CN103011071A - Preparation method of metal nano needle tip with sharp end of small curvature radius - Google Patents
Preparation method of metal nano needle tip with sharp end of small curvature radius Download PDFInfo
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- CN103011071A CN103011071A CN2012105754133A CN201210575413A CN103011071A CN 103011071 A CN103011071 A CN 103011071A CN 2012105754133 A CN2012105754133 A CN 2012105754133A CN 201210575413 A CN201210575413 A CN 201210575413A CN 103011071 A CN103011071 A CN 103011071A
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Abstract
The invention discloses a preparation method of a metal nano needle tip with a sharp end of small curvature radius. The preparation method comprises the following steps of: preparing a needle tip template through electrochemical corrosion of an anode, wherein the needle tip template is a needle tip with a sharp end of small curvature radius; cleaning the needle tip template with deionized water to remove residual corrosive solution on the surface of the needle tip template, and drying the needle tip template; fixing the needle tip template on one side of a substrate of a film preparation device, and making the direction of the sharp end of the needle tip template opposite to a diffusion direction of an evaporation source or a sputtering source; starting the film preparation device for metal deposition on the surface of the needle tip template to obtain a metal layer on the surface of the needle tip template; and obtaining the prepared metal needle tip after metal deposition is completed. The needle tip prepared by the method has the advantages of high quality, higher purity and low cost and is suitable for mass preparation. Moreover, the required device has the advantages of simple structure, low cost, convenient operation and good repeatability.
Description
Technical field
The invention belongs to the technical field of advanced micro-nano material preparation in microelectronics and information electronic, be specifically related to a kind of preparation method of metal material apiculus radius of curvature nanometer pinpoint.
Background technology
Be applied to the tip curvature radius of apiculus radius of curvature needle point structure pointer shape structure of semi-conducting material and device research less than the structure of 100 nanometers.This structure can be used for the performance test aspect of nanoscale semiconductor devices or material, such as the probe of AFM, and the probe of original position electron microscope power-electrical characteristics test, and the manipulator in the micro-nano processing is most advanced and sophisticated.Because the maximum feature that micro-nano structure has is exactly little, the fragile structure of yardstick, and conventional large scale manipulator and probe tip yardstick are all more than micron level, use conventional means directly to test the micro-nano structure of small scale, so need to apiculus radius of curvature needle point structure of the present invention to directly, effectively handling and test of micro-nano structure.
Although the preparation of apiculus radius of curvature needle point structure has had more people to be studied, the result of research concentrates on a few material at present, such as tungsten, copper and the aluminium needle point of the method preparation of using electrochemical corrosion.The method of at present electrochemical corrosion can obtain very little (less than the 10 nanometers) needle point of tip curvature radius, and repeatability is relatively good.General laboratory uses simple electrochemical corrosion just can obtain preferably needle point structure.But its defective is to prepare a few needle point structure.Such as the present general way that adopts machine cut of the precious metal materials such as gold, platinum, palladium, also namely use special instrument to cut sth. askew wire in the hope of obtaining the cutting-edge structure of an angle for difficult corroding metal or some semi-conducting material.This method success rate is usually poor, and resulting metal needle point also is difficult to have little radius of curvature, therefore is difficult to satisfy the needs of some experiment.Yet, because the peculiar oxidation resistance of precious metal material, high work function and with the excellent electric contact characteristic of semi-conducting material, use the needle point of precious metal material usually to become the first-selection of a lot of devices and testing of materials.In addition, for the test of magnetic properties, the metal material that metallic cobalt, iron are normally first-selected.Therefore, in the present circumstance, the method that find a kind of aspect, prepares the apiculus radius of curvature needle point of different metal material fast, cheaply is a problem with remarkable realistic meaning.
Summary of the invention
Goal of the invention: the preparation that the present invention is directed to the medium and small tip curvature radius of prior art needle point structure can only for the defective of a few material, provide a kind of preparation method that can prepare different metal material apiculus radius of curvature nanometer pinpoint.
Technical scheme: for solving the problems of the technologies described above, the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention adopts following technical scheme:
A kind of preparation method of metal material apiculus radius of curvature nanometer pinpoint may further comprise the steps:
1), use the method for anode electrochemical corrosion to prepare the template needle point, described template needle point is apiculus radius of curvature needle point;
2), the template needle point of step 1) is removed the residual corrosive liquid of template needle surface with washed with de-ionized water, dry;
3), with step 2) the template needle point that obtains is fixed on substrate one side of equipment for producing thin film, make the template needle point the tip towards relative with the dispersal direction of evaporation source or sputtering source;
4), start equipment for producing thin film and carry out the deposit of metal material on the surface of template needle point, obtain the layer of metal layer on the surface of template needle point;
5), the metal material deposit finishes the metal needle point that obtains preparing.
Preferably, the material of described template needle point is aluminium, copper or tungsten.Because the preparation ratio of tungsten tip is easier to, success rate is also higher, therefore usually can prepare with the tungsten metal.
Preferably, the thickness of metal level described in the step 4) is the 5-20 nanometer.
Preferably, described sputter or thin evaporated film Preparation equipment are evaporimeter, sputter, molecular beam epitaxial device or atomic layer deposition apparatus.
Preferably, described metal material is gold, platinum, palladium, silver, cobalt or iron.
Beneficial effect: the apiculus radius of curvature needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention uses electrochemical corrosion to prepare is the template needle point, the front end that is combined in the template needle point uses sputter or the needed metal material of method of evaporating deposit, utilize the peculiar shadow effect of deposition of materials at the various metal material of template needle point preparation, to obtain the needle point structure of different metal material.Its advantage is that the quality of the needle point that obtains is good, and purity is higher, and cost is low, is suitable for preparation in enormous quantities, and needed equipment is simple, and is with low cost, easy to operate, good reproducibility.
Description of drawings
Fig. 1 is the preparation method's of metal material apiculus radius of curvature nanometer pinpoint of the present invention principle schematic, A is evaporation source among the figure, B indicates the dispersal direction of evaporation source, and C is the metal needle point as template, and D is the metal needle point structure in the preparation of the tip of template needle point;
Fig. 2 is ESEM (SEM) photo of the tungsten template needle point of anode electrochemical caustic solution preparation;
Fig. 3 is ESEM (SEM) photo of the copper mold plate needle point of anode electrochemical caustic solution preparation;
Fig. 4 is ESEM (SEM) photo of the aluminum alloy pattern plate needle point of anode electrochemical caustic solution preparation;
Fig. 5 utilizes the transmission electron microscope photo of the palladium needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares;
Fig. 6 utilizes the partial enlarged drawing of the palladium needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares;
Fig. 7 utilizes the electron diffraction diagram of the palladium needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares;
Fig. 8 utilizes the transmission electron microscope photo of the acupuncture needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares;
Fig. 9 utilizes the electron diffraction diagram of the acupuncture needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares;
Figure 10 utilizes the partial enlarged drawing of the acupuncture needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares;
Figure 11 utilizes the transmission electron microscope photo of the acupuncture needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares;
Figure 12 utilizes the electron diffraction diagram of the acupuncture needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares;
Figure 13 utilizes the partial enlarged drawing of the acupuncture needle point that the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention prepares.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, further illustrate the present invention, should understand these embodiment only is used for explanation the present invention and is not used in and limits the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
See also shown in Figure 1, Fig. 1 utilizes the preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention to prepare the principle schematic of metal needle point, A is evaporation source among the figure, B indicates the dispersal direction of evaporation source, C is the metal needle point as template, and D is the metal needle point structure in the preparation of the tip of template needle point.
The preparation method's of metal material apiculus radius of curvature nanometer pinpoint of the present invention concrete preparation flow is as follows:
1, use the method for anode electrochemical corrosion to prepare the template needle point.The material of needle point can be that aluminium, copper or tungsten etc. hold corrosion-prone material.Because the preparation ratio of tungsten tip is easier to, success rate is also higher, therefore usually can prepare with the tungsten metal.Use the tungsten filament of diameter smaller (being generally less than as required 2 millimeters), surface finish is smooth, and one end inserts corrosive liquid 0.2 millimeter to remove oxide on surface, and corrosive liquid uses the sodium hydroxide solution of 0.5 mol/L.The external power positive pole is connected on the tungsten wire to be corroded, and negative pole is received a carbon-point and is inserted in the corrosive liquid, and two-stage passes into 3-6 V voltage, and can see the tungsten wire by very fast corrosion this moment, regulates the speed that applied voltage can be regulated corrosion.Different according to the initial diameter of tungsten filament and the voltage that applies see after some minutes that generally tungsten filament is corroded to the tungsten metal needle point that the voltage of using instead when very thin about 1.0-2.0 V corrodes at a slow speed to obtain small curvature radius.Resulting tungsten metal needle point is through for subsequent use behind the cleaning-drying.Use the typical pattern of the standby tungsten metal needle point of this legal system as shown in Figure 2.
Also can use aluminium, copper etc. to prepare the material of needle point as template by electrochemical corrosion easily according to the difference of concrete needs.The concrete technology of copper and the corrosion of aluminium needle point is difference to some extent, such as, the typical process of anodic attack aluminium needle point is: the HCl of 1.5 mol/L mixes the Na of 0.25 mol/L
2SO
4Apply 0.5 V DC voltage, Current Control is at 0.01 A; The typical process of anodic attack copper needle point is: the HNO of 2.23 mol/L under the room temperature
3Apply 4 V DC voltages, Current Control is at 0.01 A.
2, the template needle point is removed through washed with de-ionized water to be placed on behind the residual corrosive liquid of template needle surface and is dried dryly to prevent surface oxidation in the drying box, and the needle point after general the cleaning need to use with interior as early as possible at 24 hours.
3, the template needle point is fixed on substrate one side of the equipment for producing thin film such as sputter or evaporation, make the template needle point the tip towards relative with the dispersal direction of evaporation source or sputtering source.
4, start equipment for producing thin film and carry out the deposit of needed metal material, obtain the layer of metal layer on the surface of template needle point.Wherein, metal material can be for being gold, platinum, palladium, silver, cobalt or iron.Control evaporation or sputter thickness are in the 5-20 nanometer as required.The needle point that the method for use sputter prepares other metals need to use sputter (Sputtering).The templated metal needle point that has prepared is adhered on the sample base of sputter, make needle point towards sputtering source.Begin to vacuumize after placing tungsten metal needle point and target, after vacuum reaches the sputter requirement, can begin to carry out sputter.But according to the metal level of general needs in needle surface sputter 5-20 nanometer thickness.Because the particular form of sputter-deposited materials can form the needed metal of one deck on the surface of tungsten tip template, therefore obtains needed needle point structure (seeing also shown in Figure 1).Wherein, equipment for producing thin film also can adopt evaporimeter (evaporation), molecular beam epitaxy (MBE) equipment or ald (ALD) equipment.
The needle point that the templated metal needle point can use copper, aluminium etc. to prepare by electrochemical corrosion easily; Vacuum chamber can be the various shape specification; The depositional mode of metal can be evaporation or pulsed laser deposition.
5, the metal material deposit finishes, and takes out the metal needle point for preparing, and is kept in the drying box stand-by.
See also Fig. 2, Fig. 3 and shown in Figure 4, the typical shape appearance figure as the template needle point of anode electrochemical caustic solution preparation.Wherein Fig. 3 is tungsten tip ESEM (SEM) photo, and Fig. 4 is the TEM photo of copper needle point, and Fig. 5 is the TEM photo of aluminium needle point.Can use these to corrode the needle point of preparation as template by Anodic.
See also Fig. 5, Fig. 6 and shown in Figure 7, Fig. 5 has provided the transmission electron microscope photo that uses the palladium metal needle point of template synthesis.Can see that the palladium that the tungsten tip surface as template is deposited covers on scheme.Fig. 6 has provided the partial enlarged drawing of needle surface, and the zone of amplification goes out at Fig. 5 center.Can see that surface coverage the palladium particle of little crystallite dimension on scheme.The electronic diffraction of Fig. 7 has confirmed surperficial palladium polycrystalline structure.Several representative palladium crystal face diffraction mark at figure.
See also Fig. 8, Fig. 9 and shown in Figure 10, Fig. 8 has provided the transmission electron microscope photo that uses the acupuncture needle point of template synthesis.Can see that the gold that the tungsten tip surface as template is deposited covers on scheme.Fig. 9 has provided the electron diffraction diagram of the gold grain of surface coverage.This diffraction pattern is consistent with the electronic diffraction collection of illustrative plates of gold copper-base alloy, has confirmed the formation of polycrystalline structure gold on the surface.Figure 10 has provided the partial enlarged drawing of needle surface, and the zone of amplification goes out at Fig. 8 center.Can see the gold grain of the polycrystalline structure of surface coverage from Figure 10.
See also Figure 11, Figure 12 and shown in Figure 13, Figure 11 has provided the transmission electron microscope photo that uses the acupuncture needle point of template synthesis.Can see that the silver that the tungsten tip surface as template is deposited covers on scheme.Figure 12 has provided the electron diffraction diagram of the silver-colored particle of surface coverage.Several representative silver-colored crystal face diffraction mark at figure.Confirmed the tectal formation of silver surface of polycrystalline structure.Figure 13 has provided the partial enlarged drawing of needle surface.Can see the silver-colored particle of the polycrystalline structure of surface coverage from Figure 13.
The preparation method of metal material apiculus radius of curvature nanometer pinpoint of the present invention uses tungsten, copper or the aluminium needle point of the apiculus radius of curvature that electrochemical corrosion prepares to be template, the front end that is combined in the template needle point uses sputter or the needed metal material of method of evaporating deposit, utilize the peculiar shadow effect of deposition of materials at the various metal material of template needle point preparation, to obtain the needle point structure of different metal material.Its advantage that has is that the quality of the needle point that obtains is good, and purity is higher, and cost is low, is suitable for preparation in enormous quantities, and needed equipment is simple, and is with low cost, easy to operate, good reproducibility.
Claims (5)
1. the preparation method of a metal material apiculus radius of curvature nanometer pinpoint is characterized in that, may further comprise the steps:
1), use the method for anode electrochemical corrosion to prepare the template needle point, described template needle point is apiculus radius of curvature needle point;
2), the template needle point of step 1) is removed the residual corrosive liquid of template needle surface with washed with de-ionized water, dry;
3), with step 2) the template needle point that obtains is fixed on substrate one side of equipment for producing thin film, make the template needle point the tip towards relative with the dispersal direction of evaporation source or sputtering source;
4), start equipment for producing thin film and carry out the deposit of metal material on the surface of template needle point, obtain the layer of metal layer on the surface of template needle point;
5), the metal material deposit finishes the metal needle point that obtains preparing.
2. the preparation method of metal material apiculus radius of curvature nanometer pinpoint as claimed in claim 1 is characterized in that, the material of described template needle point is aluminium, copper or tungsten.
3. the preparation method of metal material apiculus radius of curvature nanometer pinpoint as claimed in claim 1 is characterized in that, the thickness of metal level described in the step 4) is the 5-20 nanometer.
4. the preparation method of metal material apiculus radius of curvature nanometer pinpoint as claimed in claim 1 is characterized in that, described equipment for producing thin film is evaporimeter, sputter, molecular beam epitaxial device or atomic layer deposition apparatus.
5. the preparation method of metal material apiculus radius of curvature nanometer pinpoint as claimed in claim 1 is characterized in that, described metal material is gold, platinum, palladium, silver, cobalt or iron.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104003351A (en) * | 2014-05-30 | 2014-08-27 | 孔祥贵 | Preparation method for nano-grade gold needle composite electrode |
| CN111089988A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | High-uniformity magnetic probe and preparation method thereof |
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| US20080098805A1 (en) * | 2004-10-06 | 2008-05-01 | Sungho Jin | Nanotube-Based Nanoprobe Structure and Method for Making the Same |
| CN101105469A (en) * | 2007-08-03 | 2008-01-16 | 厦门大学 | Nanometer ring-disc electrode preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003351A (en) * | 2014-05-30 | 2014-08-27 | 孔祥贵 | Preparation method for nano-grade gold needle composite electrode |
| CN111089988A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | High-uniformity magnetic probe and preparation method thereof |
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Application publication date: 20130403 |