872696A CN 200610019327 CN200610019327A CN1872696A CN 1872696 A CN1872696 A CN 1872696A CN 200610019327 CN200610019327 CN 200610019327 CN 200610019327 A CN200610019327 A CN 200610019327A CN 1872696 A CN1872696 A CN 1872696A
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Abstract
This invention relates to a method for preparing lanthanum hydroxide and lanthanum oxide nanotubes. The method comprises: (1) mixing 0.1-2 mol of water-soluble lanthanum salt and 1-20 mol of urea, and dissolving into water; (2) reacting at 50-120 deg.C for 0.1-168 h, cooling to room temperature, and filtering to obtain the precipitate; (3) washing with deionized water, and drying at 80-90 deg.C to obtain white powder of lanthanum hydroxide nanotubes; (4) calcining the lanthanum hydroxide nanotubes at 200-900 deg.C for 0.5-8 h, and cooling to room temperature to obtain lanthanum oxide nanotubes. The method has such advantages of simple process and high suitability for industrial production. The lanthanum hydroxide and lanthanum oxide nanotubes have potential applications in such fields as semiconductors, displays, high performance ceramics and catalysts.
Description
Technical field
The present invention relates to the preparation method of lanthanum hydroxide nanotube and lanthanum trioxide nanotube, belong to the inorganic material preparation process technical field.
Background technology
Rare earth compound is many requisite integral parts with functional materials of excellent magnetic, optical property in aspect extensive application such as optical material, electronic material, magneticsubstance, catalysis, high-performance ceramic, medicine.Because China is the first in the world rare earth big country, having verified industrial store content is the first in the world, and rare-earth industry has become one of China's important chemical industry.Over past ten years, it is found that, after the size of material reaches nano level, the character different occurs through regular meeting, as the enhancing of photoluminescent property with body phase material.Therefore the synthetic and property research of novel rare-earth compound nano-material becomes the focus of broad research.
Domestic and international research concentrates on the preparation (Y.Hasegaw etc. of oxide nano particles at present, Angew.Chem.Int.Ed.2002,41,2073.), preparation (the Y.D.Li etc. that the sulphur rare earth oxide is nanocrystalline, Inorg.Chem., 2000,39,3418.), and the part rare earth oxide, hydroxide nano pipe (Adv.Funct.Mater.2003 such as Y.-P.Fang, 13 (12), 955-960.) etc. the research of aspect, but the rare earth nano tube preparation method of having reported is less, and its preparation method is mainly the legal (Li Yadong etc. of hydro-thermal, patent of invention publication number CN 1424257A) or adopt the technology (M.Yada etc. of tensio-active agent as soft template aid preparation rare-earth oxide nano, Adv.Mater.2002,14,309.).
And the rarely found report of research of lanthanum hydroxide nanotube and lanthanum trioxide nanotube.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of lanthanum hydroxide nanotube and lanthanum trioxide nanotube, wherein the preparation of lanthanum trioxide nanotube depends on the preparation of lanthanum hydroxide nanotube.
Technical scheme of the present invention is:
Water-soluble salt with Rare Earth Lanthanum is a raw material, under normal pressure, prepares the hydroxide nano pipe by chemical coprecipitation.Roasting obtains rare-earth oxide nano under proper temperature.
The preparation method of lanthanum hydroxide nanotube comprises the steps:
With the mole proportioning is the water-soluble salt 0.1-2 mole of Rare Earth Lanthanum, and urea 1-20 mole mixes soluble in water; Above-mentioned solution was reacted 0.1-168 hour under 50 ℃ of-120 ℃ of following conditions, be cooled to room temperature then, filter the precipitation obtain, deionized water wash, 80-90 ℃ of oven dry obtains the lanthanum hydroxide nanotube of white powder state.
In order to obtain more tiny lanthanum hydroxide nanotube, can increase the microwave treatment step.The reaction times of microwave treatment is also shorter, can obtain the lanthanum hydroxide nanotube faster.Specific as follows:
With the mole proportioning is the water-soluble salt 0.1-2 mole of Rare Earth Lanthanum, and urea 1-20 mole mixes soluble in water; At 50 ℃-120 ℃, the microwave heating reaction is 0.1-3 hour under the microwave frequency 1000-1200MHz condition with above-mentioned solution; Be cooled to room temperature then, filter the precipitation obtain, deionized water wash, 80-90 ℃ of oven dry obtains the lanthanum hydroxide nanotube of white powder state.
The preparation method of lanthanum trioxide nanotube comprises the steps:
With the mole proportioning is the water-soluble salt 0.1-2 mole of Rare Earth Lanthanum, and urea 1-20 mole mixes soluble in water; Above-mentioned solution was reacted 0.1-168 hour under 50 ℃ of-120 ℃ of following conditions, be cooled to room temperature then, the precipitation that filtration obtains, deionized water wash, 80-90 ℃ of oven dry obtains the lanthanum hydroxide nanotube of white powder state, with the lanthanum hydroxide nanotube 200-900 ℃ of roasting, 0.5-8 be chilled to room temperature after hour, promptly make the lanthanum trioxide nanotube.
The invention has the advantages that: the present invention adds hot preparation lanthanum hydroxide and lanthanum trioxide nanotube under normal pressure, have the advantages that technology is simple, be easy to realize suitability for industrialized production, lanthanum hydroxide nanotube and lanthanum trioxide nanotube will have good prospects for application in fields such as semiconductor element, display device, high-performance ceramic, catalysis.
Embodiment
Embodiment 1:
Taking by weighing 2 molar nitric acid lanthanums and 1.4 mole of urea respectively mixes and is dissolved in the 1600ml deionized water, under the normal pressure, above-mentioned solution is heated to 80 ℃ in flask, isothermal reaction 6 hours, be cooled to room temperature then, filter the precipitation that obtains, deionized water wash, 80 ℃ of oven dry obtain the lanthanum hydroxide nanotube of white powder state.Detect through the TEM Electronic Speculum, product is about 15 nanometers of internal diameter, about 60 nanometers of external diameter, the about 5 microns lanthanum hydroxide nanotube of length.
Embodiment 2:
Take by weighing 2 molar nitric acid lanthanums and 1.4 mole of urea respectively and mix, the reacting by heating temperature is controlled at 95 ℃, in 12 hours reaction times, can obtain about 20 nanometers of internal diameter, about 80 nanometers of external diameter, the about 3 microns lanthanum hydroxide nanotube of length.All the other are with embodiment 1.
Embodiment 3:
Take by weighing 0.1 molar nitric acid lanthanum and 1 mole of urea respectively and mix and be dissolved in the 600ml deionized water, the reacting by heating temperature is controlled at 50 ℃, in 0.1 hour reaction times, obtain the lanthanum hydroxide nanotube.All the other are with embodiment 1.
Embodiment 4:
Take by weighing 2 molar nitric acid lanthanums and 20 mole of urea respectively and mix and be dissolved in the 10000ml deionized water, the reacting by heating temperature is controlled at 120 ℃, in 168 hours reaction times, obtain the lanthanum hydroxide nanotube.All the other are with embodiment 1.
Embodiment 5:
Take by weighing 0.9 molar nitric acid lanthanum and 3.6 mole of urea respectively and mix, the reacting by heating temperature is controlled at 70 ℃, in 15 hours reaction times, obtain the lanthanum hydroxide nanotube.All the other are with embodiment 1.
Embodiment 6:
Lanthanum hydroxide nanotube with embodiment 1 gained is a raw material, and 450 ℃ of calcinations are 4 hours in retort furnace, obtains the lanthanum trioxide nanotube of about 30 nanometers of internal diameter, about 50 nanometers of external diameter, about 400 nanometers of length.
Embodiment 7:
Lanthanum hydroxide nanotube with embodiment 2 gained is a raw material, and 200 ℃ of calcinations are 8 hours in retort furnace, obtains the lanthanum trioxide nanotube of about 45 nanometers of internal diameter, about 75 nanometers of external diameter, about 600 nanometers of length.
Embodiment 8:
Lanthanum hydroxide nanotube with embodiment 3 gained is a raw material, and 900 ℃ of calcinations are 0.5 hour in retort furnace, obtains the lanthanum trioxide nanotube of about 30 nanometers of internal diameter, about 60 nanometers of external diameter, about 500 nanometers of length.
Embodiment 9:
Take by weighing 2 molar nitric acid lanthanums and 1.4 mole of urea respectively and mix and be dissolved in the 1600ml deionized water, under the normal pressure, at 80 ℃, the microwave heating reaction is 1 hour under the microwave frequency 1100MHz condition with above-mentioned solution; The precipitation that filtration obtains, deionized water wash, 80 ℃ of oven dry obtain the lanthanum hydroxide nanotube of white powder state.Detect through the TEM Electronic Speculum, product is about 8 nanometers of internal diameter, about 40 nanometers of external diameter, the about 4 microns lanthanum hydroxide nanotube of length.
Embodiment 10:
Take by weighing 0.5 molar nitric acid lanthanum and 2.4 mole of urea respectively and mix and be dissolved in the 3000ml deionized water, under the normal pressure, at 50 ℃, the microwave heating reaction is 0,2 hour under the microwave frequency 1200MHz condition with above-mentioned solution; The precipitation that filtration obtains, deionized water wash, 85 ℃ of oven dry obtain the lanthanum hydroxide nanotube of white powder state.Detect through the TEM Electronic Speculum, product is about 10 nanometers of internal diameter, about 35 nanometers of external diameter, the about 8 microns lanthanum hydroxide nanotube of length.
Embodiment 11:
Take by weighing 0.1 molar nitric acid lanthanum and 1 mole of urea respectively and mix and be dissolved in the 800ml deionized water, under the normal pressure, at 120 ℃, the microwave heating reaction is 3 hours under the microwave frequency 1000MHz condition with above-mentioned solution; The precipitation that filtration obtains, deionized water wash, 90 ℃ of oven dry obtain the lanthanum hydroxide nanotube of white powder state.
Embodiment 12:
Replace lanthanum nitrate with Lanthanum trichloride, all the other repeat above all embodiment respectively.
The water-soluble salt of Rare Earth Lanthanum mainly contains Lanthanum trichloride and lanthanum nitrate.Lanthanum trichloride and lanthanum nitrate can be summarized the water-soluble salt of Rare Earth Lanthanum.
Claims (3)
1, the preparation method of lanthanum hydroxide nanotube, it is characterized in that comprising the steps: with the mole proportioning is the water-soluble salt 0.1-2 mole of Rare Earth Lanthanum, urea 1-20 mole mixes soluble in water; Above-mentioned solution was reacted 0.1-168 hour under 50 ℃ of-120 ℃ of following conditions, be cooled to room temperature then, filter the precipitation obtain, deionized water wash, 80-90 ℃ of oven dry obtains the lanthanum hydroxide nanotube of white powder state.
2, the preparation method of lanthanum hydroxide nanotube, it is characterized in that comprising the steps: with the mole proportioning is the water-soluble salt 0.1-2 mole of Rare Earth Lanthanum, urea 1-20 mole mixes soluble in water; At 50 ℃-120 ℃, the microwave heating reaction is 0.1-3 hour under the microwave frequency 1000-1200MHz condition with above-mentioned solution; Be cooled to room temperature then, filter the precipitation obtain, deionized water wash, 80-90 ℃ of oven dry obtains the lanthanum hydroxide nanotube of white powder state.
3, the preparation method of lanthanum trioxide nanotube, it is characterized in that comprising the steps: with the mole proportioning is the water-soluble salt 0.1-2 mole of Rare Earth Lanthanum, urea 1-20 mole mixes soluble in water; Above-mentioned solution was reacted 0.1-168 hour under 50 ℃ of-120 ℃ of following conditions, be cooled to room temperature then, the precipitation that filtration obtains, deionized water wash, 80-90 ℃ of oven dry obtains the lanthanum hydroxide nanotube of white powder state, with the lanthanum hydroxide nanotube 200-900 ℃ of roasting, 0.5-8 be chilled to room temperature after hour, promptly make the lanthanum trioxide nanotube.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279767B (en) * | 2008-04-28 | 2010-06-16 | 哈尔滨工业大学 | Preparation of lanthanide series rare-earth doped bismuth titanate nano-tube |
| CN101787574A (en) * | 2010-03-04 | 2010-07-28 | 长春理工大学 | Method for preparing lanthanum hydroxide porous hollow nano-fiber and chain-like nano-fiber |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002187717A (en) * | 2000-10-04 | 2002-07-05 | Tosoh Corp | Rare earth element compound, rare earth element oxide, phosphor and method for manufacturing them |
| CN1216803C (en) * | 2003-01-10 | 2005-08-31 | 清华大学 | Rare earth hydroxide nano tubes and synthesis of serial rare earth compounds nano tubes |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279767B (en) * | 2008-04-28 | 2010-06-16 | 哈尔滨工业大学 | Preparation of lanthanide series rare-earth doped bismuth titanate nano-tube |
| CN101787574A (en) * | 2010-03-04 | 2010-07-28 | 长春理工大学 | Method for preparing lanthanum hydroxide porous hollow nano-fiber and chain-like nano-fiber |
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