CN102134747A - Method for preparing cerium doped aluminum borate nanowire - Google Patents
Method for preparing cerium doped aluminum borate nanowire Download PDFInfo
- 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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- Prior art keywords
- cerium
- aluminum borate
- doped aluminum
- tube furnace
- nano wire
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- 239000002070 nanowire Substances 0.000 title claims abstract description 23
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 16
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 14
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 title abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 22
- 239000004411 aluminium Substances 0.000 claims description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims 1
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- 229920000742 Cotton Polymers 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010348 incorporation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000010671 solid-state reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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
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.
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110021901 CN102134747A (en) | 2011-01-18 | 2011-01-18 | Method for preparing cerium doped aluminum borate nanowire |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110021901 CN102134747A (en) | 2011-01-18 | 2011-01-18 | Method for preparing cerium doped aluminum borate nanowire |
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| Publication Number | Publication Date |
|---|---|
| CN102134747A true CN102134747A (en) | 2011-07-27 |
Family
ID=44294661
Family Applications (1)
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|---|---|---|---|
| CN 201110021901 Pending CN102134747A (en) | 2011-01-18 | 2011-01-18 | Method for preparing cerium doped aluminum borate nanowire |
Country Status (1)
| Country | Link |
|---|---|
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Cited By (3)
| 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)
| 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 | Rare earth Al2O3－B2O3Preparation of green luminescent material |
-
2011
- 2011-01-18 CN CN 201110021901 patent/CN102134747A/en active Pending
Patent Citations (1)
| 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 | Rare earth Al2O3－B2O3Preparation of green luminescent material |
Non-Patent Citations (2)
| 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)
| 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 |