CN1256276C - Process for preparing aluminium boroxide nano thread - Google Patents
Process for preparing aluminium boroxide nano thread Download PDFInfo
- Publication number
- CN1256276C CN1256276C CN 200410016494 CN200410016494A CN1256276C CN 1256276 C CN1256276 C CN 1256276C CN 200410016494 CN200410016494 CN 200410016494 CN 200410016494 A CN200410016494 A CN 200410016494A CN 1256276 C CN1256276 C CN 1256276C
- Authority
- CN
- China
- Prior art keywords
- citric acid
- boric acid
- analytically pure
- aluminum nitrate
- nano wire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910052782 aluminium Inorganic materials 0.000 title claims description 20
- 239000004411 aluminium Substances 0.000 title claims description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 18
- 238000004519 manufacturing process Methods 0.000 title abstract 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 45
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004327 boric acid Substances 0.000 claims abstract description 16
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000002070 nanowire Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 9
- 239000012467 final product Substances 0.000 claims description 4
- 235000012054 meals Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 238000003980 solgel method Methods 0.000 abstract description 3
- -1 aluminum boron oxygen Chemical compound 0.000 abstract 3
- 230000002349 favourable effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 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 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 230000002950 deficient Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Catalysts (AREA)
Abstract
The present invention discloses an aluminum boron oxygen nanometer wire which comprises Al4B2O9 and Al18B4O33. A sol-gel method is adopted and comprises the steps that firstly, 99% of analytically pure aluminum nitrate, boric acid and citric acid are prepared into solution according to the mole ratio: aluminum nitrate: boric acid: citric acid==1:1:1 to 1:10:10, and the solution is dried at 10 to 500 DEG C to obtain gel products; secondly, the gel products are calcined at 100 to 1000 DEG C for 5 minutes to 200 hours to generate white powder, and the Al4B2O9 nanometer wires are obtained, or the gel products are calcined at 1000 to 2000 DEG C for 5 minutes to generate white powder, and the Al18B4O33 nanometer wires are obtained; the obtained nanometer wires are dissolved in water, and then, soluble B2O3 impurities are centrifugally removed. The aluminum boron oxygen nanometer wire of the present invention has the advantages of simple technology, easy mass production and favorable performance. If the prepared aluminum boron oxygen nanometer wire is organically combined with other block material, the toughness and the strength of ceramic material are possible to enhance.
Description
Technical field
The present invention relates to the preparation method of aluminium boroxide nano thread.
Background technology
Because monodimension nanometer material has character such as unique mechanical, electricity, optics, magnetics, so exist the wide industrial application prospect, becomes a focus of recent investigation of materials.The 1-dimention nano silk has the mechanical property of many uniquenesses, has caused great concern.Compare with the body material, whisker is because the defective of unit length is few, so engineering properties strengthens greatly.Compare with whisker, the mechanical properties of monodimension nanometer material also increases substantially.The mechanical property of the whisker that increases the material SiC that threads commonly used does not reach theoretical value far away.
Aluminium boroxide (Al
4B
2O
9, Al
18B
4O
33) be ceramic material preferably.The aluminium boroxide whisker has similar Young's modulus, tensile strength and thermal expansivity with the SiC whisker.The method of synthetic aluminium boroxide nano wire is generally thermal evaporation (Al
2O
3And B
2O
3Evaporate after mixing), or catalyst method.But these methods have a lot of shortcomings, and are less as the amount that thermal evaporation is produced, and need the equipment complexity, and the impurity that catalyst method is produced is more, is difficult for removing.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, prepares in a large number aluminium boroxide (Al
4B
2O
9, Al
18B
4O
33) method of nano wire.
The aluminium boroxide nano thread of the present invention's preparation comprises A
L4B
2O
9And Al
18B
4O
33Two kinds, employing be sol-gel processing.
Preparation Al
4B
2O
9The method of aluminium boroxide nano wire, it may further comprise the steps:
1) with 99% analytically pure aluminum nitrate, 99% analytically pure boric acid and 99% analytically pure citric acid, aluminum nitrate in molar ratio: boric acid: the ratio wiring solution-forming of citric acid=1: 1: 1～1: 10: 10 10 ℃～150 ℃ oven dry down, obtains the gel product;
2) with the gel product 750 ℃～1000 ℃ roastings 4 hours to 200 hours, generate the powder of white, get A1
4B
2O
9Nano wire;
3) with Al obtained above
4B
2O
9Nano wire is water-soluble, centrifugally removes soluble B
2O
3Impurity gets final product.
Preparation Al
18B
4O
33The method of aluminium boroxide nano thread, it may further comprise the steps:
1) with 99% analytically pure aluminum nitrate, 99% analytically pure boric acid and 99% analytically pure citric acid, aluminum nitrate in molar ratio: boric acid: the ratio wiring solution-forming of citric acid=1: 1: 1～1: 10: 10 10 ℃～150 ℃ oven dry down, obtains the gel product;
2) with the gel product 1050 ℃～2000 ℃ following roastings 4 hours to 200 hours, generate the meal of white, Al
18B
4O
33Nano thread;
3) with Al obtained above
18B
4O
33Nano wire is water-soluble, centrifugally removes soluble B
2O
3Impurity gets final product.
The present invention can be used for controlling the diameter of nano wire by changing the ratio of magnesium nitrate, boric acid, citric acid, and such as the increase along with the boric acid amount, the diameter of nano wire will increase.
The inventive method technology is simple, easily forms and produces the aluminium boroxide nano wire (Al that makes in enormous quantities
4B
2O
9, Al
18B
4O
33) function admirable, aluminium boroxide nano wire and other block materials that makes combined, be expected to strengthen toughness and the intensity of ceramic material.
Description of drawings
Fig. 1 is the Al that the present invention makes
4B
2O
9Nano wire dissolves the XRD figure behind the impurity;
Fig. 2 is the Al that dissolves impurity
4B
2O
9The TEM figure of nano wire, the upper right corner is electron diffraction diagram;
Fig. 3 is the Al that the present invention makes
18B
4O
33XRD figure behind the molten decon of nano thread;
Fig. 4 is the Al of molten decon
18B
4O
33The TEM figure of nano thread, the upper right corner is its electron-diffraction diagram.
Embodiment
Embodiment 1:
With aluminum nitrate (Al (NO
3)
3Analyze pure 99%), boric acid (H
3BO
3Analyze pure 99%) and citric acid (C
6H
8O
7H
2O analyzes pure 99%) aluminum nitrate in molar ratio: boric acid: citric acid=1: 4: 5 wiring solution-forming, make gel 150 ℃ of lower oven dry; 750 ℃ of lower roastings 4 hours, generate the powder of white then; White powder is water-soluble, centrifugally remove soluble B
2O
3Impurity gets aluminium boroxide (Al
4B
2O
9) nano wire.
To dissolve B
2O
3Aluminium boroxide (Al
4B
2O
9) nano wire detects with XRD, the results are shown in Figure 1, diffraction maximum is sharp-pointed, and the nano wire well-crystallized is described; Use transmission electron microscope observing, the results are shown in Figure 2, show the aluminium boroxide (Al that generates with sol-gal process
4B
2O
9) the nano wire diameter is more even, substantially all is monocrystalline, belongs to rhombic system.
Embodiment 2:
With aluminum nitrate (Al (NO
3)
3Analyze pure 99%), boric acid (H
3BO
3Analyze pure 99%) and citric acid (C
6H
8O
7H
2O analyzes pure 99%) aluminum nitrate in molar ratio: boric acid: citric acid=1: 3: 5 wiring solution-forming, make gel 150 ℃ of lower oven dry, then 1050 ℃ of lower roastings 4 hours, generate the powder of white, the powder of white is water-soluble, centrifugally remove soluble B
2O
3Impurity gets aluminium boroxide (Al
18B
4O
33) nano wire.
With the molten B that goes
2O
3Aluminium boroxide (Al
18B
4O
33) nano thread detects with XRD, the results are shown in Figure 3, uses transmission electron microscope observing, the results are shown in Figure 4; From the result of XRD and transmission electron microscope as can be seen, the aluminium boroxide (Al that generates with sol-gel method
18B
4O
33) the nano thread diameter is more even, substantially all is monocrystalline, belongs to rhombic system.
The Al that relatively makes
4B
2O
9And Al
18B
4O
33, Al
4B
2O
9The diameter of nano thread is very little, is generally 10～20 nanometers; High-temperature product Al
18BxO
33The diameter of nano thread is generally 50～100 nanometers, and length is all more than 1um.
Claims (2)
1. prepare Al
4B
2O
9The method of aluminium boroxide nano wire is characterized in that may further comprise the steps:
1) with 99% analytically pure aluminum nitrate, 99% analytically pure boric acid and 99% analytically pure citric acid, aluminum nitrate in molar ratio: boric acid: the ratio wiring solution-forming of citric acid=1: 1: 1～1: 10: 10 10 ℃～150 ℃ oven dry down, obtains the gel product;
2) with the gel product 750 ℃～1000 ℃ roastings 4 hours to 200 hours, generate the powder of white, get Al
4B
2O
9Nano wire;
3) with Al obtained above
4B
2O
9Nano wire is water-soluble, centrifugally removes soluble B
2O
3Impurity gets final product.
2. prepare Al
18B
4O
33The method of aluminium boroxide nano thread is characterized in that may further comprise the steps:
1) with 99% analytically pure aluminum nitrate, 99% analytically pure boric acid and 99% analytically pure citric acid, aluminum nitrate in molar ratio: boric acid: the ratio wiring solution-forming of citric acid=1: 1: 1～1: 10: 10 10 ℃～150 ℃ oven dry down, obtains the gel product;
2) with the gel product 1050 ℃～2000 ℃ following roastings 4 hours to 200 hours, generate the meal of white, Al
18B
4O
33Nano thread;
3) with Al obtained above
18B
4O
33Nano wire is water-soluble, centrifugally removes soluble B
2O
3Impurity gets final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410016494 CN1256276C (en) | 2004-02-20 | 2004-02-20 | Process for preparing aluminium boroxide nano thread |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410016494 CN1256276C (en) | 2004-02-20 | 2004-02-20 | Process for preparing aluminium boroxide nano thread |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1559899A CN1559899A (en) | 2005-01-05 |
| CN1256276C true CN1256276C (en) | 2006-05-17 |
Family
ID=34440505
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410016494 Expired - Fee Related CN1256276C (en) | 2004-02-20 | 2004-02-20 | Process for preparing aluminium boroxide nano thread |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1256276C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1301216C (en) * | 2005-04-11 | 2007-02-21 | 北京科技大学 | Method for preparing calcium carbonate nano wire |
| CN100372766C (en) * | 2005-12-02 | 2008-03-05 | 华中师范大学 | Al18B4O33 nano wire uniform cladded with BN and preparation process thereof |
| CN101845668B (en) * | 2010-02-07 | 2012-05-16 | 浙江工业大学 | Method for preparing nano nickel borate whiskers |
-
2004
- 2004-02-20 CN CN 200410016494 patent/CN1256276C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1559899A (en) | 2005-01-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1800023A (en) | Acicular alpha-Al2O3 nanometer powder preparation method | |
| CN103193273A (en) | Preparation method of extra-long manganese dioxide nanowires | |
| Shao et al. | MgO nanofibres via an electrospinning technique | |
| CN101746826B (en) | Method for preparing niobium pentoxide hollow nanosphere | |
| WO2013115497A1 (en) | Nanofiber composite and preparation method thereof | |
| CN1256276C (en) | Process for preparing aluminium boroxide nano thread | |
| Xu et al. | A rapid, green and versatile route to synthesize metal carbonate superstructures via the combination of regenerated silk fibroin and compressed CO 2 | |
| Zheng et al. | Synthesis and characterization of LaPO4 powder heat treated at various temperatures | |
| CN1733611A (en) | Zirconium dioxide nano powder material preparation method | |
| CN110512310B (en) | Preparation method of micron-scale alumina fiber | |
| CN1234648C (en) | Process of preparing magnesium boron oxygen nano thread | |
| CN1305773C (en) | Preparation for zinc oxide nanometer material | |
| Wang et al. | Hydrothermal synthesis of SnO2 nanoflower arrays and their optical properties | |
| CN1818153A (en) | Production of nanometer wire with cadmium sulfide | |
| CN110683518A (en) | Process for producing metal oxide | |
| CN1818152A (en) | Method for SiC whisker growth | |
| CN1556067A (en) | Preparaton method of ordered macro porous inorganic oxide material | |
| Xing et al. | Single-crystalline Bi2S3 nanobelts: hydrothermal synthesis and growth mechanism | |
| Truong et al. | Hydrothermal synthesis of hierarchical TiO2 microspheres using a novel titanium complex coordinated by picolinic acid | |
| Li et al. | Shape‐controlled synthesis of yttria nanocrystals under hydrothermal conditions | |
| Hu et al. | Creation of novel ZnO nanostructures: self-assembled nanoribbon/nanoneedle junction networks and faceted nanoneedles on hexagonal microcrystals | |
| CN1324767A (en) | Low temperature prepn. of rutile type nanometer titania by using titanic acid as raw material | |
| CN1834309A (en) | Method of synthetizing two kinds of different shaped silicon carbid nano wire | |
| CN100339305C (en) | Microwave synthesis preparation method for praseodymium hydroxide nanometer rod | |
| CN1239389C (en) | Silicon dioxide composite material containing media pores in concentric ring shaped or in hexagonal structure, and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060517 Termination date: 20130220 |