CN100453707C - Method for preparing diameter different monocrystal bismuth nanowire microarray by using uniform hole diameter alumina template - Google Patents
Method for preparing diameter different monocrystal bismuth nanowire microarray by using uniform hole diameter alumina template Download PDFInfo
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- CN100453707C CN100453707C CNB2004100651102A CN200410065110A CN100453707C CN 100453707 C CN100453707 C CN 100453707C CN B2004100651102 A CNB2004100651102 A CN B2004100651102A CN 200410065110 A CN200410065110 A CN 200410065110A CN 100453707 C CN100453707 C CN 100453707C
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Abstract
The present invention discloses a method for preparing diameter different monocrystal bismuth nano wire micro-arrays by using a uniform hole diameter alumina template. The method comprises a pulse electrodeposition method; especially, electrodeposition liquid is formed by preparing 5 to 15 g/l of bismuth trichloride, 40 to 60 g/l of tartaric acid, 85 to 105 g/l of glycerol and 40-60 g/l of sodium chloride; a pH value is from 0.9 to 1.3; pulse voltage is composed pulse delay voltage with 0 V and pulse deposition voltage with-1.1 to 1.8 V, wherein the time of the pulse delay voltage is the time of 40 to 60 ms; the time of the pulse deposition voltage is from 10 to 45 ms; the time of the pulse deposition voltage is the time of 10 to 20 ms; the time of the pulse delay voltage is from 10 to 50 ms. A micro-array comprises a bismuth nano wire array; especially, a monocrystal bismuth nano wire is made of the following raw material: 5 to 15 g/l of bismuth trichloride, 40 to 60 g/l of tartaric acid, 85 to 105 g/l of glycerol and 40 to 60 g/l of sodium chloride; the diameter of the monocrystal bismuth nano wire is the hole diameter of 5 nm of alumina template. Needed monocrystal bismuth nano wire micro-arrays with different diameters can be prepared on a uniform hole diameter alumina template.
Description
Technical field
The present invention relates to a kind of method for preparing monocrystal bismuth nanowire microarray, especially use single aperture alumina formwork to prepare the method for different diameter monocrystal bismuth nanowire microarray.
Background technology
Current society is more and more higher to various components and parts performance demands, impel people constantly to explore and to break through device size ultimate approach, no matter and quasi-one-dimensional nanometer material is as novel light, electricity, magnetic device, as the needle point of Scanning Probe Microscopy STM, photon cable, quantum chip etc., still the line between the device nodes all has very wide application prospect.Bismuth is typical semi-metallic, have the Fermi surface of each diversity of height, very little electron effective mass, big carrier mean free path and semi-metal-characteristics such as semi-conductor transformation, extremely wide application prospect is arranged in fields such as thermoelectricity, transmitter and huge magnetic impedances.Therefore, people are in order to obtain the nano thread array of bismuth, adopted multiple technical measures, as " University Of Tianjin's journal) " the 7th volume the 3rd interim " adopting electrodeposition technology for preparing bismuth nano-wire array " (the Transactions of Tianjin University that publishes in September calendar year 2001, Vol 7No.3 Sep.2001, Fabrication of Binanowire array by electrodepositiontechnology) literary composition once disclosed a kind of use pulse electrodeposition prepared bismuth nano-wire material, in this technology, with platinum is electrode, adopt the impulse electrodeposition technology of fixed pulse width, by with bismuth deposit in aluminum oxide porous film nanometer level microporous, prepare the bismuth nano-wire array material.But this technology exists weak point, and at first, the diameter of the nano wire of preparing is changeless, and the size of its diameter depends on the aperture of aluminum oxide porous film, is identical with the nanometer level microporous footpath of aluminum oxide porous film promptly also; Secondly, theoretical investigation shows that along with reducing of nano thread diameter, the thermoelectricity capability of bismuth can improve significantly, and because the technology of preparing of small-bore alumina formwork is imperfect as yet, obtains so template is extremely difficult, makes the bismuth nanowire of preparation minor diameter be difficult to realize; Its three, even the small-bore alumina formwork is easy to get, along with reducing of alumina formwork bore dia, the assembling of the high quality nano thread difficulty that also becomes further.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of practicality for overcoming weak point of the prior art, and the single aperture of use easy to use alumina formwork prepares the method for different diameter monocrystal bismuth nanowire microarray.
The method of using single aperture alumina formwork to prepare the different diameter monocrystal bismuth nanowire microarray comprises the pulse electrodeposition method, particularly said electrodeposit liquid is formulated by the sodium-chlor of the glycerine of the tartrate of the Trichlorobismuthine of 5～15g/l, 40～60g/l, 85～105g/l and 40～60g/l, its pH value is 0.9～1.3, the order of electrodeposit liquid preparation is, earlier with sodium-chlor and glycerine mixing mutually, add tartrate and mixing again, add Trichlorobismuthine and mixing at last; Said pulsed voltage is made of the pulsed deposition voltage of 0 volt pulse delay voltage and-1.1～-1.8 volt, wherein, the time of pulse delay voltage is certain when point between 40～60ms, the time of regulating impulse deposition voltage is 10～45ms, thereby makes the monocrystal bismuth nanowire microarray of required different diameter.
As using single aperture alumina formwork to prepare the further improvements in methods of different diameter monocrystal bismuth nanowire microarray, described electrodeposit liquid is formulated by 10g/l Trichlorobismuthine, 50g/l tartrate, 95g/l glycerine and 50g/l sodium-chlor, and its pH value is 1; The time of described pulse delay voltage, the time of pulsed deposition voltage was 10～45ms when being 50ms; The one side of described aluminium sesquioxide bilateral template with single aperture is covered with golden film and is placed in the electrodeposit liquid, and is that negative electrode, graphite are anode with golden film; The aperture of described aluminium sesquioxide bilateral template is≤98nm.
The monocrystal bismuth nanowire microarray that uses single aperture alumina formwork to prepare the method preparation of different diameter monocrystal bismuth nanowire microarray comprises monocrystal bismuth nanowire microarray, and particularly said monocrystal bismuth nanowire is to be made by the raw material of following ratio: Trichlorobismuthine 5～15g/l, tartrate 40～60g/l, glycerine 85～105g/l and sodium-chlor 40～60g/l; The diameter of said monocrystal bismuth nanowire is the aperture of 5nm～aluminium sesquioxide bilateral template.
Beneficial effect with respect to prior art is, one, the monocrystal bismuth nanowire microarray that makes is used x-ray diffractometer respectively, after transmission electron microscope and field emission scanning electron microscope characterize and test, from the X-ray diffracting spectrum that obtains, transmission electron microscope photo and corresponding selected area electron diffraction photo, and stereoscan photograph as can be known, bismuth nanowire is height-oriented, and along with transfer from (110) to (202) direction has appearred in the increase of pulsed deposition time, the resulting bismuth nanowire of selected area electron diffraction analytical proof of corresponding nano thread is good monocrystalline, simultaneously, along with the diameter of the increase bismuth nanowire of pulsed deposition voltage time increases gradually, this point can the fact littler than the aperture of the template that is wrapped in be able to clearly witness by the diameter of bismuth nanowire, thereby has realized the adjustable of bismuth nanowire diameter on a large scale; They are two years old, through test a large amount of, repeatedly, only adopting different electrodeposit liquid prescriptions, and strictly limit under the situation of sequencing of electrodeposit liquid configuration, the monocrystal bismuth nanowire of different diameter could be both in the alumina formwork in same aperture, prepared, and the homogeneity of the diameter of the monocrystal bismuth nanowire prepared can be guaranteed again; Its three, by a large amount of tests, draw by its result, have only the time point and the corresponding width of setting and regulating suitable pulse delay voltage and pulsed deposition voltage respectively, just can make the monocrystal bismuth nanowire of required diameter; Its four, the diameter of bismuth nanowire can be adjustable on a large scale, especially the nano thread of minor diameter can be adjusted to about 5nm, has fully satisfied the needs of using in the future; Its five, be covered with golden film in the one side of bilateral template and be placed in the electrodeposit liquid, and be that negative electrode, graphite are anode with golden film, make the bismuth ion in the electrodeposit liquid be easier to deposit in the micropore of alumina templates; Its six, the aperture of aluminium sesquioxide bilateral template is elected as≤98nm, can satisfy at present the demand to the diameter of monocrystal bismuth nanowire fully.
Description of drawings
Below in conjunction with accompanying drawing optimal way of the present invention is described in further detail.
Fig. 1 is to after adopting prepared monocrystal bismuth nanowire microarray of different pulsed deposition time to use the test of Philips Pw 1700X type rotating anode X-ray diffractometer, the X ray diffracting spectrum (XRD) of the monocrystal bismuth nanowire array that obtains, wherein, the ordinate zou of XRD is an intensity, X-coordinate is angle (2 θ), the test result of four spectral lines among the figure when respective pulses depositing time is 10ms, 20ms, 30ms, 40ms respectively;
Fig. 2 be to take the photograph after adopting prepared monocrystal bismuth nanowire of different pulsed deposition time with the observation of H-800 type conventional transmission electron microscope photo, wherein, (a) be transmission electron microscope photo with the bismuth nanowire of pulsed deposition time of 10ms preparation, the upper right corner is its corresponding selected area electron diffraction photo in the sheet, (b) be transmission electron microscope photo with the bismuth nanowire of pulsed deposition time of 20ms preparation, the upper right corner is its corresponding selected area electron diffraction photo in the sheet, (c) be transmission electron microscope photo with the bismuth nanowire of pulsed deposition time of 30ms preparation, the upper right corner is its corresponding selected area electron diffraction photo in the sheet, (d) be transmission electron microscope photo with the bismuth nanowire of pulsed deposition time of 45ms preparation, the upper right corner is its corresponding selected area electron diffraction photo in the sheet, can be by photo (a), see clearly that (b) diameter of bismuth nanowire is more much smaller than the aperture of the template of wrapping up it;
Fig. 3 is to adopting different prepared monocrystal bismuth nanowire microarrays of pulsed deposition time, after dissolving away aluminium sesquioxide lamina membranacea wherein, again with take the photograph after the JEOL JSM-6700F type field emission scanning electron microscope observation photo, wherein, (a) be stereoscan photograph with the bismuth nanowire of pulsed deposition time of 20ms preparation, monocrystal bismuth nanowire in the sheet is positive, its diameter is 16nm, (b) be stereoscan photograph with the bismuth nanowire of pulsed deposition time of 30ms preparation, monocrystal bismuth nanowire in the sheet is the side, its diameter is 40nm, (c) be stereoscan photograph with the bismuth nanowire of pulsed deposition time of 45ms preparation, monocrystal bismuth nanowire in the sheet is the bottom surface, and its diameter is 80nm.
Embodiment
Obtain the order mesoporous bilateral template of aluminium sesquioxide in same aperture earlier successively with anonizing, metal chloride removal method and phosphoric acid perforate method, wherein, the specific surface area of bilateral template is 9～19m
2/ g, porosity are 30～50%, the aperture is 98nm, and the thickness of template is 60～120 μ m.
Embodiment 1: the one side that with the aperture that makes is the order mesoporous bilateral template of aluminium sesquioxide of 98nm earlier is the goldleaf of 30nm with the last thickness of vacuum vapour deposition spraying; It is 0.9 electrodeposit liquid that the template that will be covered with goldleaf again places by the formulated pH value of Trichlorobismuthine, tartrate, glycerine and sodium-chlor, wherein, Trichlorobismuthine is that 5g/l, tartrate are that 60g/l, glycerine are that 85g/l, sodium-chlor are 60g/l, the order of this electrodeposit liquid preparation is: earlier with sodium-chlor and glycerine mixing mutually, add tartrate and mixing again, add Trichlorobismuthine and mixing at last; At last, with the goldleaf on the template is negative electrode, graphite flake in the electrodeposit liquid is an anode, timesharing ground in addition 0 volt pulse delay voltage and-1.1 volts pulsed deposition voltage between negative electrode and anode, wherein, the time of pulse delay voltage is 60ms, and the time of pulsed deposition voltage is 10ms, thereby makes as the spectral line among Fig. 1, Fig. 2 (a), be similar to the monocrystal bismuth nanowire microarray of diameter shown in Fig. 3 (a).
Embodiment 2: the one side that with the aperture that makes is the order mesoporous bilateral template of aluminium sesquioxide of 98nm earlier is the goldleaf of 30nm with the last thickness of vacuum vapour deposition spraying; It is 1 electrodeposit liquid that the template that will be covered with goldleaf again places by the formulated pH value of Trichlorobismuthine, tartrate, glycerine and sodium-chlor, wherein, Trichlorobismuthine is that 8g/l, tartrate are that 55g/l, glycerine are that 90g/l, sodium-chlor are 55g/l, the order of this electrodeposit liquid preparation is: earlier with sodium-chlor and glycerine mixing mutually, add tartrate and mixing again, add Trichlorobismuthine and mixing at last; At last, with the goldleaf on the template is negative electrode, graphite flake in the electrodeposit liquid is an anode, timesharing ground in addition 0 volt pulse delay voltage and-1.2 volts pulsed deposition voltage between negative electrode and anode, wherein, the time of pulse delay voltage is 55ms, and the time of pulsed deposition voltage is 20ms, thereby makes the monocrystal bismuth nanowire microarray of diameter shown in the spectral line among Fig. 1, Fig. 2 (b), Fig. 3 (a).
Embodiment 3: the one side that with the aperture that makes is the order mesoporous bilateral template of aluminium sesquioxide of 98nm earlier is the goldleaf of 30nm with the last thickness of vacuum vapour deposition spraying; It is 1.1 electrodeposit liquid that the template that will be covered with goldleaf again places by the formulated pH value of Trichlorobismuthine, tartrate, glycerine and sodium-chlor, wherein, Trichlorobismuthine is that 10g/l, tartrate are that 50g/l, glycerine are that 95g/l, sodium-chlor are 50g/l, the order of this electrodeposit liquid preparation is: earlier with sodium-chlor and glycerine mixing mutually, add tartrate and mixing again, add Trichlorobismuthine and mixing at last; At last, with the goldleaf on the template is negative electrode, graphite flake in the electrodeposit liquid is an anode, timesharing ground in addition 0 volt pulse delay voltage and-1.4 volts pulsed deposition voltage between negative electrode and anode, wherein, the time of pulse delay voltage is 50ms, and the time of pulsed deposition voltage is 25ms, thereby makes the monocrystal bismuth nanowire microarray that is similar to diameter shown in the spectral line among Fig. 1, Fig. 2 (c), Fig. 3 (b).
Embodiment 4: the one side that with the aperture that makes is the order mesoporous bilateral template of aluminium sesquioxide of 98nm earlier is the goldleaf of 30nm with the last thickness of vacuum vapour deposition spraying; It is 1.2 electrodeposit liquid that the template that will be covered with goldleaf again places by the formulated pH value of Trichlorobismuthine, tartrate, glycerine and sodium-chlor, wherein, Trichlorobismuthine is that 12g/l, tartrate are that 45g/l, glycerine are that 100g/l, sodium-chlor are 45g/l, the order of this electrodeposit liquid preparation is: earlier with sodium-chlor and glycerine mixing mutually, add tartrate and mixing again, add Trichlorobismuthine and mixing at last; At last, with the goldleaf on the template is negative electrode, graphite flake in the electrodeposit liquid is an anode, timesharing ground in addition 0 volt pulse delay voltage and-1.6 volts pulsed deposition voltage between negative electrode and anode, wherein, the time of pulse delay voltage is 45ms, and the time of pulsed deposition voltage is 30ms, thereby makes the monocrystal bismuth nanowire microarray of diameter shown in the spectral line among Fig. 1, Fig. 2 (c), Fig. 3 (b).
Embodiment 5: the one side that with the aperture that makes is the order mesoporous bilateral template of aluminium sesquioxide of 98nm earlier is the goldleaf of 30nm with the last thickness of vacuum vapour deposition spraying; It is 1.3 electrodeposit liquid that the template that will be covered with goldleaf again places by the formulated pH value of Trichlorobismuthine, tartrate, glycerine and sodium-chlor, wherein, Trichlorobismuthine is that 15g/l, tartrate are that 40g/l, glycerine are that 105g/l, sodium-chlor are 40g/l, the order of this electrodeposit liquid preparation is: earlier with sodium-chlor and glycerine mixing mutually, add tartrate and mixing again, add Trichlorobismuthine and mixing at last; At last, with the goldleaf on the template is negative electrode, graphite flake in the electrodeposit liquid is an anode, timesharing ground in addition 0 volt pulse delay voltage and-1.8 volts pulsed deposition voltage between negative electrode and anode, wherein, the time of pulse delay voltage is 40ms, and the time of pulsed deposition voltage is 45ms, thereby makes the monocrystal bismuth nanowire microarray of diameter shown in the spectral line among Fig. 1, Fig. 2 (d), Fig. 3 (c).
Obviously, those skilled in the art can carry out various changes and modification to the method that the single aperture of use of the present invention alumina formwork prepares the different diameter monocrystal bismuth nanowire microarray and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (5)
1, a kind of method of using single aperture alumina formwork to prepare the different diameter monocrystal bismuth nanowire microarray comprises the pulse electrodeposition method, it is characterized in that:
1.1, said electrodeposit liquid is formulated by the sodium-chlor of the glycerine of the tartrate of the Trichlorobismuthine of 5～15g/l, 40～60g/l, 85～105g/l and 40～60g/l, its pH value is 0.9～1.3, the order of electrodeposit liquid preparation is, earlier with sodium-chlor and glycerine mixing mutually, add tartrate and mixing again, add Trichlorobismuthine and mixing at last;
1.2, said pulsed voltage is made of 0 volt pulse delay voltage and-1.1～-1.8 volts pulsed deposition voltage, wherein, the time of pulse delay voltage is certain when point between 40～60ms, the time of regulating impulse deposition voltage is 10～45ms, thereby makes the monocrystal bismuth nanowire microarray of required different diameter.
2, the single aperture of use according to claim 1 alumina formwork prepares the method for different diameter monocrystal bismuth nanowire microarray, it is characterized in that electrodeposit liquid is formulated by 10g/l Trichlorobismuthine, 50g/l tartrate, 95g/l glycerine and 50g/l sodium-chlor, its pH value is 1.
3, the single aperture of use according to claim 1 alumina formwork prepares the method for different diameter monocrystal bismuth nanowire microarray, and the time that it is characterized in that pulse delay voltage, the time of pulsed deposition voltage was 10～45ms when being 50ms.
4, the single aperture of use according to claim 1 alumina formwork prepares the method for different diameter monocrystal bismuth nanowire microarray, it is characterized in that one side with the aluminium sesquioxide bilateral template in single aperture is covered with golden film and is placed in the electrodeposit liquid, and be that negative electrode, graphite are anode with golden film.
5, the single aperture of use according to claim 1 alumina formwork prepares the method for different diameter monocrystal bismuth nanowire microarray, and the aperture that it is characterized in that aluminium sesquioxide bilateral template is 98nm.
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| CN101857971B (en) * | 2009-04-07 | 2013-04-03 | 中国科学院合肥物质科学研究院 | Bismuth/bismuth-antimony extensional superlattice nanowire and preparation method thereof |
| JP2013147489A (en) * | 2011-12-22 | 2013-08-01 | Gc Corp | Agent for imparting fluorescence to ceramic |
| CN102672162B (en) * | 2012-06-04 | 2014-01-29 | 中山大学 | Bismuth nanofiber three-dimensional structural material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6187165B1 (en) * | 1997-10-02 | 2001-02-13 | The John Hopkins University | Arrays of semi-metallic bismuth nanowires and fabrication techniques therefor |
| CN1401558A (en) * | 2002-09-06 | 2003-03-12 | 南京大学 | Method for preparing AIN nanowire and its array |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6187165B1 (en) * | 1997-10-02 | 2001-02-13 | The John Hopkins University | Arrays of semi-metallic bismuth nanowires and fabrication techniques therefor |
| CN1401558A (en) * | 2002-09-06 | 2003-03-12 | 南京大学 | Method for preparing AIN nanowire and its array |
Non-Patent Citations (4)
| Title |
|---|
| FABRICATION OF Bi NANOWIRE ARRAY BYELECTRODEPOSITION TECHNOLOGY. 王为，王惠，巩运兰.天津大学学报(英文版),，第7卷第3期. 2001 * |
| Processing and Charaterization of Single-crystalline UltrafineBismuth Nanowires. Zhibo Zhang, Dmitry Gekhtman.Chem. Mater.,No.11. 1999 * |
| 电化学组装一维纳米线阵列温差电材料. 王为，贾法龙，巩运兰，王惠，张伟玲.天津大学学报，第37卷第8期. 2004 * |
| 电沉积技术及其在合成纳米材料中的应用. 鲍英，杨金觊，孙金全，王积森，徐庆莘，刘静萍，闫怀英.山东机械，第4期. 2003 * |
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