CN113376406A - Preparation method of carbon nanotube probe - Google Patents
Preparation method of carbon nanotube probe Download PDFInfo
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- CN113376406A CN113376406A CN202110464872.3A CN202110464872A CN113376406A CN 113376406 A CN113376406 A CN 113376406A CN 202110464872 A CN202110464872 A CN 202110464872A CN 113376406 A CN113376406 A CN 113376406A
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- 239000000523 sample Substances 0.000 title claims abstract description 118
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 68
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 84
- 238000012545 processing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 18
- 238000003754 machining Methods 0.000 claims description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 230000009977 dual effect Effects 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- CKHJYUSOUQDYEN-UHFFFAOYSA-N gallium(3+) Chemical compound [Ga+3] CKHJYUSOUQDYEN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 14
- 238000000089 atomic force micrograph Methods 0.000 description 4
- 238000003384 imaging method Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004621 scanning probe microscopy Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of a carbon nano tube probe, which comprises the following steps: 1) growing a carbon nanotube bundle at the tip of a scanning probe microscope probe; 2) and processing the probe with the carbon nanotube bundle by using a focused ion beam system to obtain a slender carbon nanotube tip. The invention can obtain the probe of the scanning probe microscope with larger major diameter ratio, and has high-precision measurement capability on the measurement of the complex fine structure with high aspect ratio.
Description
Technical Field
The invention belongs to the technical field of micro-nano manufacturing and measuring, and particularly relates to a preparation method of a carbon nano tube probe.
Background
With the continuous development of the application fields of aerospace, integrated circuits, micro-nano sensing and the like, the measurement requirement of a complex fine structure with a high depth-to-width ratio is continuously increased. A high aspect ratio complex microstructure generally refers to a micro-nano structure with a width of micro-nano scale and a depth of micro-nano scale, and has the characteristics of vertical sidewalls and narrow gaps. In the depth direction, it is difficult to perform accurate measurement, and the measurement is used to ensure the processing, and the precision is usually at least an order of magnitude higher than that of the processing, so if there is no advanced measurement means to ensure or check the processed three-dimensional microstructure, the processing will not be standard and can be followed, and it is difficult to develop more intensive research on the function, the purpose and the novel manufacturing process of the structure.
The current measuring methods are mainly divided into two categories, namely non-contact methods and contact methods. The measurement range of a typical non-contact optical measurement technology is limited by the wavelength of light waves, and the technology is not suitable for measuring complex curved surfaces with large concave-convex changes. The common instrument for contact measurement is a high-precision probe type contourgraph, and the transverse resolution is related to the radius of a needle point. When in measurement, the probe is contacted with the measured surface under certain pressure, so that the unit area of the measured surface bears large contact pressure, and if the hardness of the measured surface is low, the probe can scratch the measured surface, so that the method is not suitable for micro-nano surfaces processed by soft metals such as copper, aluminum and the like. In addition, most of the probes used at present are made of metal tungsten or diamond, and a reliable process is not available, so that the length-diameter ratio of the probe is large enough, and the probe cannot be used for measuring a high-aspect-ratio fine structure. In contrast, the scanning probe microscopy contact measurement method has higher resolution, but the aspect ratio of the common probe is smaller, the resolution is limited by the curvature radius of the probe tip, and the common probe generates a remarkable widening effect when the size of the sample is equivalent to the curvature radius of the probe, particularly when the aspect ratio of the sample structure is larger. It is difficult to meet the measurement requirements of high aspect ratio structures.
The carbon nano tube is a novel nano material with a special structure and the physicochemical properties of the protrusions, and has wide application prospect. The carbon nano tube is combined with the probe of the scanning probe microscope, so that the imaging performance of the atomic force microscope can be greatly improved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a carbon nano tube probe so as to meet the requirements of stability, reliability, high precision and the like of high aspect ratio fine structure measurement.
The invention is realized by adopting the following technical scheme:
a preparation method of a carbon nanotube probe comprises the following steps:
1) growing a carbon nanotube bundle at the tip of a scanning probe microscope probe;
2) and processing the probe with the carbon nanotube bundle by using a focused ion beam system to obtain a slender carbon nanotube tip.
The further improvement of the invention is that the specific implementation method of the step 1) is as follows:
and (3) placing the catalyst and the probe of the scanning probe microscope in a reactor, introducing water vapor and organic matters after reduction treatment, carrying out continuous reaction at high temperature, growing the carbon nano tube on the surface of the probe of the scanning probe microscope, and obtaining the probe with the carbon nano tube bundle growing at the tip after the reaction is finished.
A further development of the invention is that the catalyst type is K/SiO2Wherein K is Fe, Co, or Ni.
The invention is further improved in that the reduction treatment process is carried out in a reducing atmosphere by using H2Or treating for 0.5-1.5h at 800-1000 deg.C in the atmosphere of CO gas.
The invention is further improved in that the molar ratio of the water vapor to the organic matter is 2: 1 or 3: 1 and in a protective gas N2Or introducing Ar inert gas under the protection of the Ar inert gas, wherein the temperature of the continuous reaction is 600-900 ℃;
the organic matter is one or more of methane, toluene, acetylene, ethylene, ethanol or phenol.
The further improvement of the invention is that the specific implementation method of the step 2) is as follows:
fixing a probe to be processed on a sample platform of a focused ion beam dual-beam system after processing parameters are set by using the focused ion beam system, determining the working distance between the probe and the focused ion beam by adjusting the position of the sample platform, enabling the ion beam emergent direction of the focused ion beam dual-beam system to be aligned to an excess carbon nanotube bundle except for the vertical part of the tip, starting the focused ion beam system dual-beam to remove the excess carbon nanotube bundle, and processing the probe with the carbon nanotube bundle grown in the step 1) by using the focused ion beam dual-beam system to obtain the probe tip with a large length-diameter ratio.
The invention has the further improvement that the focused ion beam double-beam system firstly adopts the modes of rough machining and then finish machining to remove the redundant carbon nanotube bundle, and the energy of the ion beam and the current of the ion beam are controlled in the operation.
The invention is further improved in that the ion beam of the focused ion beam dual beam system adopts a gallium ion beam.
The invention is further improved in that the working distance between the probe and the focused ion beam dual-beam system is 10-15 mm.
The invention has the following beneficial technical effects:
the preparation method of the carbon nanotube probe can obtain the probe of a scanning probe microscope with a large long diameter ratio, and has high-precision measurement capability on the measurement of a complex fine structure with a high aspect ratio. The invention overcomes the problem that the imaging false image is easy to generate when the probe of the scanning probe microscope is used for imaging the fine structure with high depth-to-width ratio at present. The preparation method is suitable for probes of various scanning probe microscopes, the processing and real-time observation can be carried out through a double-beam system of focused ion beams, namely the double-beam system is matched with a Scanning Electron Microscope (SEM) high-multiple electron microscope, and the controllable preparation of the carbon nano tube probe can be realized.
Drawings
FIG. 1 is a scanning electron microscope image of an AFM probe used in an embodiment of the present invention.
Fig. 2 is a scanning electron microscope picture of the atomic force microscope probe tip with carbon nanotube bundles grown thereon according to an embodiment of the present invention.
FIG. 3 is a schematic diagram of a carbon nanotube probe with a large length-to-diameter ratio according to an embodiment of the present invention.
Fig. 4 is a comparison between an AFM image a of a grating structure measured by a common silicon probe and an AFM image b of a grating structure measured by a carbon nanotube probe with a large length-diameter ratio, which is obtained by a controllable preparation method in an embodiment of the present invention.
Detailed Description
The invention is further explained below with reference to the figures and examples.
The invention provides a preparation method of a carbon nano tube probe with a large length-diameter ratio for measuring a complex fine structure with a high aspect ratio, which comprises the following steps:
1) growing carbon nanotube bundle at the tip of scanning probe microscope probe
Putting the catalyst and the probe of a scanning probe microscope into a reactor, and reacting in a reducing atmosphere from H2Or treating for 0.5-1.5h in the atmosphere formed by CO gas at 800-1000 ℃. After reduction treatment, in a protective gas N2Or introducing water vapor and one or more organic matters of methane, toluene, acetylene, ethylene, ethanol or phenol under the protection of inert gases such as Ar, wherein the molar ratio of the water vapor to the organic matters is 2: 1 or 3: 1, the temperature of the continuous reaction is 600-900 ℃, the carbon nano tube grows on the surface of the probe of the scanning probe microscope, and the probe with the carbon nano tube bundle growing at the tip is obtained after the reaction is finished.
2) Focused ion beam machining
Roughly processing by using a focused ion beam system, fixing a probe to be processed on a sample stage of a focused ion beam dual-beam system, adjusting the working distance between the probe of a scanning probe microscope and the focused ion beam to be 10-15mm (working distance: the distance between an ion beam emergent end and the surface of a sample), enabling the ion beam emergent direction of the focused ion beam dual-beam system to be aligned to the redundant carbon nanotube bundle except the vertical part of the tip, setting the energy of the ion beam to be 30KeV and the ion beam to be 200 and 300pA, and starting the focused ion beam system dual-beam to remove the redundant carbon nanotube bundle. And finishing, namely setting the energy of the ion beam to be 20KeV and the ion beam current to be 100-150pA, and starting a focused ion beam system to remove the redundant carbon nanotube bundle.
Example 1
1) Growing carbon nanotube bundle at the tip of atomic force microscope probe
Mixing Ni/SiO2The catalyst was placed in reverse with the probe of the atomic force microscope as shown in FIG. 1In the reactor, in a reducing atmosphere, from H2The treatment was carried out for 0.5h in a gas atmosphere at a temperature of 800 ℃. After reduction treatment, in a protective gas N2Introducing steam and methane under protection, wherein the molar ratio of the steam to the methane is 2: 1, the temperature for the continuous reaction was 600 ℃. The carbon nanotubes grow on the surface of the probe of the atomic force microscope, and the probe with the carbon nanotube bundle growing at the tip is obtained after the reaction is finished and is shown in fig. 2.
2) Focused ion beam machining
Roughly processing by utilizing a focused ion beam system, fixing a probe to be processed on a sample table of the focused ion beam dual-beam system, adjusting the working distance between the probe of a scanning probe microscope and the focused ion beam to be 10mm (working distance: the distance from an ion beam emergent end to the surface of a sample), aligning the ion beam emergent direction of the focused ion beam dual-beam system to an excessive carbon nanotube bundle except a vertical part of a tip, setting the energy of the ion beam to be 30KeV and the ion beam to be 200pA, and starting the focused ion beam system dual-beam to remove the excessive carbon nanotube bundle. The machining process and results can be observed in real time by matching with a Scanning Electron Microscope (SEM) high-magnification electron microscope, then finish machining is carried out, the energy of an ion beam is set to be 20KeV, the ion beam current is set to be 100pA, a focused ion beam dual-beam system is started to remove redundant carbon nanotube bundles, and the obtained SEM image of the carbon nanotube probe with the large length-diameter ratio is shown in figure 3. Fig. 4 is a performance test of the carbon nanotube probe prepared by the present invention, fig. 4a is an AFM image of a grating structure measured by a common silicon probe, and fig. 4b is an AFM image of a grating structure measured by a carbon nanotube probe prepared by the present invention.
1) Growing carbon nanotube bundle at the tip of atomic force microscope probe
Mixing Fe/SiO2The catalyst and the probe of the atomic force microscope as shown in FIG. 1 are placed in a reactor and reacted in a reducing atmosphere with H2Treating for 1h in an atmosphere of gas at 900 deg.C. After reduction treatment, in a protective gas N2Introducing steam and methane under protection, wherein the molar ratio of the steam to the methane is 2: 1, the temperature for the continuous reaction was 600 ℃. Growing carbon nanotube on the probe surface of atomic force microscope, and finishing the reactionThe probe with the carbon nanotube bundle growing on the tip is obtained as shown in FIG. 2.
2) Focused ion beam machining
The method comprises the steps of firstly carrying out rough machining by using a focused ion beam system, fixing a probe to be processed on a sample table of the focused ion beam dual-beam system, adjusting the working distance between the probe of a scanning probe microscope and a focused ion beam to be 12mm (working distance: the distance from an ion beam emergent end to the surface of a sample), enabling the ion beam emergent direction of the focused ion beam dual-beam system to be aligned to an excessive carbon nanotube bundle except a vertical part of a tip, setting the energy of the ion beam to be 30KeV and the ion beam to be 250pA, and starting the focused ion beam system dual-beam to remove the excessive carbon nanotube bundle. The machining process and results can be observed in real time by matching with a Scanning Electron Microscope (SEM) high-magnification electron microscope, then finish machining is carried out, the energy of an ion beam is set to be 20KeV, the ion beam current is set to be 120pA, a focused ion beam dual-beam system is started to remove redundant carbon nanotube bundles, and the obtained SEM image of the carbon nanotube probe with the large length-diameter ratio is shown in figure 3.
Example 3
1) Growing carbon nanotube bundles at the tip of an electrostatic force microscope probe
Mixing Co/SiO2The catalyst and the probe of the electrostatic force microscope are placed in a reactor and treated for 1.5h under the atmosphere formed by reducing atmosphere CO gas, and the temperature is 1000 ℃. After reduction treatment, in a protective gas N2Under the protection of (2), introducing water vapor and acetylene, wherein the molar ratio of the water vapor to the acetylene is 3: 1. the temperature for the duration of the reaction was 900 ℃. The carbon nano tube grows on the surface of the probe of the electrostatic force microscope, and the probe with the carbon nano tube bundle growing at the tip is obtained after the reaction is finished.
2) Focused ion beam machining
Roughly processing by utilizing a focused ion beam system, fixing a probe to be processed on a sample table of a focused ion beam double-beam system, adjusting the working distance between the probe of a scanning probe microscope and the focused ion beam to be 10-15mm (working distance: the distance between an ion beam emergent end and the surface of a sample), aligning the ion beam emergent direction of the focused ion beam double-beam system to the redundant carbon nanotube bundle except the vertical part of the tip, setting the energy of the ion beam to be 30KeV and the ion beam to be 300pA, and starting the focused ion beam system double-beam to remove the redundant carbon nanotube bundle. The machining process and the results can be observed in real time by matching with a Scanning Electron Microscope (SEM) high-multiple electron microscope, then finish machining is carried out, the energy of an ion beam is set to be 20KeV, the ion beam current is set to be 150pA, a focused ion beam double-beam system is started to remove redundant carbon nanotube bundles, and the carbon nanotube probe with the large length-diameter ratio is obtained.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A preparation method of a carbon nanotube probe is characterized by comprising the following steps:
1) growing a carbon nanotube bundle at the tip of a scanning probe microscope probe;
2) and processing the probe with the carbon nanotube bundle by using a focused ion beam system to obtain a slender carbon nanotube tip.
2. The method for preparing a carbon nanotube probe according to claim 1, wherein the step 1) is implemented by the following steps:
and (3) placing the catalyst and the probe of the scanning probe microscope in a reactor, introducing water vapor and organic matters after reduction treatment, carrying out continuous reaction at high temperature, growing the carbon nano tube on the surface of the probe of the scanning probe microscope, and obtaining the probe with the carbon nano tube bundle growing at the tip after the reaction is finished.
3. The method of claim 2, wherein the catalyst is K/SiO2Wherein K is Fe, Co, or Ni.
4. The method of claim 2, wherein the carbon nanotube probe is prepared by a method comprisingIn that the reduction treatment is carried out in a reducing atmosphere from H2Or treating for 0.5-1.5h at 800-1000 deg.C in the atmosphere of CO gas.
5. The method of claim 2, wherein the molar ratio of water vapor to organic substance is 2: 1 or 3: 1 and in a protective gas N2Or introducing Ar inert gas under the protection of the Ar inert gas, wherein the temperature of the continuous reaction is 600-900 ℃;
the organic matter is one or more of methane, toluene, acetylene, ethylene, ethanol or phenol.
6. The method for preparing a carbon nanotube probe according to claim 2, wherein the step 2) is implemented by the following steps:
fixing a probe to be processed on a sample platform of a focused ion beam dual-beam system after processing parameters are set by using the focused ion beam system, determining the working distance between the probe and the focused ion beam by adjusting the position of the sample platform, enabling the ion beam emergent direction of the focused ion beam dual-beam system to be aligned to an excess carbon nanotube bundle except for the vertical part of the tip, starting the focused ion beam system dual-beam to remove the excess carbon nanotube bundle, and processing the probe with the carbon nanotube bundle grown in the step 1) by using the focused ion beam dual-beam system to obtain the probe tip with a large length-diameter ratio.
7. The method as claimed in claim 6, wherein the focused ion beam dual beam system removes the excess carbon nanotube bundles by rough machining and then finish machining, and the energy of the ion beam and the current of the ion beam are controlled during the operation.
8. The method of claim 6, wherein the ion beam of the focused ion beam dual beam system is a gallium ion beam.
9. The method as claimed in claim 6, wherein the working distance between the probe and the focused ion beam dual beam system is 10-15 mm.
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PCT/CN2021/098451 WO2022227230A1 (en) | 2021-04-28 | 2021-06-04 | Preparation method for carbon nanotube probe |
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