CN113219211B - Preparation method of nano probe - Google Patents
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- CN113219211B CN113219211B CN202110464814.0A CN202110464814A CN113219211B CN 113219211 B CN113219211 B CN 113219211B CN 202110464814 A CN202110464814 A CN 202110464814A CN 113219211 B CN113219211 B CN 113219211B
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- 239000000523 sample Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 82
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- 239000004094 surface-active agent Substances 0.000 claims abstract description 17
- CIJQGPVMMRXSQW-UHFFFAOYSA-M sodium;2-aminoacetic acid;hydroxide Chemical compound O.[Na+].NCC([O-])=O CIJQGPVMMRXSQW-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 9
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 8
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000002105 nanoparticle Substances 0.000 claims description 14
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 13
- 229910052737 gold Inorganic materials 0.000 claims description 13
- 239000010931 gold Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 6
- 239000011133 lead Substances 0.000 claims description 5
- 239000002923 metal particle Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910001385 heavy metal Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 239000000084 colloidal system Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- 239000000693 micelle Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910021514 lead(II) hydroxide Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- -1 iron oxide compound Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
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- 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 nano probe, which comprises the following steps: 1) adding a metal nanoparticle solution and a metal compound solution containing metal ions into an aminoacetic acid-sodium hydroxide solution for reaction, uniformly mixing, reacting for a period of time at a set temperature, cooling to room temperature, and washing with deionized water for several times to obtain a metal nanoparticle solution with a preset concentration; 2) firstly, mixing a surfactant P123, 1M hydrochloric acid and ethanol, adding silicon tetrachloride, stirring to form a solution, pouring the solution into an evaporation pan, and standing to obtain a semi-solid silicic acid mixed solution; adding the metal nanoparticle solution prepared in the step 1) into the semi-solid silicic acid mixed solution formed in the step 2) to obtain a mixed solution, and immersing the AFM probe into the mixed solution for a period of time and then taking out to obtain the metal nanoprobe. The probe tip ball prepared by the invention is in nano scale and is suitable for various measurement applications in nano scale.
Description
Technical Field
The invention belongs to the technical field of nano manufacturing and measurement, and particularly relates to a preparation method of a nano probe.
Background
Nanotechnology is an emerging field of scientific development in the world today, and its core is nanotechnology. The improvement of the nano processing technology level can have great influence on the technical fields of aerospace, micro-nano sensing, life science, integrated circuits and the like. The nano-machining technology cannot be separated from nano-manufacturing and nano-measurement, which are used for ensuring the machining precision, the precision is usually at least one order of magnitude higher than that of machining, otherwise the nano-machining cannot be followed by standards. It is seen that nanofabrication and measurement will play an extremely important role in the development of nanotechnology in nanofabrication. In recent years, with the development and application of Atomic Force Microscope (AFM) technology, more accurate experimental data can be obtained from experimental research in nanoscale. In the AFM colloidal probe technology developed in recent years, the surface potential and the surface charge density are obtained by measuring the force of the charged surface on the colloidal probe in the electrolyte solution. The colloid probe technology is characterized in that a micron-sized microsphere is bonded to the tail end of a probe cantilever of an AFM to be used as a sensor, and the measurement of the interfacial interaction force is realized. The AFM colloid probe technology is an effective means for exploring the influence of surface charge in the nanoscale measurement of electrostatic interaction. However, the colloidal probe has a size of 1-10 microns, the test precision is limited, and the measurement on a nanometer scale is lacked. Meanwhile, the colloid probe is pasted through glue, the pasting position of the colloid probe is difficult to control and influence the accuracy, and the colloid probe is easy to fall off when meeting high temperature or liquid.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a nanoprobe.
The invention is realized by adopting the following technical scheme:
a preparation method of a nano probe is provided, the method obtains the nano probe by attaching metal nano particles to the tip of an AFM microscope probe, and the method specifically comprises the following implementation steps:
1) preparation of Metal nanoparticle solution
Adding a metal nanoparticle solution and a metal compound solution containing metal ions into an aminoacetic acid-sodium hydroxide solution for reaction, uniformly mixing, reacting for a period of time at a set temperature, cooling to room temperature, and washing with deionized water for several times to obtain a metal nanoparticle solution with a preset concentration;
2) assembling metal nanoparticles at AFM probe tip
Firstly, mixing a surfactant P123, 1M hydrochloric acid and ethanol, adding silicon tetrachloride, stirring to form a solution, pouring the solution into an evaporation pan, and standing to obtain a semi-solid silicic acid mixed solution; adding the metal nanoparticle solution prepared in the step 1) into the semi-solid silicic acid mixed solution formed in the step 2) to obtain a mixed solution, and immersing the AFM probe into the mixed solution for a period of time and then taking out to obtain the metal nanoprobe.
The further improvement of the invention is that in the step 1), the concentration of the metal nanoparticle solution is 120-150pM, and silver nanoparticles or gold nanoparticles are selected.
The invention further improves that in the step 1), the type of the metal particles is selected from one of copper, lead, zinc, iron, cobalt and nickel in the heavy metal particles, and the concentration is 3-5 mu M.
In a further development of the invention, in step 1), the concentration of glycine-sodium hydroxide is 3 to 5 mM.
The further improvement of the invention is that in the step 1), the volume ratio of the metal nanoparticle solution, the metal ion solution and the glycine-sodium hydroxide solution is (3-5): (1-1.5): (1-1.5).
The further improvement of the invention is that in the step 1), the reaction temperature is 160-200 ℃, and the reaction time is 5-10 h.
The further improvement of the invention is that in the step 2), the volume ratio of the surfactant P123, the 1M hydrochloric acid and the ethanol is 1 (0.2-0.5) to (2-5): (0.5-1.5).
The further improvement of the invention is that in the step 2), the solution is poured into an evaporating dish and then stands for 12-24 hours.
The further improvement of the invention is that in the step 2), the AFM probe is immersed into the mixed solution for 15-30min and then taken out to obtain the metal nano probe.
The invention has the following beneficial technical effects:
according to the preparation method of the nano probe, provided by the invention, the interface in the nano-to-micron scale range is accurately measured, the scale vacancy is filled, the surface potential and the surface charge density can be measured, and the important technical bottleneck in the field of nano tribology is solved. In the prior art, a small ball at the tip of a spherical probe is in a micron scale, while a small ball at the probe tip prepared by the invention is in a nanometer scale, so that the probe in the invention is more suitable for various measurement applications in the nanometer scale.
Drawings
Fig. 1 is a scanning electron microscope image of a conventional colloidal probe.
FIG. 2 is a scanning electron microscope image of an AFM probe used in an embodiment of the present invention.
Fig. 3 is a scanning electron microscope picture of an atomic force microscope probe tip with gold nanoparticles grown thereon according to 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 nano probe. The method comprises the following specific steps:
1) preparation of Metal nanoparticle solution
The gold or silver nanoparticle solution of 120-150pM (M is mol/L) and the metal compound solution containing heavy metal particles such as copper, lead, zinc, iron, cobalt and nickel are added into the glycine-sodium hydroxide solution with the concentration of 3-5mM for reaction, wherein the concentration of the metal compound solution is 3-5 mu M. Mixing the metal nano particle solution, the metal ion solution and the glycine-sodium hydroxide solution according to the volume ratio of (3-5) to (1-1.5). After being mixed evenly, the mixture reacts for 5 to 10 hours at the temperature of 160-200 ℃, then is cooled to room temperature, and is washed for a plurality of times by deionized water, thus obtaining the metal nano particle solution with certain concentration.
2) Assembling metal nanoparticles at AFM probe tip
Firstly, mixing a surfactant P123, 1M hydrochloric acid and ethanol according to a certain volume ratio, wherein the ratio of the surfactant P123 to the 1M hydrochloric acid to the ethanol to silicon tetrachloride is 1 (0.2-0.5) to 2-5): 0.5-1.5, and preparing 200-500mL of solution. Pouring the solution into an evaporating dish, standing for 12-24h, and volatilizing the micelle formed by the surfactant along with the ethanol. Adding the solution prepared in the step 1) into the solution formed in the step 2) to obtain a mixed solution. And (4) immersing the AFM probe into the mixed solution for 15-30min, and taking out to obtain the metal nano probe.
Example 1
1) Preparation of gold nanoparticle solution
A120 pM solution of gold nanoparticles and a solution of an iron oxide compound containing iron particles at a concentration of 3. mu.M were added to a 3mM glycine-sodium hydroxide solution to effect a reaction. And mixing the gold nanoparticle solution, the ferric oxide solution and the glycine-sodium hydroxide solution according to the volume ratio of 3:1: 1. After being mixed evenly, the mixture reacts for 5 hours at the temperature of 160 ℃, then is cooled to room temperature, and is washed for a plurality of times by deionized water, thus obtaining the gold nano particle solution with certain concentration.
2) Assembling gold nanoparticles at AFM probe tip
Fig. 1 is an SEM image of a general colloid probe, and fig. 2 is a probe of AFM. Firstly, mixing a surfactant P123, 1M hydrochloric acid and ethanol according to a certain volume ratio, wherein the ratio of the surfactant P123 to the 1M hydrochloric acid to the ethanol to silicon tetrachloride is 1:0.2:2:0.5, and preparing 200mL of solution. Pouring the solution into an evaporating dish, and standing for 12h, wherein the micelle formed by the surfactant volatilizes along with the ethanol. Adding the solution prepared in the step 1) into the solution formed in the step 2) to obtain a mixed solution. And (3) immersing the AFM probe into the mixed solution for 15min, and taking out to obtain the gold nano probe as shown in figure 3. The nanoparticles greatly reduced the curvature half-value of the tip compared to the tip of figure 1.
Example 2
1) Preparation of gold nanoparticle solution
A135 pM solution of gold or silver nanoparticles and a lead hydroxide solution containing lead particles at a concentration of 4. mu.M were added to a glycine-sodium hydroxide solution at a concentration of 4mM to effect a reaction. Mixing the metal nanoparticle solution, the metal ion solution and the glycine-sodium hydroxide solution according to the volume ratio of 4:1.2: 1.2. After being mixed evenly, the mixture reacts for 8 hours at the temperature of 180 ℃, then is cooled to room temperature, and is washed for a plurality of times by deionized water, thus obtaining silver nano particle solution with certain concentration.
2) Assembling silver nanoparticles at AFM probe tip
Firstly, mixing a surfactant P123, 1M hydrochloric acid and ethanol according to a certain volume ratio, wherein the ratio of the surfactant P123 to the 1M hydrochloric acid to the ethanol to the silicon tetrachloride is 1:0.3: 3:1, prepare 300mL of solution. Pouring the solution into an evaporating dish, standing for 18h, and volatilizing the micelle formed by the surfactant along with the ethanol. Adding the solution prepared in the step 1) into the solution formed in the step 2) to obtain a mixed solution. And (4) immersing the AFM probe into the mixed solution for 25min, and taking out to obtain the silver nano probe.
Example 3
1) Preparation of silver nanoparticle solution
A150 pM solution of gold or silver nanoparticles and a lead hydroxide solution containing lead particles at a concentration of 5. mu.M were added to a glycine-sodium hydroxide solution at a concentration of 5mM to effect a reaction. Mixing the metal nanoparticle solution, the metal ion solution and the glycine-sodium hydroxide solution according to the volume ratio of 5:1.5: 1.5. After being mixed evenly, the mixture reacts for 10 hours at the temperature of 200 ℃, then is cooled to room temperature, and is washed for a plurality of times by deionized water, thus obtaining silver nano particle solution with certain concentration.
2) Assembling silver nanoparticles at AFM probe tip
Firstly, mixing a surfactant P123, 1M hydrochloric acid and ethanol according to a certain volume ratio, wherein the ratio of the surfactant P123 to the 1M hydrochloric acid to the ethanol to silicon tetrachloride is 1:0.5: 5:1.5, prepare 300mL of solution. Pouring the solution into an evaporating dish, standing for 24h, and volatilizing the micelle formed by the surfactant along with the ethanol. Adding the solution prepared in the step 1) into the solution formed in the step 2) to obtain a mixed solution. And (4) immersing the AFM probe into the mixed solution for 30min, and taking out to obtain the silver nano probe.
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 nano probe is characterized in that the nano probe is obtained by attaching metal nano particles to the tip of an AFM microscope probe, and the method specifically comprises the following implementation steps:
1) preparation of Metal nanoparticle solution
Adding a metal nanoparticle solution and a metal compound solution containing metal ions into an aminoacetic acid-sodium hydroxide solution for reaction, uniformly mixing, reacting for a period of time at a set temperature, cooling to room temperature, and washing with deionized water for several times to obtain a metal nanoparticle solution with a preset concentration;
2) assembling metal nanoparticles at AFM probe tip
Firstly, mixing a surfactant P123, 1M hydrochloric acid and ethanol, adding silicon tetrachloride, stirring to form a solution, pouring the solution into an evaporation pan, and standing to obtain a semi-solid silicic acid mixed solution; adding the metal nanoparticle solution prepared in the step 1) into the semi-solid silicic acid mixed solution formed in the step 2) to obtain a mixed solution, and immersing the AFM probe into the mixed solution for a period of time and then taking out to obtain the metal nanoprobe.
2. The method as claimed in claim 1, wherein the concentration of the metal nanoparticle solution in step 1) is 120-150pM, and the silver nanoparticles or the gold nanoparticles are selected.
3. The method for preparing a nanoprobe according to claim 1, wherein in the step 1), the type of the metal particle is selected from one of copper, lead, zinc, iron, cobalt and nickel in the heavy metal particle, and the concentration is 3-5 μ M.
4. The method for preparing a nanoprobe according to claim 1, wherein the concentration of glycine-sodium hydroxide in step 1) is 3-5 mM.
5. The method as claimed in claim 1, wherein the volume ratio of the metal nanoparticle solution, the metal compound solution containing metal ions and the glycine-sodium hydroxide solution in step 1) is (3-5): (1-1.5): (1-1.5).
6. The method as claimed in claim 1, wherein the reaction temperature in step 1) is 160-200 ℃ and the reaction time is 5-10 h.
7. The method for preparing a nanoprobe according to claim 1, wherein in the step 2), the volume ratio of the surfactant P123, the 1M hydrochloric acid, the ethanol and the silicon tetrachloride is 1 (0.2-0.5) to (2-5): (0.5-1.5).
8. The method for preparing a nanoprobe according to claim 1, wherein in the step 2), the solution is poured into an evaporating dish and then is left standing for 12-24 h.
9. The method for preparing the nanoprobe according to claim 1, wherein in the step 2), the AFM probe is immersed in the mixed solution for 15-30min and then taken out to obtain the metal nanoprobe.
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| CN202110464814.0A CN113219211B (en) | 2021-04-28 | 2021-04-28 | Preparation method of nano probe |
| PCT/CN2021/098450 WO2022227229A1 (en) | 2021-04-28 | 2021-06-04 | Method for preparing nanoprobe |
| GB2207755.6A GB2611841A (en) | 2021-04-28 | 2021-06-04 | Method for preparing nanoprobe |
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| WO2022227229A1 (en) | 2022-11-03 |
| CN113219211A (en) | 2021-08-06 |
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