CN101845646B - Preparation method of gold nano-wire of monocrystalline and polycrystalline structure - Google Patents
Preparation method of gold nano-wire of monocrystalline and polycrystalline structure Download PDFInfo
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- CN101845646B CN101845646B CN2009100808135A CN200910080813A CN101845646B CN 101845646 B CN101845646 B CN 101845646B CN 2009100808135 A CN2009100808135 A CN 2009100808135A CN 200910080813 A CN200910080813 A CN 200910080813A CN 101845646 B CN101845646 B CN 101845646B
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- gold
- nanowires
- monocrystalline
- preparation
- polycrystalline structure
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Abstract
The invention relates to a preparation method of a gold nano-wire of a monocrystalline and polycrystalline structure, which comprises the following steps: 1) forming metal electrodes of gold or platinum on a silicon chip with a semiconductor technology; 2) placing the silicon chip into plating solution in a plating bath, and powering up the metal electrode pairs with AC current for electrodeposition of the gold nano-wire; and 3) taking out, cleaning and drying the silicon chip, thereby completing the preparation of the gold nano-wire of the monocrystalline and polycrystalline structure. The method of the invention needs no template, and can simply, rapidly and economically realize the preparation of the gold nano-wire of the monocrystalline and polycrystalline structure. The diameter of the obtained gold nano-wire of the monocrystalline and polycrystalline structure is 5-100nm, and the aspect ratio thereof is higher than 200.
Description
Technical field
The present invention relates to a kind of preparation method of nanowires of gold, particularly relate to a kind of method of utilizing the preparation of alternating-current depositing operation to have monocrystalline and polycrystalline nanowires of gold.
Background technology
Nano wire is a kind of urstoff based on nanoscale, method by physics and chemistry, arrange the nanostructure system of the line array that assembles according to certain rules, it is the basis of design ultramicro-quantum structure devices of new generation, and is manifesting great application prospect as the line of syringe needle, nano-device and the super large unicircuit of scanning tunnel microscope, the microelectrode of chemical sensor, the aspects such as super strengthening agent of matrix material.Nanowires of gold is a kind of in numerous nano wires, is specially adapted to make the wire of nanometer micro-electrode and nano-device.
The present method that adopts the prepared by electrodeposition nano wire is generally the aluminum oxide masterplate or photoetching masterplate householder method obtains, as document 1:K.Biswas, and et al.Physica Status Solidi a, 2007,204:3152; H.J.H.Chen, et al.Nanotechnology, 2005,16:2913 introduces.But utilize alumina formwork or Lithographic template auxiliary law to obtain nano wire at present, exist template and be not easy to obtain, hole density and bore length such as are restricted at problem.
Summary of the invention
The objective of the invention is to: overcome the template that exists in the existing nanowires of gold technology of preparing and be not easy to obtain, and the hole density of template and bore length such as are restricted at problem; Thereby provide a kind of fast simple, no template, utilize the interchange prepared by electrodeposition to have the method for the nanowires of gold of monocrystalline and polycrystalline structure.
The object of the present invention is achieved like this:
Preparation provided by the invention has the method for monocrystalline and polycrystalline nanowires of gold, may further comprise the steps:
1) the preparation metal electrode is right on silicon chip: adopt the semi-conductor filming technology, the metal electrode of arbitrary shape that forms spacing and be 2～100um on silicon chip is right;
2) utilize alternating-current deposited gold nano wire: metal electrode the is arranged right silicon chip that step 1) is obtained is put into the electroplate liquid of plating tank, described metal electrode on, pass to alternating-current and electroplate, realize the galvanic deposit of nanowires of gold, obtain being deposited on metal electrode between nanowires of gold; Wherein, the voltage peak of the alternating-current that is applied is 12～20V, and frequency is 10
2～10
7Hz; Conduction time 5～10s; Described electroplate liquid is that the gold concentration scope is 2 * 10
-8Mol/l～2 * 10
-3The gold plating liquid of mol/l;
3) cleaning and oven dry: step 2) silicon chip of the deposited gold nano wire that obtains takes out, and adopts the semi-conductor cleaning to clean and oven dry, finishes the preparation of the nanowires of gold with monocrystalline and polycrystalline structure.
In above-mentioned technical scheme, the nanowires of gold that is obtained is carried out tem observation, the gained nanowires of gold is monocrystalline and polycrystalline structure, and diameter is between 10～100nm.
In above-mentioned technical scheme, the semiconductor coated film technology in the described step 1) comprises: the method for vacuum plating or sputtering method.
In above-mentioned technical scheme, the metal electrode in the described step 1) is to being the metallic film that gold or platinum are made, and the thickness of described metallic film is 200nm.
In above-mentioned technical scheme, in step 2) described in gold plating liquid be: 5 * 10
-7G～5 * 10
-2G potassiumiodide, 5 * 10
-7G～5 * 10
-2G iodine, 4 * 10
-8G～4 * 10
-3G gold and 10ml ethanol are formed.
In above-mentioned technical scheme, clean in the described step 3) and adopt dehydrated alcohol.
The invention has the advantages that:
The invention provides the preparation method of the nanowires of gold of a kind of monocrystalline and polycrystalline structure, it is right to adopt semiconductor technology to form metal electrode on silicon chip, again by alternating-current metal electrode on the method for deposited gold nano wire.This method need not template, can prepare nanowires of gold between the electrode pair arbitrarily, has the preparation that simply realizes the nanowires of gold of monocrystalline and polycrystalline structure fast, economically; The diameter of the monocrystalline that is obtained and the nanowires of gold of polycrystalline structure is at 10～100nm, and length-to-diameter ratio is greater than 200.
Description of drawings
Fig. 1 is the device synoptic diagram that the present invention prepares nanowires of gold.
Caption:
1, silicon chip 2, metal electrode to 3, nanowires of gold
4, SiO
2Layer 5, signal generator 6, electroplate liquid 7, plating tank
Embodiment
In detail preparation method of the present invention is described below in conjunction with embodiment and accompanying drawing:
Embodiment 1
The invention provides between the electrode that alternating-current is deposited on 2 interdigitated gold, preparation has the method for the nanowires of gold of monocrystalline and polycrystalline structure, specifically may further comprise the steps:
1). the present invention at first adopts the method for sputter, at the SiO of silicon chip 1
2Carry out sputter on the layer 4, form the electrode pair 2 of interdigitated gold, the interelectrode distance of the electrode pair 2 of this interdigitated gold is that 2～20um, interdigital spacing are 5um; Wherein, splash-proofing sputtering process parameter: coating chamber vacuum tightness is that 4Pa, sputtering current 5mA, sputtering voltage 1000V, sputtering time are 45s; The thickness of the gold thin film of institute's sputter is 200nm, and promptly the thickness of Jin electrode pair 2 is 200nm;
2). in above-mentioned steps 1) metal electrode of the gold that makes is on 2 the silicon chip 1, put into the electroplate liquid 6 of plating tank 7, carry out galvanic deposit, use signal generator 5, at the metal electrode of gold to 2 two ends, pass to alternating-current and carry out galvanic deposit, switched on for 5～10 seconds, on silicon chip, make nanowires of gold with monocrystalline and polycrystalline structure; Wherein concrete electrodeposition condition: pass to alternating-current (P-to-P voltage 12～20V, frequency 10
2～10
7Hz); The electroplate liquid 6 that present embodiment carries out deposited Au nano wire 3 is that (gold concentration is 4 * 10 to trace level
-3Mol/l) gold plating liquid, this gold plating liquid prescription is as follows:
Potassiumiodide 5 * 10
-2g
Iodine 5 * 10
-2g
Gold 4 * 10
-3g
Ethanol 10ml;
3). with taking out on the silicon chip 1, clean up, dry with dehydrated alcohol, finish diameter and be 5～100nm, length-to-diameter ratio is greater than 200 the preparation with monocrystalline and polycrystalline nanowires of gold.
Embodiment 2
The invention provides and use the alternating-current electroplating technology, between the electrode of 2 rectangular-shaped platinum, preparation has the method for the nanowires of gold of monocrystalline and polycrystalline structure, specifically may further comprise the steps:
1). the present invention at first adopts the method (the coating process parameter: vacuum tightness is 3E-3, evaporation current 12A, evaporation time 5min) of vacuum plating, at the SiO of silicon chip 1
2On the layer 4, the metal electrode that formation has platinum material is to 2, and this metal electrode is the rectangular-shaped of 5～100um to 2 interelectrode distance; The thickness of the platinum film of vacuum plating is 200nm, and promptly the thickness of the electrode pair 2 of platinum is 200nm;
2). in above-mentioned steps 1) make have platinum metal electrode on 2 the silicon chip 1, carry out the deposited Au nano wire: the metal electrode of step 1) being made platinum is to 2 sample, put into the electroplate liquid 6 of plating tank 7, use signal generator 5, metal electrode to platinum passes to alternating-current to 2 two ends, alternating-current P-to-P voltage 12～20V, frequency 10
2～10
7Hz switched on for 5～10 seconds the deposited Au nano wire;
The electroplate liquid 6 that present embodiment carries out deposited Au nano wire 3 is trace level (1 * 10
-6Mol/l) gold plating liquid, this gold plating liquid prescription:
Potassiumiodide 2.5 * 10
-5g
Iodine 2.5 * 10
-5g
Gold 2 * 10
-6g
Ethanol 10ml;
3). silicon chip 1 is taken out, cleans up, dries with dehydrated alcohol, finish between rectangular-shaped platinum electrode, make diameter be 5～100nm, have a nanowires of gold of monocrystalline and polycrystalline structure.
Embodiment 3
The invention provides at the metal electrode of tip-angled shape gold a preparation is had the method for the nanowires of gold of monocrystalline and polycrystalline structure, the preparation method specifically may further comprise the steps with embodiment 1:
1). the present invention at first adopts the method for sputter, at the SiO of silicon chip 1
2Layer carries out sputter on 4, and the tip-angled shape gold electrode that forms the interelectrode distance that has gold copper-base alloy and be 10～100um is to 2 substrate; Wherein, splash-proofing sputtering process parameter: coating chamber vacuum tightness is that 4Pa, sputtering current 5mA, sputtering voltage 1000V, sputtering time are 45s;
2). in above-mentioned steps 1) sample of deposited Au nano wire on substrate, put into plating tank, use signal generator 5, to gold electrode to 2 two ends, pass to alternating-current and carry out galvanic deposit, switched on for 5～10 seconds, on silicon chip, make nanowires of gold with monocrystalline and polycrystalline structure; Wherein concrete electrodeposition condition: pass to alternating-current (P-to-P voltage 12～20V, frequency 10
2～10
7Hz); The electroplate liquid 6 that present embodiment carries out deposited Au nano wire 3 is that (gold concentration is 2 * 10 to trace level
-8Mol/l) gold plating liquid, this gold plating liquid prescription is as follows:
Potassiumiodide 5 * 10
-7g
Iodine 5 * 10
-7g
Gold 4 * 10
-8g
Ethanol 10ml
3). the silicon chip 1 of step 3) being made the nanowires of gold with monocrystalline and polycrystalline structure takes out, with dehydrated alcohol clean up, and oven dry, finish the tip-angled shape gold electrode to the preparation with monocrystalline and polycrystalline nanowires of gold.
Claims (6)
1. the preparation method with nanowires of gold of monocrystalline and polycrystalline structure is characterized in that, may further comprise the steps:
1) adopt semiconductor coated film technology on silicon chip, the formation spacing is that the arbitrary shape metal electrode of 2～100 μ m is right;
2) metal electrode the is arranged right silicon chip that step 1) is obtained is put into the electroplate liquid of plating tank, described metal electrode on pass to alternating-current and electroplate, realize the galvanic deposit of nanowires of gold; Wherein, the voltage peak of the alternating-current that is applied is 12～20V, and frequency is 10
2～10
7Hz; Conduction time 5～10s; Described electroplate liquid is that the gold concentration scope is 2 * 10
-8Mol/l～2 * 10
-3The gold plating liquid of mol/l, described gold plating liquid is by 5 * 10
-7G～5 * 10
-2G potassiumiodide, 5 * 10
-7G～5 * 10
-2G iodine, 4 * 10
-8G～4 * 10
-3G gold and 10ml ethanol are formed;
3) with step 2) the nanowires of gold silicon chip that obtains takes out, and adopts the semi-conductor cleaning to clean and oven dry, finishes the preparation with monocrystalline and polycrystalline nanowires of gold.
2. by the described preparation method of claim 1, it is characterized in that the semiconductor coated film technology in the described step 1) comprises technique for vacuum coating with nanowires of gold of monocrystalline and polycrystalline structure.
3. by the described preparation method of claim 1, it is characterized in that the semiconductor coated film technology in the described step 1) is sputter coating process with nanowires of gold of monocrystalline and polycrystalline structure.
4. by the described preparation method with nanowires of gold of monocrystalline and polycrystalline structure of claim 1, it is characterized in that the metal electrode in the described step 1) is to being the metallic film that gold or platinum are made, the thickness of described metallic film is 200nm.
5. by the described preparation method of claim 1, it is characterized in that described step 2 with nanowires of gold of monocrystalline and polycrystalline structure) in resulting nanowires of gold diameter be 5～100nm.
6. by the described preparation method of claim 1, it is characterized in that adopting the semi-conductor cleaning to clean in the described step 3) is to clean with dehydrated alcohol with nanowires of gold of monocrystalline and polycrystalline structure.
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| CN101845646B true CN101845646B (en) | 2011-11-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103990793A (en) * | 2014-05-09 | 2014-08-20 | 北京威士恩科技有限公司 | High-length-to-diameter-ratio solid-walled hollow gold/gold-silver nanotube and manufacturing method thereof |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105593409A (en) * | 2013-08-07 | 2016-05-18 | 艾克泽基因公司 | Sensor growth controller |
| CN111893527A (en) * | 2020-08-04 | 2020-11-06 | 淮南师范学院 | Nano electrode pair and preparation method thereof |
| CN116835523B (en) * | 2023-08-31 | 2023-11-28 | 常州天策电子科技有限公司 | Preparation method of thin film pressure sensor based on nanowire array and pressure sensor |
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| CN1995468A (en) * | 2006-12-18 | 2007-07-11 | 天津理工大学 | Diameter-controllable metal nm-line array preparation method |
| JP2007239055A (en) * | 2006-03-10 | 2007-09-20 | Kyushu Univ | Method for producing metal nanowire |
| KR100813113B1 (en) * | 2007-02-26 | 2008-03-17 | 성균관대학교산학협력단 | Manufacturing method for au nano wire |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007239055A (en) * | 2006-03-10 | 2007-09-20 | Kyushu Univ | Method for producing metal nanowire |
| CN1995468A (en) * | 2006-12-18 | 2007-07-11 | 天津理工大学 | Diameter-controllable metal nm-line array preparation method |
| KR100813113B1 (en) * | 2007-02-26 | 2008-03-17 | 성균관대학교산학협력단 | Manufacturing method for au nano wire |
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| 徐剑.一维金属纳米材料的制备技术.《粉末冶金材料科学与工程》.2006,第11卷(第1期),13-18. * |
| 李桂春.碘化浸金时从浸出液中提金及碘再生方法研究.《矿冶工程》.2006,第26卷(第3期),42-47. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103990793A (en) * | 2014-05-09 | 2014-08-20 | 北京威士恩科技有限公司 | High-length-to-diameter-ratio solid-walled hollow gold/gold-silver nanotube and manufacturing method thereof |
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| CN101845646A (en) | 2010-09-29 |
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Granted publication date: 20111109 Termination date: 20120323 |