CN114217097B - Preparation method of graphene functionalized silicon-based probe - Google Patents
Preparation method of graphene functionalized silicon-based probe Download PDFInfo
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- CN114217097B CN114217097B CN202111401739.XA CN202111401739A CN114217097B CN 114217097 B CN114217097 B CN 114217097B CN 202111401739 A CN202111401739 A CN 202111401739A CN 114217097 B CN114217097 B CN 114217097B
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- 239000000523 sample Substances 0.000 title claims abstract description 117
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000010703 silicon Substances 0.000 title claims abstract description 75
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 75
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 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 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 238000007747 plating Methods 0.000 claims abstract description 19
- 239000002608 ionic liquid Substances 0.000 claims abstract description 16
- 238000010791 quenching Methods 0.000 claims abstract description 16
- 230000000171 quenching effect Effects 0.000 claims abstract description 16
- 238000003763 carbonization Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 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 6
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 17
- 230000005540 biological transmission Effects 0.000 description 8
- 238000001000 micrograph Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000001755 magnetron sputter deposition Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000000149 penetrating effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000000313 electron-beam-induced deposition Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000010408 film Substances 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
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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 functional silicon-based probe provided by the invention, the ionic liquid is adopted to carry out carbonization pretreatment on a probe sample, a carbon layer plated on the surface of the probe in advance is utilized to protect the silicon-based probe tip, and in the high-temperature quenching process of graphene growth, the reaction between a metal plating layer and the silicon-based probe is effectively avoided, so that the graphene successfully grows on the surface of the probe, the appearance of the probe tip is maintained, the surface of the probe tip is smooth, and the diameter of the probe tip is kept in a nano size. The graphene functional silicon-based probe prepared by the method has excellent needle tip sharpness, conductivity and oxidation resistance.
Description
Technical Field
The invention relates to a functional material, in particular to a preparation method of a graphene functionalized silicon-based probe.
Background
In recent years, graphene has attracted considerable attention worldwide due to its excellent physicochemical properties, including optical properties, electrical properties, and thermal properties. After extensive exploration of the performance and potential applications of graphene, 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 by which high quality graphene films can be grown on metal or dielectric substrates, such as redox methods, epitaxial growth methods, and Chemical Vapor Deposition (CVD). Among them, CVD is the most commonly used method for synthesizing graphene thin films at present. The method has the main advantages that high-quality graphene with controllable layer number can be obtained, but the practical application is considered, and meanwhile, some limitations still exist. Synthetic methods based on CVD processes still require heating the sample for a relatively long time, are prone to damage to the nano-sized tips, and are not suitable for growing graphene on high curvature surfaces.
Disclosure of Invention
In practice, the inventor finds that the probe tip structure is easy to damage in the preparation process of the graphene functional silicon-based probe, and the main reason is that a Ni layer or other catalytic metal plating layer on the surface of the Si probe is easy to react with Si at high temperature so as to damage the probe tip structure. In order to solve the problem, the inventor firstly coats a layer of carbon on the silicon-based probe and then coats a layer of metal on the silicon-based probe, wherein the carbon layer is used for protecting the silicon-based probe, so that the damage to the needle tip caused by the reaction between 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-methylimidazole acetate ionic liquid; under the catalysis of the metal element, the surface of the silicon-based probe is subjected to carbonization reaction to form a metal carbide shell structure;
3) Quenching the silicon-based probe treated in the step 2); and obtaining the graphene functional silicon-based probe.
Preferably, in step 1), the silicon-based probes include silicon-based AFM probes, silicon-based array probes, silicon-based OLED probes, and the like, specifically, for example, silicon-based AFM probes.
Preferably, in step 1), the metal is selected from one or a combination of several of Ni (nickel), pt, cu, au, etc., more preferably Ni.
Preferably, in step 1), the thickness of the carbon layer is 3nm to 20nm, more preferably 5nm to 10nm; the thickness of the metal plating layer is 25nm to 100nm, more preferably 16nm to 50nm. The research shows that the silicon-based probe can be protected in the thickness range of the carbon layer and the metal coating, and the graphene can be successfully grown on the surface of the silicon-based probe. If the plating layer is not appropriate in thickness, graphene is difficult to grow on the surface of the probe.
Among them, the conventional plating method in the art, such as magnetron sputtering, electron beam deposition and vacuum evaporation, can be used in step 1).
Preferably, in step 2), the depth of the ion liquid which penetrates through the silicon-based probe tip is 500 um-2 mm, such as 1mm; thus, the probe tip can be ensured to fully react with the ionic liquid.
Preferably, in step 2), the ionic liquid has a temperature of 200 ℃ to 350 ℃, more preferably 180 ℃ to 250 ℃; preferably, the carbonization reaction is carried out for 15min to 60min, more preferably 25min to 60min.
Preferably, the quenching treatment in step 3) is performed by raising the temperature of the silicon-based probe to 800-1500 c, more preferably 1050-1100 c, within 0.1 s-10 s, and then immediately cooling.
In some embodiments, the quenching treatment in step 3) is performed by raising the temperature of the silicon-based probe to 1050-1100 ℃ within 0.16s-0.50s, followed by immediate cooling.
The research shows that after carbon plating and metal plating, the silicon-based probe forms a metal carbide shell structure in the ionic liquid, and then the metal carbide shell structure is subjected to ultrafast quenching treatment, so that the damage of the silicon-based probe is avoided, the morphology of the probe tip is maintained, and the graphene functionalized silicon-based probe with high quality can be successfully prepared.
Preferably, in step 3) the quenching treatment is performed in a vacuum or inert atmosphere.
Preferably, in step 3), the quenching treatment method includes a pulse current quenching method, an induced 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 of 5 nm-10 nm; plating metal on the carbon layer to form a metal plating layer with the thickness of 16 nm-50 nm; the metal is nickel;
2) Immersing the silicon-based probe treated in the step 1) into 1-butyl-3-methylimidazole acetate ionic liquid at 180-250 ℃; under the catalysis of the metal element, the surface of the silicon-based probe is subjected to carbonization reaction to form a metal carbide shell structure; the carbonization reaction time is 25min-60min;
3) Raising the silicon-based probe treated in the step 2) to 1050-1100 ℃ within 0.1-10 s, and then immediately cooling; and obtaining the graphene functional silicon-based probe.
The invention also comprises the graphene functional silicon-based probe prepared by the method.
According to the graphene functional silicon-based probe provided by the invention, the ionic liquid is adopted to carry out carbonization pretreatment on a probe sample, a carbon layer plated on the surface of the probe in advance is utilized to protect the silicon-based probe tip, and in the high-temperature quenching process of graphene growth, the reaction between a metal plating layer and the silicon-based probe is effectively avoided, so that the graphene successfully grows on the surface of the probe, the appearance of the probe tip is maintained, the surface of the probe tip is smooth, and the diameter of the probe tip is kept in a nano size. The graphene functionalized nano 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 microscope image of a silicon-based AFM probe coated with a carbon layer according to example 1.
FIG. 3 is a transmission electron microscope image of a nickel plated silicon-based AFM probe 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 thereof.
Comparative example 1
And plating a nickel layer with the thickness of 25nm plus or minus 5nm on the surface of the silicon-based AFM probe by utilizing a magnetron sputtering method. After coatingIs immersed in a small 10ml beaker containing 2ml of 1-butyl-3-methylimidazole acetate ionic liquid. The depth of the ion liquid which is used for penetrating through the tip of the silicon-based probe is about 1mm; the ionic liquid was heated to 250 ℃ with an electric hot plate for 25min at 250 ℃. Taking out the carbonized probe, and heating at 6.4X10 by microwave -6 The probe is quenched in a vacuum chamber of hPa. Quenching temperature is 1050 ℃, quenching time is 0.16s, and natural cooling is carried out. After the sample has cooled, the silicon-based AFM probe is removed and its Transmission Electron Microscope (TEM) image is shown in FIG. 1. As can be seen from fig. 1 (a), the surface of the probe is rugged, and the nickel particles with black surface react with the silicon-based probe, so that the probe morphology is damaged. As can be seen from FIG. 1 (b), the probe tip diameter is about 100nm, which is significantly larger than the tip diameter of the original silicon-based AFM probe (30 nm).
Example 1
A carbon layer with the thickness of about 5nm is firstly plated on the surface of a silicon-based AFM probe by utilizing a magnetron sputtering method, and a transmission electron microscope image is shown in figure 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-methylimidazole acetate ionic liquid. The depth of the ion liquid which is used for penetrating through the tip of the silicon-based probe is about 1mm; the ionic liquid was heated to 250 ℃ with an electric hot plate for 25min at 250 ℃. Taking out the carbonized probe, and heating at 6.4X10 by microwave -6 The probe is quenched in a vacuum chamber of hPa. The silicon-based probe was raised to 1050 ℃ within 0.16s and then cooled naturally. After the sample cooled, the silicon-based AFM probe was removed and its transmission electron microscopy image was 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 successfully grows 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 30 nm) of the original silicon-based AFM probe.
Example 2
And plating a carbon layer with the thickness of 10nm on the surface of the silicon-based AFM probe by utilizing a magnetron sputtering method, and then continuing to plate 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-methylimidazole acetate ionic liquid. The depth of the ion liquid which is used for penetrating through the tip of the silicon-based probe is about 1mm; heating the ionic liquid to 180 ℃ by using an electric heating plate, wherein the duration of 180 ℃ is 60min. Taking out the carbonized probe, and quenching the probe in a vacuum cavity of 6.4X10-6 hPa by adopting a microwave heating method. The silicon-based probe was raised to 1050 ℃ within 0.16s and cooled naturally. After the sample has cooled, the silicon-based AFM probe is removed and its transmission electron microscopy image 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 successfully grows on the surface of the probe while more amorphous carbon is present.
The above examples are only illustrative of 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 by those skilled in the art to the technical solution of the present invention should fall within the scope of protection defined by the claims of the present invention without departing from the spirit of the design of the present invention.
Claims (4)
1. The preparation method of the graphene functionalized silicon-based probe is characterized by comprising the following steps of:
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; the metal is selected from one or a combination of a plurality of Ni, pt, cu, au; the thickness of the carbon layer is 5 nm-10 nm; the thickness of the metal coating is 16 nm-50 nm;
2) Immersing the silicon-based probe treated in the step 1) in 1-butyl-3-methylimidazole acetate ionic liquid; under the catalysis of the metal element, the surface of the silicon-based probe is subjected to carbonization reaction to form a metal carbide shell structure; the depth of the ionic liquid which passes through the tip of the silicon-based probe is 500 mu m-2 mm;
3) Quenching the silicon-based probe treated in the step 2); obtaining a graphene functional silicon-based probe; the quenching treatment method is that the temperature of the silicon-based probe is raised to 1050 ℃ within 0.16 s; and then immediately cooled.
2. The method of claim 1, wherein in step 1), the silicon-based probe comprises a silicon-based AFM probe, a silicon-based array probe, or a silicon-based OLED probe.
3. The method of claim 1 or 2, wherein in step 2) the ionic liquid is at a temperature of 180-250 ℃; the carbonization reaction time is 25min-60min.
4. A graphene-functionalized silica-based probe prepared by the method of any one of claims 1-3.
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