CN114217097A - Preparation method of graphene functionalized silicon-based probe - Google Patents
Preparation method of graphene functionalized silicon-based probe Download PDFInfo
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- CN114217097A CN114217097A CN202111401739.XA CN202111401739A CN114217097A CN 114217097 A CN114217097 A CN 114217097A CN 202111401739 A CN202111401739 A CN 202111401739A CN 114217097 A CN114217097 A CN 114217097A
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- 239000000523 sample Substances 0.000 title claims abstract description 125
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 83
- 239000010703 silicon Substances 0.000 title claims abstract description 83
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000002608 ionic liquid Substances 0.000 claims abstract description 21
- 238000010791 quenching Methods 0.000 claims abstract description 17
- 230000000171 quenching effect Effects 0.000 claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 238000007747 plating Methods 0.000 claims description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 20
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- BSKSXTBYXTZWFI-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;acetate Chemical compound CC([O-])=O.CCCC[N+]=1C=CN(C)C=1 BSKSXTBYXTZWFI-UHFFFAOYSA-M 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- HCGMDEACZUKNDY-UHFFFAOYSA-N 1-butyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCCCN1CN(C)C=C1 HCGMDEACZUKNDY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 239000000956 alloy Substances 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 7
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001755 magnetron sputter deposition Methods 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000000313 electron-beam-induced deposition Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
- G01Q60/38—Probes, their manufacture, or their related instrumentation, e.g. holders
- G01Q60/42—Functionalisation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q70/00—General aspects of SPM probes, their manufacture or their related instrumentation, insofar as they are not specially adapted to a single SPM technique covered by group G01Q60/00
- G01Q70/16—Probe manufacture
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q70/00—General aspects of SPM probes, their manufacture or their related instrumentation, insofar as they are not specially adapted to a single SPM technique covered by group G01Q60/00
- G01Q70/16—Probe manufacture
- G01Q70/18—Functionalisation
Abstract
The invention provides a preparation method of a graphene functionalized silicon-based probe. According to the graphene functionalized silicon-based probe provided by the invention, the probe sample is subjected to carbonization pretreatment by adopting the ionic liquid, the silicon-based probe tip is protected by utilizing the carbon layer plated on the surface of the probe in advance, and the reaction between the metal coating and the silicon-based probe is effectively avoided in the high-temperature quenching process of graphene growth, so that the morphology of the probe tip is maintained while the graphene successfully grows on the surface of the probe, the surface of the probe tip is smooth, and the diameter of the probe tip keeps a nanometer size. The graphene functionalized silicon-based probe prepared by the method disclosed by the invention has excellent needle point sharpness, conductivity and oxidation resistance.
Description
Technical Field
The invention relates to a functional material, in particular to a preparation method of a graphene functional silicon-based probe.
Background
In recent years, graphene has attracted great attention worldwide due to its excellent physicochemical properties, including optical properties, electrical properties, and thermal properties. After extensive exploration on the performance and potential applications of graphene, the emphasis of graphene research is currently focused on realizing practical applications of graphene materials, including probes, transparent electrodes, sensors, field effect transistors, electromagnetic attenuation materials, and the like. There are several methods to grow high quality graphene thin films on metal or dielectric substrates, such as redox, epitaxial growth, and Chemical Vapor Deposition (CVD). Among them, CVD is currently the most commonly used method for synthesizing graphene thin films. The main advantage is that high-quality graphene with controllable layer number can be obtained, but there are some limitations while considering practical application. The synthesis method based on the CVD process still requires a relatively long time for heating the sample, easily causes damage to the nano-sized needle tip, and is not suitable for growing graphene on a high curvature surface.
Disclosure of Invention
The inventor finds in practice that the probe tip structure is easily damaged in the preparation process of the graphene functionalized silicon-based probe, and the main reason is that the Ni layer or other catalytic metal plating on the surface of the Si probe is easily reacted with Si at high temperature to damage the probe tip structure. Aiming at the problem, the inventor plates a layer of carbon on the silicon-based probe firstly and then plates a layer of metal, and the carbon layer is used for protecting the silicon-based probe, so that the damage of a needle point caused by the reaction of the silicon-based probe and the metal coating can be avoided.
Specifically, the invention provides a preparation method of a graphene functionalized silicon-based probe, which comprises the following steps:
1) firstly, plating carbon on a silicon-based probe to form a carbon layer; plating metal on the carbon layer to form a metal plating layer;
2) immersing the silicon-based probe treated in the step 1) in 1-butyl-3-methylimidazolium acetate ionic liquid; under the catalytic action of the metal element, the surface of the silicon-based probe is subjected to a carbonization reaction to form a metal carbide shell structure;
3) quenching the silicon-based probe processed in the step 2); and obtaining the graphene functionalized silicon-based probe.
Preferably, in step 1), the silicon-based probe includes a silicon-based AFM probe, a silicon-based array probe, a silicon-based OLED probe, and the like, specifically, the silicon-based AFM probe.
Preferably, in step 1), the metal is selected from one or a combination of several of Ni (nickel), Pt, Cu, Au, and the like, and more preferably Ni.
Preferably, in step 1), the carbon layer has a thickness of 3nm to 20nm, more preferably 5nm to 10 nm; the thickness of the metal plating layer is 25nm to 100nm, and more preferably 16nm to 50 nm. Researches find that the carbon layer and the metal coating can protect the silicon-based probe within the thickness range, and graphene can successfully grow on the surface of the silicon-based probe. If the thickness of the plating layer is not proper, graphene is difficult to grow on the surface of the probe.
Among them, the step 1) may employ a conventional plating method in the art, such as magnetron sputtering, electron beam deposition, and vacuum evaporation.
Preferably, in the step 2), the depth of the ionic liquid passing through the tip of the silicon-based probe is 500 um-2 mm, such as 1 mm; thus, the probe tip can be ensured to be fully reacted with the ionic liquid.
Preferably, in step 2), the temperature of the ionic liquid is 200 ℃ to 350 ℃, more preferably 180 ℃ to 250 ℃; the carbonization reaction time is preferably 15min to 60min, more preferably 25min to 60 min.
Preferably, the quenching treatment in step 3) is carried out by raising the temperature of the silicon-based probe to 800-1500 ℃ within 0.1-10 s, more preferably 1050-.
In some embodiments, the quenching process in step 3) is performed by raising the temperature of the silicon-based probe to 1050-.
Researches show that after the silicon-based probe is subjected to carbon plating and metal plating, a metal carbide shell structure is formed in the ionic liquid, and then the silicon-based probe is subjected to ultra-fast quenching treatment, so that the damage of the silicon-based probe is avoided, the shape of the probe tip can be maintained, and the high-quality graphene functionalized silicon-based probe can be successfully prepared.
Preferably, the quenching treatment in step 3) is performed in vacuum or inert atmosphere.
Preferably, in step 3), the quenching process includes a pulse current quenching method, an induction current quenching method, or a microwave quenching method.
Preferably, the preparation method of the graphene-functionalized silicon-based probe comprises the following steps:
1) firstly plating carbon on a silicon-based probe to form a carbon layer with the thickness of 5 nm-10 nm; plating metal on the carbon layer to form a metal plating layer of 16-50 nm; the metal is nickel;
2) immersing the silicon-based probe treated in the step 1) in 1-butyl-3-methylimidazole acetate ionic liquid at the temperature of 180 ℃ and 250 ℃; under the catalytic action of the metal element, the surface of the silicon-based probe is subjected to a carbonization reaction to form a metal carbide shell structure; the carbonization reaction time is 25min-60 min;
3) raising the temperature of the silicon-based probe treated in the step 2) to 1050-; and obtaining the graphene functionalized silicon-based probe.
The invention also discloses the graphene functionalized silicon-based probe prepared by the method.
According to the graphene functionalized silicon-based probe provided by the invention, the probe sample is subjected to carbonization pretreatment by adopting the ionic liquid, the silicon-based probe tip is protected by utilizing the carbon layer plated on the surface of the probe in advance, and the reaction between the metal coating and the silicon-based probe is effectively avoided in the high-temperature quenching process of graphene growth, so that the morphology of the probe tip is maintained while the graphene successfully grows on the surface of the probe, the surface of the probe tip is smooth, and the diameter of the probe tip keeps a nanometer size. The graphene functionalized nanometer needle tip prepared by the method has excellent needle tip sharpness, conductivity and oxidation resistance.
Drawings
FIG. 1 is a transmission electron microscope image of a silicon-based AFM probe prepared by the method of comparative example 1.
FIG. 2 is a transmission electron micrograph of a carbon coated silicon based AFM probe of example 1.
FIG. 3 is a transmission electron micrograph of a silicon-based AFM probe plated with nickel layer of example 1.
FIG. 4 is a transmission electron microscope image of a silicon-based AFM probe prepared by the method of example 1.
FIG. 5 is a transmission electron microscope image of a silicon-based AFM probe prepared by the method of example 2.
Detailed Description
The following examples illustrate the invention but are not intended to limit the scope of the invention.
Comparative example 1
And plating a nickel layer with the thickness of 25nm +/-5 nm on the surface of the silicon-based AFM probe by using a magnetron sputtering method. The coated AFM probe was immersed in a 10ml small beaker containing 2ml of 1-butyl-3-methylimidazolium acetate ionic liquid. The depth of the ionic liquid submerging the tip of the silicon-based probe is about 1 mm; the ionic liquid is heated to 250 ℃ by an electric heating plate, and the duration of 250 ℃ is 25 min. Taking out the carbonized probe, and heating by microwave at 6.4 × 10-6And quenching the probe in a vacuum cavity of hPa. The quenching temperature is 1050 ℃, the quenching time is 0.16s, and the steel plate is naturally cooled. After the sample was cooled, the silicon-based AFM probe was removed and its Transmission Electron Microscopy (TEM) image is shown in FIG. 1. As can be seen from fig. 1 (a), the probe has uneven surface, and the nickel particles with black surface react with the silicon-based probe, so that the morphology of the probe is damaged. It can be seen from FIG. 1 (b) that the probe tip diameter is around 100nm, which is significantly larger than the tip diameter (30 nm) of the original silicon-based AFM probe.
Example 1
A magnetron sputtering method is utilized to plate a carbon layer with the thickness of about 5nm on the surface of the silicon-based AFM probe, and a transmission electron microscope image is shown in FIG. 2. Then, a nickel layer with the thickness of about 16nm is plated on the surface of the carbon layer, and a transmission electron microscope image is shown in FIG. 3. The coated AFM probe was immersed in a 10ml small beaker containing 2ml of 1-butyl-3-methylimidazolium acetate ionic liquid. The depth of the ionic liquid submerging the tip of the silicon-based probe is about 1 mm; the ionic liquid is heated to 250 ℃ by an electric heating plate, and the duration of 250 ℃ is 25 min. Taking out the carbonized probe, and heating by microwave at 6.4 × 10-6Quenching part of probe in vacuum cavity of hPaAnd (6) processing. The silicon-based probe was raised to 1050 ℃ in 0.16s and then allowed to cool naturally. And after the sample is cooled, taking out the silicon-based AFM probe, wherein a transmission electron microscope image of the silicon-based AFM probe is shown in FIG. 4. As can be seen from fig. 4 (a), the probe surface is relatively flat, and the tapered shape of the silicon-based probe remains intact. From FIG. 4 (b), it can be seen that graphene is successfully grown on the surface of the probe, and the diameter of the tip of the probe is about 40nm, which is equivalent to the tip diameter (about 30nm) of the original silicon-based AFM probe.
Example 2
Firstly plating a carbon layer with the thickness of 10nm on the surface of the silicon-based AFM probe by using a magnetron sputtering method, and then continuously plating a nickel layer with the thickness of 50nm on the surface of the carbon layer. The coated AFM probe was immersed in a 10ml small beaker containing 2ml of 1-butyl-3-methylimidazolium acetate ionic liquid. The depth of the ionic liquid submerging the tip of the silicon-based probe is about 1 mm; the ionic liquid is heated to 180 ℃ by an electric heating plate, and the duration of 180 ℃ is 60 min. The carbonized probe was taken out and quenched by microwave heating in a vacuum chamber of 6.4X 10-6 hPa. The silicon-based probe was raised to 1050 ℃ in 0.16s and allowed to cool naturally. And after the sample is cooled, taking out the silicon-based AFM probe, wherein a transmission electron microscope image of the silicon-based AFM probe is shown in FIG. 5. As can be seen from fig. 5 (a), the probe surface is relatively flat, and the tapered shape of the silicon-based probe remains intact. From fig. 5 (b), it can be seen that graphene was successfully grown on the surface of the probe, and more amorphous carbon was present.
The above examples are only for describing the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. A preparation method of a graphene functionalized silicon-based probe is characterized by comprising the following steps:
1) firstly, plating carbon on a silicon-based probe to form a carbon layer; plating metal on the carbon layer to form a metal plating layer;
2) immersing the silicon-based probe treated in the step 1) in 1-butyl-3-methylimidazolium acetate ionic liquid; under the catalytic action of the metal element, the surface of the silicon-based probe is subjected to a carbonization reaction to form a metal carbide shell structure;
3) quenching the silicon-based probe processed in the step 2); and obtaining the graphene functionalized silicon-based probe.
2. The method for preparing the probe of claim 1, wherein in the step 1), the silicon-based probe comprises a silicon-based AFM probe, a silicon-based array probe and a silicon-based OLED probe.
3. The method for preparing the alloy according to claim 1 or 2, wherein in the step 1), the metal is one or more of Ni, Pt, Cu and Au.
4. The production method according to any one of claims 1 to 3, wherein in step 1), the carbon layer has a thickness of 3nm to 20 nm; the thickness of the metal coating is 25 nm-100 nm.
5. The production method according to any one of claims 1 to 4, wherein in step 1), the carbon layer has a thickness of 5nm to 10 nm; the thickness of the metal coating is 16 nm-50 nm.
6. The method according to any one of claims 1 to 5, wherein the depth of the ionic liquid over the silicon-based probe tip in step 2) is 500um to 2 mm.
7. The method according to any one of claims 1 to 6, wherein in step 2), the temperature of the ionic liquid is 200 ℃ to 350 ℃, more preferably 180 ℃ to 250 ℃; and/or the time of the carbonization reaction is 15 min-60min, preferably 25min-60 min.
8. The method as claimed in any one of claims 1 to 7, wherein the quenching treatment in step 3) is performed by raising the temperature of the silicon-based probe to 800-1500 ℃, preferably 1050-1100 ℃ within 0.1-10 s; and then immediately cooled.
9. The production method according to claim 1 or 2, characterized by comprising:
1) firstly plating carbon on a silicon-based probe to form a carbon layer with the thickness of 5 nm-10 nm; plating metal on the carbon layer to form a metal plating layer of 16-50 nm; the metal is nickel;
2) immersing the silicon-based probe treated in the step 1) in 1-butyl-3-methylimidazole acetate ionic liquid at the temperature of 180 ℃ and 250 ℃; under the catalytic action of the metal element, the surface of the silicon-based probe is subjected to a carbonization reaction to form a metal carbide shell structure; the carbonization reaction time is 25min-60 min;
3) raising the temperature of the silicon-based probe treated in the step 2) to 1050-; and obtaining the graphene functionalized silicon-based probe.
10. A graphene-functionalized silicon-based probe, characterized by being prepared by the method of any one of claims 1 to 9.
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