CN102021654A - Method for preparing magnetic nanotube - Google Patents
Method for preparing magnetic nanotube Download PDFInfo
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- CN102021654A CN102021654A CN 201010575330 CN201010575330A CN102021654A CN 102021654 A CN102021654 A CN 102021654A CN 201010575330 CN201010575330 CN 201010575330 CN 201010575330 A CN201010575330 A CN 201010575330A CN 102021654 A CN102021654 A CN 102021654A
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Abstract
The invention discloses a method for preparing a magnetic nanotube. The method comprises the following steps of: placing a 100 to 200nm-aperture aluminum oxide film into the middle of two quartz reaction tanks; adding unitary or binary ferric metal ion plating solution with the total concentration of 0.02 to 0.1 mol/L into one quartz reaction tank, and adding 5 to 15g/L sodium borohydride aqueous solution into the other quartz reaction tank; standing at room temperature for 2 to 20 minutes; taking a black nanotube/an aluminum oxide composite membrane down; dissolving the black nanotube/ the aluminum oxide composite membrane in 1 to 2mol/L NaOH solution for not less than 5 minutes; and washing the dissolved nanotube for multiple times through distilled water and absolute ethanol, and drying under vacuum at room temperature to constant weight. Compared with the prior art, the method has the advantages that: the nanotube is synthesized by a one-step method, a synthesizing device is simple and the preparation cycle is short. The prepared magnetic nanotube has good loading function due to a porous structure so as to provide magnetic raw materials for the medicine in loading, targeted transport and the like.
Description
Technical field:
The present invention relates to preparation of nanomaterials, belong to the preparation method of Magnetic nano-pipe especially.
Background technology:
At present, synthetic method for Magnetic nano-pipe also is not very ripe, reporting more is the template electrochemical deposition method, yet this method synthesizing magnetic nanotube, the method that usually all need adopt the vacuum evaporating conducting film in the one side of alumina formwork or be coated with conductive resin is made conductive layer and just can be carried out the electrochemistry operation, there is the equipment requirements height in this method, poor practicability, problems such as gained material aftertreatment trouble.Simultaneously to use some special synthetic technology and strategies usually, could obtain through multistep is synthetic in order to obtain tubular structure.For example, need carry out the chemically modified pre-treatment to alumina formwork, use molecule anchor or precursor induce synthetic, adopt multilayer template replica technique and template carried out local metal spraying so that formed ring electrode substrate etc.The general bad control on nanotube is synthesizing of this method.
Summary of the invention:
Technical problem to be solved by this invention provides a kind of preparation method of simple and easy controlled Magnetic nano-pipe.
The technical scheme of technical solution problem of the present invention is: a kind of preparation method of Magnetic nano-pipe comprises following operation:
With aperture 100-200nm pellumina, be placed on the centre in two quartz reaction ponds, it is 0.02-0.1mol/L monobasic or binary Ferrious material ion plating bath that total concn is injected in a quartz reaction pond, the 5-15g/L sodium borohydride aqueous solution is injected in another quartz reaction pond, left standstill under the room temperature 2-20 minute, take off black nano pipe/aluminum oxide composite membrane, be no less than 5 minutes with the dissolving of 1-2mol/L NaOH solution, the nanotube that is dissolved out is cleaned for several times through distilled water and dehydrated alcohol again, the vacuum room temperature is dried to constant weight, obtains amorphous Magnetic nano-pipe.
In order to obtain the nanotube of crystalline state, in 300-500 ℃ of heating under vacuum annealing 30-100 minute, vacuum tightness was greater than 0.995 crust with corresponding amorphous nano pipe.
Described Ferrious material ion is ferrous ion, divalent cobalt ion, bivalent nickel ion.
In order to obtain the nanotube of magnetic oxide, with 300-500 ℃ of heating 60-100 minute in air of amorphous iron nanotube.
As shown in Figure 2, as microreactor, wherein pellumina has played the effect of hard template with the nano aperture of multiaperture pellumina in the present invention; Sodium borohydride molecule and reduced metal ion enter hole from the template both sides respectively, and when in the template hole, meeting, redox reaction takes place immediately and discharge a large amount of gases, because the aperture of template is very little, so the gas that generates preferentially moves and discharges from the less hole axis of resistance, make the ion that is reduced in hole wall place deposition and to adhere to; Sedimentary metal or alloy particle can be used as new vegetative point on the template hole wall, adds that the activity of template hole wall is very high, and other ion just continues to continue on these vegetative point along the tube wall growth, thereby has formed nanotube.
One of advantage of the inventive method is, it has realized the simple and easy method of single stage method synthesis of nano pipe, and synthesizer is very simple, and preparation cycle is very short, can efficiently be utilized, and has promotion and application preferably and is worth.
Second advantage of the inventive method be, it has expanded the technology of template synthesizing one-dimensional nano material, and the Magnetic nano-pipe pattern that synthesizes is controlled, and array is good.
The 3rd advantage of the inventive method be, it has solved the novel method of a kind of synthesizing magnetic metal, magneticalloy and ferrite nano pipe, for the research of magneticsubstance provide research means.
The 4th advantage of the inventive method is that it provides a kind of synthetic method of magnetic amorphous nanotube.
The 5th advantage of the inventive method is by the further anneal to target magnetic amorphous nanotube, can obtain corresponding crystalline state Magnetic nano-pipe, thereby the simple and easy synthetic technology of crystalline state Magnetic nano-pipe also is provided.
The 6th advantage of the inventive method be, the Magnetic nano-pipe that present technique synthesizes, and its vesicular structure can provide good loading functional, provides the magnetic raw material thereby also can be drug loading and target transportation etc.
Description of drawings
Fig. 1 is a device synoptic diagram of the present invention;
Fig. 2 forms synoptic diagram for nanotube among the present invention;
Fig. 3 is the electron scanning micrograph of cobalt nanotube;
Fig. 4 is the electron scanning micrograph of nickel nanotube;
Fig. 5 is the electron scanning micrograph of iron nanotube;
Fig. 6 is the electron scanning micrograph of cobalt nickel nanotube;
Fig. 7 is the electron scanning micrograph of ferro-cobalt nanotube;
Fig. 8 is the electron scanning micrograph of iron nickel nanotube.
In Fig. 1,1 is that quartz reaction pond, 2 is that plating bath, 3 is pellumina, and 4 is sodium borohydride aqueous solution.
Embodiment:
Below in conjunction with embodiment the present invention is done detailed explanation.
200nm pellumina 3 a slices of getting purchase place the centre in two quartz reaction ponds 1, and a quartz reaction pond implantation concentration is 0.08mol/L CoSO
4Solution 2,10g/L sodium borohydride aqueous solution 4 is injected in another quartz reaction pond, left standstill under the room temperature 8 minutes, take off black nano pipe/aluminum oxide composite membrane, clean this composite membrane 3-4 time with distilled water and dehydrated alcohol respectively again, put into the vacuum drying oven drying at room temperature to constant weight, be partly dissolved the shape appearance figure (Fig. 3) that available scanning electronic microscope detects nano-tube array with 2mol/L NaOH; Immerse 2mol/L NaOH 48 hours and all dissolve to pellumina, again through the distilled water eccentric cleaning to pH be neutrality, use the dehydrated alcohol rinsing at last 2 times, put into the vacuum drying oven drying at room temperature to constant weight, can obtain magnetic amorphous cobalt nanotube.The magnetic cobalt nanotube of gained was annealed 80 minutes in 380 ℃ of heating under vacuum, and vacuum tightness can obtain corresponding crystalline state cobalt nanotube greater than 0.995 crust.
The 200nm pellumina a slice of getting purchase places the centre in two quartz reaction ponds, and a quartz reaction pond implantation concentration is 0.06mol/L NiSO
4Solution, the 8g/L sodium borohydride aqueous solution is injected in another quartz reaction pond, left standstill under the room temperature 10 minutes, take off black nano pipe/aluminum oxide composite membrane, clean this composite membrane 3-4 time with distilled water and dehydrated alcohol respectively again, put into the vacuum drying oven drying at room temperature to constant weight, be partly dissolved the shape appearance figure (Fig. 4) that available scanning electronic microscope detects nano-tube array with 2mol/LNaOH; Immerse 2mol/L NaOH 48 hours and all dissolve to pellumina, again through the distilled water eccentric cleaning to pH be neutrality, use the dehydrated alcohol rinsing at last 2 times, put into the vacuum drying oven drying at room temperature to constant weight, can obtain magnetic amorphous nickel nanotube.
The magnetic nickel nano pipe of gained was annealed 100 minutes in 420 ℃ of heating under vacuum, and vacuum tightness can obtain corresponding crystalline state nickel nanotube greater than 0.995 crust.
The 200nm pellumina a slice of getting purchase places the centre in two quartz reaction ponds, and a quartz reaction pond implantation concentration is 0.05mol/L FeSO
4Solution, the 5g/L sodium borohydride aqueous solution is injected in another quartz reaction pond, left standstill under the room temperature 12 minutes, take off black nano pipe/aluminum oxide composite membrane, clean this composite membrane 3-4 time with distilled water and dehydrated alcohol respectively again, put into the vacuum drying oven drying at room temperature to constant weight, be partly dissolved the shape appearance figure (Fig. 5) that available scanning electronic microscope detects nano-tube array with 2mol/LNaOH; Immerse 2mol/L NaOH 48 hours and all dissolve to pellumina, again through the distilled water eccentric cleaning to pH be neutrality, use the dehydrated alcohol rinsing at last 2 times, put into the vacuum drying oven drying at room temperature to constant weight, can obtain the magnetic amorphous iron nanotube.
The magnetic amorphous iron nanotube of gained was annealed 80 minutes in 350 ℃ of heating under vacuum, and vacuum tightness can obtain corresponding crystalline state iron nanotube greater than 0.995 crust.
With the magnetic amorphous iron nanotube of gained in air in 350 ℃ of heating 60 minutes, can obtain the magnetic ferric oxide nano pipe.
The 200nm pellumina a slice of getting purchase places the centre in two quartz reaction ponds, and a quartz reaction pond implantation concentration is 0.06mol/L CoSO
4, 0.02mol/L NiSO
4Solution, the 10g/L sodium borohydride aqueous solution is injected in another quartz reaction pond, left standstill under the room temperature 10 minutes, take off black nano pipe/aluminum oxide composite membrane, clean this composite membrane 3-4 time with distilled water and dehydrated alcohol respectively again, put into the vacuum drying oven drying at room temperature to constant weight, be partly dissolved the shape appearance figure (Fig. 6) that available scanning electronic microscope detects nano-tube array with 2mol/L NaOH; Immerse 2mol/L NaOH 48 hours and all dissolve to pellumina, again through the distilled water eccentric cleaning to pH be neutrality, use the dehydrated alcohol rinsing at last 2 times, put into the vacuum drying oven drying at room temperature to constant weight, can obtain magnetic amorphous cobalt nickel nanotube.
The magnetic cobalt nickel nanotube of gained was annealed 80 minutes in 380 ℃ of heating under vacuum, and vacuum tightness can obtain corresponding crystalline state nanotube greater than 0.995 crust.
Embodiment 5
The 200nm pellumina a slice of getting purchase places the centre in two quartz reaction ponds, and a quartz reaction pond implantation concentration is 0.05mol/L CoSO
4, 0.03mol/L FeSO
4Solution, the 7g/L sodium borohydride aqueous solution is injected in another quartz reaction pond, left standstill under the room temperature 8 minutes, take off black nano pipe/aluminum oxide composite membrane, clean this composite membrane 3-4 time with distilled water and dehydrated alcohol respectively again, put into the vacuum drying oven drying at room temperature to constant weight, be partly dissolved the shape appearance figure (Fig. 7) that available scanning electronic microscope detects nano-tube array with 2mol/L NaOH; Immerse 2mol/L NaOH 48 hours and all dissolve to pellumina, again through the distilled water eccentric cleaning to pH be neutrality, use the dehydrated alcohol rinsing at last 2 times, put into the vacuum drying oven drying at room temperature to constant weight, can obtain magnetic amorphous ferro-cobalt nanotube.
The magnetic ferro-cobalt nanotube of gained was annealed 80 minutes in 400 ℃ of heating under vacuum, and vacuum tightness can obtain corresponding crystalline state nanotube greater than 0.995 crust.
The 200nm pellumina a slice of getting purchase places the centre in two quartz reaction ponds, and a quartz reaction pond implantation concentration is 0.04mol/L NiSO
4, 0.02mol/L FeSO
4Solution, the 5g/L sodium borohydride aqueous solution is injected in another quartz reaction pond, left standstill under the room temperature 12 minutes, take off black nano pipe/aluminum oxide composite membrane, clean this composite membrane 3-4 time with distilled water and dehydrated alcohol respectively again, put into the vacuum drying oven drying at room temperature to constant weight, be partly dissolved the shape appearance figure (Fig. 8) that available scanning electronic microscope detects nano-tube array with 2mol/L NaOH; Immerse 2mol/L NaOH 48 hours and all dissolve to pellumina, again through the distilled water eccentric cleaning to pH be neutrality, use the dehydrated alcohol rinsing at last 2 times, put into the vacuum drying oven drying at room temperature to constant weight, can obtain magnetic amorphous ferronickel nanotube.
The magnetic ferronickel nanotube of gained was annealed 100 minutes in 400 ℃ of heating under vacuum, and vacuum tightness can obtain corresponding crystalline state nanotube greater than 0.995 crust.
Claims (4)
1. the preparation method of a Magnetic nano-pipe is characterized in that: comprise following operation:
With aperture 100-200nm pellumina, be placed on the centre in two quartz reaction ponds, it is 0.02-0.1mol/L monobasic or binary Ferrious material ion plating bath that total concn is injected in a quartz reaction pond, the 5-15g/L sodium borohydride aqueous solution is injected in another quartz reaction pond, left standstill under the room temperature 2-20 minute, take off black nano pipe/aluminum oxide composite membrane, be no less than 5 minutes with the dissolving of 1-2mol/L NaOH solution, the nanotube that is dissolved out is cleaned for several times through distilled water and dehydrated alcohol again, the vacuum room temperature is dried to constant weight, obtains amorphous Magnetic nano-pipe.
2. the preparation method of a kind of Magnetic nano-pipe according to claim 1, it is characterized in that: described Ferrious material ion is ferrous ion, divalent cobalt ion, bivalent nickel ion.
3. the preparation method of a kind of Magnetic nano-pipe according to claim 1 is characterized in that: in 300-500 ℃ of heating under vacuum annealing 30-100 minute, vacuum tightness can obtain the Magnetic nano-pipe of crystalline state greater than 0.995 crust with amorphous nanotube.
4. the preparation method of a kind of Magnetic nano-pipe according to claim 1 is characterized in that: with 300-500 ℃ of heating 60-100 minute in air of amorphous iron nanotube, can obtain the oxide magnetic nanotube.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103406547A (en) * | 2013-08-01 | 2013-11-27 | 皖南医学院 | Controllable efficient dye degradation nano-catalyst synthesis method and nanotube |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2310065A1 (en) * | 1997-11-18 | 1999-05-27 | Martin Moskovits | Controlled synthesis and metal-filling of aligned carbon nanotubes |
| CN1621338A (en) * | 2004-12-17 | 2005-06-01 | 清华大学 | Synthesis method of iron nanotube array |
| CN101148271A (en) * | 2007-05-31 | 2008-03-26 | 中国科学院电工研究所 | Preparation method for gamma-Fe2O3 nano-tube |
| CN101319407A (en) * | 2008-06-25 | 2008-12-10 | 北京理工大学 | Preparation method of metallic oxide nanometer granular nano-array material |
| US7585474B2 (en) * | 2005-10-13 | 2009-09-08 | The Research Foundation Of State University Of New York | Ternary oxide nanostructures and methods of making same |
| CN101692364A (en) * | 2009-10-12 | 2010-04-07 | 钢铁研究总院 | One-dimensional permanent magnetic nano-material, in which hard magnetic tubes are coated with soft magnetic wires and preparation method thereof |
-
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2310065A1 (en) * | 1997-11-18 | 1999-05-27 | Martin Moskovits | Controlled synthesis and metal-filling of aligned carbon nanotubes |
| CN1621338A (en) * | 2004-12-17 | 2005-06-01 | 清华大学 | Synthesis method of iron nanotube array |
| US7585474B2 (en) * | 2005-10-13 | 2009-09-08 | The Research Foundation Of State University Of New York | Ternary oxide nanostructures and methods of making same |
| CN101148271A (en) * | 2007-05-31 | 2008-03-26 | 中国科学院电工研究所 | Preparation method for gamma-Fe2O3 nano-tube |
| CN101319407A (en) * | 2008-06-25 | 2008-12-10 | 北京理工大学 | Preparation method of metallic oxide nanometer granular nano-array material |
| CN101692364A (en) * | 2009-10-12 | 2010-04-07 | 钢铁研究总院 | One-dimensional permanent magnetic nano-material, in which hard magnetic tubes are coated with soft magnetic wires and preparation method thereof |
Non-Patent Citations (5)
| Title |
|---|
| 《化学学报》 20051231 李玮瑒 Ni(OH)2纳米管的制备、表征及电化学性能 , 第05期 2 * |
| 《化学研究》 20091231 汪峰 氧化钴纳米管的制备和模板剂多孔氧化铝的孔洞结构 , 第02期 2 * |
| 《材料导报》 20100228 李祥子 镍纳米管阵列的电沉积合成及其磁学性能表征 112-114 1-4 , 第4期 2 * |
| 《物理化学学报》 20061231 任鑫 化学沉积法制备Ni-P纳米线与纳米管有序阵列 , 第01期 2 * |
| 《物理化学学报》 20091231 陶菲菲 磁性金属镍纳米管的有效合成(英文) , 第05期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103406547A (en) * | 2013-08-01 | 2013-11-27 | 皖南医学院 | Controllable efficient dye degradation nano-catalyst synthesis method and nanotube |
| CN103406547B (en) * | 2013-08-01 | 2015-12-02 | 皖南医学院 | A kind of controllable synthesis method of high efficiency dye degraded nanocatalyst and a kind of nanotube |
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