CN101585544B - Method for preparing aluminum borate nanowire - Google Patents
Method for preparing aluminum borate nanowire Download PDFInfo
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- CN101585544B CN101585544B CN2009100993333A CN200910099333A CN101585544B CN 101585544 B CN101585544 B CN 101585544B CN 2009100993333 A CN2009100993333 A CN 2009100993333A CN 200910099333 A CN200910099333 A CN 200910099333A CN 101585544 B CN101585544 B CN 101585544B
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Abstract
The present invention relates to a method for preparing aluminum borate nanowire which is Al4B2O9 or Al18B4O33 nanowire. The preparation method is implemented according to the following steps of: (1) adding the formula amount of aluminum salt into water for being dissolved sufficiently so that the concentration of aluminum salt solution is 0.01-2.0mol/L, called solution A; (2) adding the formula amount of boric acid and sugar into water for being dissolved sufficiently so that the concentration of boric acid solution is 0.01-2.0mol/L, called solution B; (3) slowly adding the solution B into the solution A for agitation for 2-72 hours, and then drying at 40-300 DEG C to obtain faint yellow xerogel; (4) calcining the xerogel obtained in the step (3) for 2-72 hours at 400-1500 DEG C in an atmosphere of air in order to generate white powder; (5) washing the white powder obtained in the step (4) with hydrochloric acid at first and then with hot water, and drying at 40-200 DEG C to obtain the aluminum borate nanowire. The method is simple in process, easy in operation, high in yield, complete in crystal formation of the product, relatively even in size distribution and high in purity.
Description
(1) technical field
The present invention relates to a kind of method for preparing the aluminum borate nano wire.
(2) background technology
Inorganic materials is all occupied critical role in national economy and national defense construction, wherein aluminium borate whisker has many specific functions as a kind of novel inorganic Material Used, and relatively inexpensive, has been subjected to people's extensive concern in recent years.Because its light weight and hard has excellent characteristics in alloy strengthening, can make alloy obtain high strength, high rigidity, good wear resisting property, low thermal expansivity, feature such as with low cost.As far back as nineteen ninety, the Japanese has just been developed and added Al in aluminium alloy
18B
4O
33The method of whisker is improved the method for alloy property.Aluminium borate whisker belongs to the oxide type whisker in addition, have excellent properties such as high temperature resistant, acid and alkali-resistance, resist chemical, thermal isolation and electrical isolation, can be used as the additive of aluminum matrix composite, engineering plastics, cement, pottery etc., to improve its resistance to compression, resistance to tension, enhancing viscosifying power and erosion resistance etc., also has extensive use in fields such as aerospace, new ceramics and biomaterials.Compare with whisker, nano wire and nanometer rod since size littler, defective still less, the enhancement that is used for matrix material is more obvious.
Up to the present, aluminum borate micron and nano structural material have had several different methods to prepare, as chemical Vapor deposition process, high temperature solid-state method, hydrothermal method etc.But there are a lot of defectives in these methods: as the equipment complexity, and preparation condition harshness (must under protection of inert gas, carry out), productive rate is not high, product pattern inconsistent (dimension distributes and disperses).
(3) summary of the invention
The preparation method who the purpose of this invention is to provide a kind of simple process, aluminum borate nano wire with low cost, free of contamination.
For realizing above purpose, the present invention is achieved through the following technical solutions:
A kind of method for preparing the aluminum borate nano wire, described aluminum borate nano wire is Al
4B
2O
9Or Al
18B
4O
33Nano wire, described method is to be that 1: 1～10: 1～100 aluminium salt, boric acid and template are by the sol-gel method preparation with the amount of substance ratio, described aluminium salt is the alkoxide of water-soluble inorganic aluminate or aluminium, described template is following a kind of soluble sugar: glucose or sucrose, described preparation is carried out as follows: the aluminium salt that (1) gets the prescription amount adds entry and fully dissolves, making the concentration of aluminum salt solution is 0.01～2.0mol/L, is named solution A; (2) get the boric acid of prescription amount and sugar and add entry and fully dissolve, make that boric acid solution concentration is 0.01～2.0mol/L, is named solution B; (3) solution B is slowly added in the solution A, stirred 2～72 hours, 40～300 ℃ of oven dry down, obtain faint yellow xerogel again; (4) xerogel that step (3) is obtained in 400～1500 ℃ of calcinings 2～72 hours, generates white meal under air atmosphere; (5) with hydrochloric acid or the hot water successively white meal that obtains of washing step (4) repeatedly, 40～200 ℃ of dryings make described aluminum borate nano wire.Usually select the salt acid elution of 0.1mol/L for use.
Aluminium salt of the present invention is inorganic aluminate, the preferred aluminum nitrate of described inorganic aluminate, Tai-Ace S 150 or potassium aluminium sulfate.When described aluminium salt is the alkoxide of aluminium, preferred aluminium secondary butylate of the alkoxide of aluminium or aluminum isopropylate.
Method of the present invention, the bake out temperature of step (3) is preferably 100～150 ℃.The calcining temperature of step (4) is preferably 750～1200 ℃.The drying temperature of step (5) is preferably 60～120 ℃.
Template of the present invention is glucose or sucrose.The preparation method of aluminum borate nano wire of the present invention, the concentration of the aluminum salt solution of described step (1) is recommended as 0.1～2.0mol/L.The boric acid solution concentration of described step (2) is 0.1～2.0mol/L.
The kind of the present invention by changing aluminium salt, sugar and the mol ratio of aluminium salt, sugar, boric acid, prepare different size one dimension Al
4B
2O
9Or Al
18B
4O
33Nano wire.
The method that the present invention prepares the aluminum borate nano wire has following beneficial effect: technology is simple, and is easy to operate, the productive rate height, and the product complete in crystal formation, distribution of sizes is more even, the purity height.Can control synthetic different lengths nano wire by change Al/B, sugared content, enlarge aluminum borate nano wire application prospect.
(4) description of drawings
The XRD figure of the aluminum borate nano wire that Fig. 1 embodiment 1 makes.
The SEM figure of the aluminum borate nano wire that Fig. 2 embodiment 1 makes.
The TEM figure of the aluminum borate nano wire that Fig. 3 embodiment 1 makes.
(5) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
Embodiment 1:
Take by weighing 3.75g Al (NO
3)
39H
2O is dissolved in the 100ml distilled water, magnetic agitation obtained mixed liquor A in 2 hours, take by weighing 1.87g boric acid and 5.62g glucose, magnetic agitation mixed and obtains solution B in 1 hour in 100ml distilled water, slowly be added drop-wise to solution B in the mixed liquor A, mix the back 150 ℃ of oven dry down, obtain faint yellow xerogel.With gel calcining 4h under 750 ℃, generate white meal, with hot wash 3 times, 60 ℃ of dryings obtain Al
4B
2O
9Nano wire detects Al through TEM and XRD
4B
2O
9Be the single crystal structure nano wire, the nanowire size uniform distribution, diameter is 25nm, length is at 200～300nm.
Embodiment 2:
Take by weighing 3.75gAl (NO
3)
39H
2O is dissolved in the 200ml distilled water, magnetic agitation obtained mixed liquor A in 24 hours, take by weighing 1.25g boric acid and 5.0g sucrose, magnetic agitation mixed and obtains solution B in 6 hours in 200ml distilled water, slowly be added drop-wise to solution B in the mixed liquor A, mix the back and evaporate 8h down, obtain the chocolate xerogel at 120 ℃.With gel calcining 2h under 1200 ℃, generate white meal, with hot wash 5 times, 100 ℃ of dryings obtain Al
18B
4O
33Nano wire detects Al through TEM and XRD
18B
4O
33Nano wire is a single crystal structure, and diameter is 50～90nm, and length is at 2～3 μ m.
Embodiment 3:
Taking by weighing the 2.46g aluminium secondary butylate is dissolved in the 100ml distilled water, magnetic agitation obtained mixed liquor A in 36 hours, take by weighing 1.24g boric acid and 3.7g glucose, magnetic agitation mixed and obtains solution B in 1 hour in 100ml distilled water, slowly be added drop-wise to solution B in the mixed liquor A, mix the back 100 ℃ of oven dry down, obtain faint yellow xerogel.With gel calcining 4h under 750 ℃, generate white meal, with hot wash 3 times, 60 ℃ of dryings obtain Al
4B
2O
9Nano wire.Detect Al through TEM and XRD
4B
2O
9Nano wire is a single crystal structure, and diameter is about 30nm, and length is 100～200nm.
Example 4:
Taking by weighing the 2.46g aluminium secondary butylate is dissolved in the 100ml distilled water, magnetic agitation obtained mixed liquor A in 36 hours, take by weighing 1.24g boric acid and 3.7g glucose, magnetic agitation mixed and obtains solution B in 1 hour in 100ml distilled water, slowly be added drop-wise to solution B in the mixed liquor A, mix the back 100 ℃ of oven dry down, obtain faint yellow xerogel.With gel calcining 4h under 1150 ℃, generate white meal, with hot wash 6 times, 60 ℃ of dryings obtain Al
18B
4O
33O
9Nano wire.Through TEM and XRD detection nano wire is single crystal structure, and diameter is about 65nm, and length is 1～3 μ m.
Example 5:
Taking by weighing the 10.3g aluminum isopropylate is dissolved in the 150ml distilled water, magnetic agitation obtained mixed liquor A in 72 hours, take by weighing 9.3g boric acid and 1.0g glucose, magnetic agitation mixed and obtains solution B in 1 hour in 100ml distilled water, slowly be added drop-wise to solution B in the mixed liquor A, mix the back 100 ℃ of oven dry down, obtain faint yellow xerogel.With gel calcining 4h under 800 ℃, generate white meal, with hot wash 4 times, 60 ℃ of dryings obtain Al
4B
2O
9Nano wire.Through TEM and XRD detection nano wire is single crystal structure, and diameter is about 25nm, and length is 300～500nm.
Example 6:
Taking by weighing the 3.4g aluminum isopropylate is dissolved in the 150ml distilled water, magnetic agitation obtained mixed liquor A in 6 hours, take by weighing 9.3g boric acid and 12.7g sucrose, magnetic agitation mixed and obtains solution B in 1 hour in 100ml distilled water, slowly be added drop-wise to solution B in the mixed liquor A, mix the back 100 ℃ of oven dry down, obtain dark brown xerogel.With gel calcining 4h under 1250 ℃, generate white meal, with hot wash 4 times, 60 ℃ of dryings obtain Al
18B
4O
33O
9Nano wire.Through TEM and XRD detection nano wire is single crystal structure, and diameter is about 200～400nm, and length is 3～5 μ m.
Example 7:
Take by weighing 0.666g Al
2(SO
4)
318H
2O is dissolved in the 100ml distilled water, magnetic agitation obtained mixed liquor A in 0.5 hour, take by weighing 0.56g boric acid and 18g glucose, magnetic agitation mixed and obtains solution B in 5 hours in 100ml distilled water, slowly be added drop-wise to solution B in the mixed liquor A, mix the back 120 ℃ of oven dry down, obtain faint yellow xerogel.Gel in 750 ℃ of following calcining 3h, is generated white meal, is that the 0.1mol/L aqueous hydrochloric acid washs 5 times with the concentration of hydrochloric acid, and 60 ℃ of dryings obtain Al
4B
2O
9Nano wire detects Al through TEM and XRD
4B
2O
9Be the single crystal structure nano wire, the nanowire size uniform distribution, diameter is 40nm, length is at 400～600nm.
Example 8:
Take by weighing 47.4g KAl (SO
4)
212H
2O is dissolved in the 200ml distilled water, magnetic agitation obtained mixed liquor A in 2 hours, take by weighing 5.6g boric acid and 1.8g glucose, magnetic agitation mixed and obtains solution B in 1 hour in 200ml distilled water, slowly be added drop-wise to solution B in the mixed liquor A, mix the back 150 ℃ of oven dry down, obtain faint yellow xerogel.With gel calcining 4h under 1200 ℃, generate white meal, with hot wash 3 times, 60 ℃ of dryings obtain Al
18B
4O
33O
9Nano wire detects Al through TEM and XRD
18B
4O
33O
9Be the single crystal structure nano wire, nanowire size uniform distribution, diameter are 400～600nm, and length is at 4～10 μ m.
Claims (10)
1. a method for preparing the aluminum borate nano wire is characterized in that described aluminum borate nano wire is Al
4B
2O
9Or Al
18B
4O
33Nano wire, described method is to be that 1: 1～10: 1～100 aluminium salt, boric acid and template are by the sol-gel method preparation with the amount of substance ratio, described aluminium salt is the alkoxide of water-soluble inorganic aluminate or aluminium, the following a kind of soluble sugar of described template: glucose or sucrose, described preparation is carried out as follows: the aluminium salt that (1) gets the prescription amount adds entry and fully dissolves, making the concentration of aluminum salt solution is 0.01～2.0mol/L, is named solution A; (2) get the boric acid of prescription amount and sugar and add entry and fully dissolve, make that boric acid solution concentration is 0.01～2.0mol/L, is named solution B; (3) solution B is slowly added in the solution A, stirred 2～72 hours, 40～300 ℃ of oven dry down, obtain faint yellow xerogel again; (4) xerogel that step (3) is obtained in 400～1500 ℃ of calcinings 2～72 hours, generates white meal under air atmosphere; (5) the white meal that obtains with hydrochloric acid or hot water priority washing step (4), 40～200 ℃ of dryings make described aluminum borate nano wire.
2. the preparation method of aluminum borate nano wire as claimed in claim 1 is characterized in that described aluminium salt is inorganic aluminate, and described inorganic aluminate is aluminum nitrate, Tai-Ace S 150 or potassium aluminium sulfate.
3. the preparation method of aluminum borate nano wire as claimed in claim 1 is characterized in that described aluminium salt is the alkoxide of aluminium, and the alkoxide of described aluminium is aluminium secondary butylate or aluminum isopropylate.
4. the preparation method of aluminum borate nano wire as claimed in claim 1, the bake out temperature that it is characterized in that described step (3) is 100～150 ℃.
5. the preparation method of aluminum borate nano wire as claimed in claim 1, the calcining temperature that it is characterized in that described step (4) is 750～1200 ℃, calcination time is 3～4 hours.
6. the preparation method of aluminum borate nano wire as claimed in claim 1, the drying temperature that it is characterized in that described step (5) is 60～120 ℃.
7. the preparation method of aluminum borate nano wire as claimed in claim 1 is characterized in that described template is glucose or sucrose.
8. the preparation method of aluminum borate nano wire as claimed in claim 1, the concentration that it is characterized in that the aluminum salt solution of described step (1) is 0.1～2.0mol/L.
9. the preparation method of aluminum borate nano wire as claimed in claim 1, the boric acid solution concentration that it is characterized in that described step (2) is 0.1～2.0mol/L.
10. the preparation method of aluminum borate nano wire as claimed in claim 1 is characterized in that the concentration of the described hydrochloric acid of described step (5) is 0.1mol/L.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845668B (en) * | 2010-02-07 | 2012-05-16 | 浙江工业大学 | Method for preparing nano nickel borate whiskers |
| CN101823724B (en) * | 2010-03-31 | 2011-09-21 | 西北有色金属研究院 | Preparation method of aluminum borate crystal |
| CN101892513A (en) * | 2010-06-24 | 2010-11-24 | 沈阳化工大学 | Method for preparing nano slabby aluminium borate whisker by hydrothermal method |
| CN103641231B (en) * | 2013-12-09 | 2016-05-18 | 浙江工业大学 | A kind of application of visible light catalyst copper borate degradation of dye waste water |
| CN103723738B (en) * | 2013-12-09 | 2015-10-07 | 浙江工业大学 | A kind of preparation method of rodlike single-crystal structure cupric borate |
| KR102323215B1 (en) * | 2015-05-20 | 2021-11-08 | 삼성전자주식회사 | Electrode active material, electrode and energy storage device including the same, and method for preparing the electrode active material |
| JP6509668B2 (en) * | 2015-08-04 | 2019-05-08 | 国立大学法人室蘭工業大学 | Method of manufacturing aluminum borate whisker |
| CN108069389B (en) * | 2017-12-07 | 2020-06-09 | 天津大学 | Preparation method of magnetic control directional fast moving micro-nano robot |
| CN110143601B (en) * | 2018-02-11 | 2022-12-23 | 天津市职业大学 | Preparation method of magnesium borate nanowire and application of magnesium borate nanowire in epoxy resin |
| CN113086986B (en) * | 2019-12-23 | 2022-08-30 | 中国石油天然气股份有限公司 | Nano aluminum borate, preparation method and application thereof, cross-linking agent and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793409A (en) * | 2005-12-02 | 2006-06-28 | 华中师范大学 | Al18B4O33 nano wire uniform cladded with BN and preparation process thereof |
| CN101378994A (en) * | 2005-12-02 | 2009-03-04 | 普罗托泰克股份有限公司 | Nanoparticles, and a method of sol-gel processing |
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2009
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793409A (en) * | 2005-12-02 | 2006-06-28 | 华中师范大学 | Al18B4O33 nano wire uniform cladded with BN and preparation process thereof |
| CN101378994A (en) * | 2005-12-02 | 2009-03-04 | 普罗托泰克股份有限公司 | Nanoparticles, and a method of sol-gel processing |
Non-Patent Citations (3)
| Title |
|---|
| Jian Wang et al..Large-scale synthesis of Al4B2O9/Al18B4O33 whiskers via a novel method.《Materials Letters》.2007,第62卷1208-1211. * |
| JP特开2004-142970A 2004.05.20 |
| Jun Wang et al..Synthesis of aluminium borate nanowires by sol–gel method.《Materials Research Bulletin》.2005,第40卷1551-1557. * |
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