CN102134747A - Method for preparing cerium doped aluminum borate nanowire - Google Patents

Method for preparing cerium doped aluminum borate nanowire Download PDF

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Publication number
CN102134747A
CN102134747A CN 201110021901 CN201110021901A CN102134747A CN 102134747 A CN102134747 A CN 102134747A CN 201110021901 CN201110021901 CN 201110021901 CN 201110021901 A CN201110021901 A CN 201110021901A CN 102134747 A CN102134747 A CN 102134747A
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China
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cerium
aluminum borate
doped aluminum
tube furnace
nano wire
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Chinese (zh)
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李培刚
王顺利
朱晖文
唐为华
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Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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Zhejiang Sci Tech University ZSTU
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Publication of CN102134747A publication Critical patent/CN102134747A/en
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Abstract

The invention discloses a method for preparing inorganic material metal cerium (Ce) doped aluminum borate (Al18B4O33), in particular to a method for preparing a cerium doped aluminum borate nanowire. The method comprises the following steps of: mixing fumed aluminum oxide (fumed Al2O3), diboron trioxide (B2O3) and cerium dioxide (CeO2); then, heating a tube furnace to 1100-1400 DEG C, maintaining the temperature for 2-5 h, and cooling to room temperature. The obtained product is the cerium doped aluminum borate (Al18B4O33) nanowire. The invention has the advantages that all reagents used in the preparation process are commercial products, complex preparation is not needed, the entire process is simple and easy to operate, the cost is low, and the prepared product has high purity and can be produced on a large scale.

Description

A kind of method for preparing the borate doped aluminium nano wire of cerium
Technical field
The present invention relates to the borate doped aluminium (Al of inorganic materials metallic cerium (Ce) 18B 4O 33) the preparation method of the borate doped aluminium nano wire of preparation method, especially cerium.
Background technology
Aluminum borate (Al 18B 4O 33) nano wire is because of having very high specific surface area, high strength, Young's modulus greatly, good thermostability and extremely strong performance such as anti-oxidant, at ceramic composite, high strength friction materials and photoelectron material are with a wide range of applications.And the adulterated aluminum borate nano wire of rare earth metal is a kind of optical material efficiently.The method that is used to prepare the adulterated aluminum borate nano wire of rare earth metal up to now mainly is elevated temperature heat reaction method (1100~1300 ℃).But utilize this elevated temperature heat reaction method can only prepare the adulterated aluminum borate nano wire of rare earth metal europium (Eu), can not prepare the adulterated aluminum borate nano wire of other rare earth metals.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, the method for preparing the borate doped aluminium nano wire of cerium that cost is low.The method for preparing the borate doped aluminium nano wire of cerium of the present invention adopts synthesis by solid state reaction, and step is as follows:
Earlier with gaseous oxidation aluminium (fumed Al 2O 3), boron trioxide (B 2O 3) and cerium dioxide (CeO 2) mix, place the tube furnace mid-way, wherein Al 2O 3And B 2O 3Mol ratio be 9: 2, CeO 2And Al 2O 3Mol ratio be 0~0.05.Tube furnace is heated to 1100~1400 ℃ then, and after being incubated 2-5 hour, is cooled to room temperature, products therefrom is the borate doped aluminium (Al of cerium 18B 4O 33) nano wire; 9: 2 proportioning among the present invention is the portfolio ratio with good result that draws after long-term, a large amount of experiment of contriver's process.
In the preparation process of the present invention, preferred temperature of reaction is 1150~1300 ℃, because tube furnace has the advantage on the in-house facility such as good sealing effect, so adopt tube furnace in the present invention, both can realize the good technical effect, can save economic spending again.
Among the present invention, the reactant aluminum oxide must be a gaseous oxidation aluminium, can not use the aluminum oxide of other thing phases.Need not add inert atmosphere protection in the reaction process, final products therefrom is high-purity borate doped aluminium nano wire of cerium, need not wash products.
Beneficial effect: in the preparation process of the present invention, agents useful for same is commerical prod, need not loaded down with trivial details preparation.In the preparation process of the present invention, can utilize to grind reactant is mixed.The present invention adopts synthesis by solid state reaction to prepare the borate doped aluminium nano wire of cerium, and technology is simple to operation, and cost is low, and the product purity height that makes can be mass-produced.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) photo of the borate doped aluminium nano wire of Ce that makes with the inventive method;
Fig. 2 is X-ray diffraction (XRD) spectrogram of the borate doped aluminium nano wire of Ce that makes with the inventive method;
Fig. 3 is transmission electron microscope power spectrum (TEM-EDX) spectrogram of the borate doped aluminium nano wire of single Ce that makes with the inventive method.
Embodiment
Further specify the present invention below in conjunction with example.
Embodiment 1
Earlier with 0.09mol gas phase Al 2O 3, 0.02mol B 2O 3, 0.0045mol CeO 2, be positioned over tubular react furnace central authorities after ground and mixed is even.Reaktionsofen is warmed up to 1250 ℃ then, and after being incubated 3 hours, is cooled to room temperature.Final product is the cotton-shaped powder of white cotton.Directly under scanning electron microscope, observe, can find that the wire product of a large amount of nano-scales generates as Fig. 1.The mean length of these nano wires is about 5 microns, and mean diameter is about 120 nanometers.The XRD diffraction spectrogram of Fig. 2 confirms that product is the aluminum borate (Al of pure rhombic system 18B 4O 33), do not find the diffraction peak of other products.Because the doping of Ce seldom, mixing of Ce element can not influence the crystalline structure of aluminum borate, so the XRD figure of gained spectrum conforms to the aluminum borate standard diffraction card (32-0003) of reference.The TEM-EDX analysis revealed single nano-wire product of Fig. 3 is by Al, O, and Ce is elementary composition.Wherein the atomic ratio of Al and O is 1: 1.81, with the Al of standard 18B 4O 33In Al and the atomic ratio of O approaching.The atomic ratio of Ce and Al is 1: 40.Wherein the C element derives from and does the used conductive carbon film of TEM-EDX analysis, and is irrelevant with sample composition.The B element is a light element, can't be detected by the TEM-EDX power spectrum.In conjunction with Fig. 1, Fig. 2 and Fig. 3, this product are defined as the adulterated aluminum borate nano wire of Ce.
Embodiment 2
With 0.09mol gas phase Al 2O 3, 0.02mol B 2O 3, 0.003mol CeO 2, be positioned over tubular react furnace central authorities after ground and mixed is even.Reaktionsofen is warmed up to 1150 ℃ then, and after being incubated 4 hours, is cooled to room temperature.Final product is the cotton-shaped powder of white cotton.The pattern of product is identical with embodiment 1 with structure.Unique different be that the incorporation of Ce element has reduced.The atomic ratio of Ce and Al is 1: 60.
Embodiment 3
With 0.09mol gas phase Al 2O 3, 0.02mol B 2O 3, 0.002mol CeO 2, be positioned over tubular react furnace central authorities after ground and mixed is even.Reaktionsofen is warmed up to 1300 ℃ then, and after being incubated 3 hours, is cooled to room temperature.Final product is the cotton-shaped powder of white cotton.The pattern of product is identical with embodiment 1 with structure.Unique different be that the incorporation of Ce element has reduced.The atomic ratio of Ce and Al is 1: 90.
Embodiment 4
With 0.09mol gas phase Al 2O 3, 0.02mol B 2O 3, 0.001mol CeO 2, be positioned over tubular react furnace central authorities after ground and mixed is even.Reaktionsofen is warmed up to 1300 ℃ then, and after being incubated 3 hours, is cooled to room temperature.Final product is the cotton-shaped powder of white cotton.The pattern of product is identical with embodiment 1 with structure.Unique different be that the incorporation of Ce element has reduced.The atomic ratio of Ce and Al is 1: 180.

Claims (3)

1. a method for preparing the borate doped aluminium nano wire of cerium is characterized in that comprising the steps:
Gaseous oxidation aluminium, boron trioxide and cerium dioxide mixing are placed on the tube furnace mid-way, wherein the mol ratio of aluminum oxide and boron trioxide is 9: 2, the mol ratio of cerium dioxide and aluminum oxide is 0~0.05: 1, tube furnace is heated to 1100~1400 ℃ then, be incubated after 2-5 hour, be cooled to room temperature, products therefrom is the borate doped aluminium nano wire of cerium.
2. preparation method according to claim 1 is characterized in that described tube furnace is heated to 1150~1300 ℃.
3. preparation method according to claim 1 is characterized in that soaking time is 3~4 hours in the described tube furnace.
CN 201110021901 2011-01-18 2011-01-18 Method for preparing cerium doped aluminum borate nanowire Pending CN102134747A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103541010A (en) * 2013-10-23 2014-01-29 北京邮电大学 Erbium-doped aluminum borate nanowire and preparation method thereof
CN104498028A (en) * 2014-12-11 2015-04-08 陕西师范大学 Al5BO9:Eu<3+> luminescent material and preparation method thereof
CN104788504A (en) * 2015-03-09 2015-07-22 陈谦 Component controllable cobalt doped metal-organic framework DMMnF monocrystalline material and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1180095A (en) * 1994-12-06 1998-04-29 中国科学院长春应用化学研究所 Preparation of rare earth Al203-B203 green luminescent material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1180095A (en) * 1994-12-06 1998-04-29 中国科学院长春应用化学研究所 Preparation of rare earth Al203-B203 green luminescent material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《APPLIED PHYSICS LETTERS》 20060720 J.Lin等 Characterization and photoluminescence properties of aluminum borate nanorods doped with Eu 033118 第89卷, *
《昆明理工大学学报》 20020630 冷崇燕等 固相反应法制备Al18B4O33:Eu3+红色荧光粉 123-125,129 第27卷, 第3期 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103541010A (en) * 2013-10-23 2014-01-29 北京邮电大学 Erbium-doped aluminum borate nanowire and preparation method thereof
CN103541010B (en) * 2013-10-23 2016-04-13 北京邮电大学 A kind of method of Er ions aluminum borate nanowire and preparation thereof
CN104498028A (en) * 2014-12-11 2015-04-08 陕西师范大学 Al5BO9:Eu<3+> luminescent material and preparation method thereof
CN104788504A (en) * 2015-03-09 2015-07-22 陈谦 Component controllable cobalt doped metal-organic framework DMMnF monocrystalline material and preparation method thereof
CN104788504B (en) * 2015-03-09 2017-09-01 陈谦 A kind of controllable cobalt doped metal organic frame DMMnF monocrystal materials of composition and preparation method thereof

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Application publication date: 20110727