CN110514873A - A kind of hydrogen reduction method prepares graphene coated atomic force microscope probe - Google Patents
A kind of hydrogen reduction method prepares graphene coated atomic force microscope probe Download PDFInfo
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- CN110514873A CN110514873A CN201910732594.8A CN201910732594A CN110514873A CN 110514873 A CN110514873 A CN 110514873A CN 201910732594 A CN201910732594 A CN 201910732594A CN 110514873 A CN110514873 A CN 110514873A
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- Prior art keywords
- graphene oxide
- probe
- atomic force
- force microscope
- graphene
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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
-
- 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
Abstract
The present invention provides a kind of hydrogen reduction method and prepares graphene coated atomic force microscope probe.Firstly, configuring graphene oxide solution using the graphene oxide of Hummers method preparation；Then, atomic force microscope probe is placed on smooth qualitative filter paper, probe tip direction is upward；Secondly, qualitative filter paper quickly sponges liquid by graphene oxide solution drop coating on cantilever and needle point；Finally, heating and using hydrogen reducing graphene oxide.The method of the invention is using graphene oxide as covering material, good dispersion, qualitative filter paper is for adsorbing extra solution, it can make the quick removal of remaining solution, graphene oxide can be adjacent to rapidly probe, and using hydrogen reduction method redox graphene, compare high temperature reduction method, oxygen-containing group can be removed in lower temperature, avoid the pollution of the destruction and exogenous impurity that bring metal layer using high temperature and strong reductant.
Description
Technical field
The present invention relates to atomic force microscope field, especially a kind of hydrogen reduction method prepares graphene coated atomic force microscopy
Mirror probe.
Background technique
As the technology of Material Field develops, probing into material surface microscopic appearance and microscopic characteristics becomes increasingly to weigh
It wants, the image of atomic resolution can be obtained by scanning probe microscopy.Atomic force microscope probe ingredient is generally silicon
Or silicon nitride, probe tip radius are generally 10 to tens nm, micro-cantilever be usually it is 100-500 μm long, 10-50 μm wide and
The silicon wafer or nitridation silicon wafer of 500nm-5 μ m-thick.Metal platinum, titanium, chromium in average probe surface plating 10-50nm thickness, platinum or iridium etc.
Obtain conductive AFM probe.However, its conductive coating is prone to wear out conductive AFM probe in use, cause its electric conductivity difficult
With permanently effective holding, need to research and develop the novel probe with high-resolution and more long life.In addition, atomic force microscope
Probe tip is highly prone to some organic and inorganic substances pollutions during transport and storage, when needle point exposes in short time
Also the pollution of exogenous impurity is highly prone to when common indoor environment or after detection use.
AFM probe belongs to the consumptive material of high-tech instrument, application field is not since application range is only limitted to atomic force microscope
Extensively.World wide has the various AFM probes of nearly more than ten factory's development and production, and market is substantially saturated.Atomic force microscope field
It updates progress and depends on relevant enterprise and relevant technical researcher, the technical progress of other field can not be in time and complete
Introduce to face atomic force microscope field.Graphene thickness only has 0.34nm, and high mechanical strength has good electric conductivity, resistance to
High temperature, corrosion-resistant, resistance to beam bombardment are used to prepare conducting atomic force microscopy probe by some seminars, to a certain degree
On improve the service performance of probe.But presently relevant preparation method, such as infusion process, transfer method, however it remains needle point packet
It is excessive to cover impurity, is unable to large scale preparation, process is sufficiently complex, coats the disadvantages of yield rate is relatively low, and production cost is higher.
Summary of the invention
The present invention provides a kind of hydrogen reduction method and prepares graphene coated atomic force microscope probe, reduces the quick mill of needle point
Damage, extends the service life of probe, avoids AFM probe to the pollution of sample, keep the high-resolution of probe and reduce cost.This
Inventing prepared AFM probe and chemically organizing on angled is Si/Si3N4Layer, metal layer are superimposed with graphene layer, from structure angle
It is traditional AFM probe needle point structure cladding two-dimensional graphene material on degree.Graphite in the relevant technical literature that can be found at present
It is all high-quality graphene that alkene, which coats graphene in atomic force microscope probe, and more common graphene oxide instead and has no
Zhu Yu report.Graphene oxide has easily dispersion, preferably package object construction, the advantages that can largely preparing, it may have lamella
The disadvantages of electric conductivity is poor, and the pollution of exogenous impurity is carried out using reducing agent zone of reduction, and destroys metal-layer structure.The present invention will
AFM probe is placed on qualitative filter paper, using liquid-transfering gun/suction pipe by graphene oxide drop drop coating on AFM probe, filter paper pair
Liquid has strong absorbent properties, most part liquid can be removed in time, can be at a lower temperature using hydrogen reduction method
Redox graphene avoids the destruction of probe structure.
The present invention adopts the following technical scheme:
A kind of hydrogen reduction method prepares graphene coated atomic force microscope probe, includes the following steps:
(1) graphene oxide composite material is obtained using Hummers method, is configured to graphene oxide solution；
(2) atomic force microscope probe is placed on smooth qualitative filter paper, probe tip direction is upward；
(3) use pipettor or dropper by graphene oxide solution drop coating on cantilever and needle point, qualitative filter paper is quickly inhaled
Receive liquid, it is dry；
(4) atomic force microscope probe is transferred on silicon wafer, is put into tube furnace, be passed through nitrogen and exclude air, heating
And it is passed through hydrogen reducing graphene oxide.
Graphene oxide solution concentration in step (1) is 0.001-10mg/mL.
Graphene oxide solution solvent for use in step (1) is water, ethyl alcohol, propyl alcohol, methylene chloride, gasoline, butanol, third
Ketone, ether, acetaldehyde, petroleum ether, benzene,toluene,xylene, pentane, hexane, octane, hexamethylene, cyclohexanone, toluene cyclohexanone, chlorine
Benzene, dichloro-benzenes, methylene chloride, methanol, isopropanol, propylene oxide, methyl acetate, ethyl acetate, propyl acetate, espeleton,
Methylisobutylketone, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, acetonitrile, pyridine, phenol and its mixed solution.
Pipettor or dropper in step (3) every time can drop coating liquor capacity be 1uL-1mL, drying time 1s-
1800s, drying temperature are 0-80 DEG C.
Heating temperature in step (4) is 350-450 DEG C, heating time 0.5-2h.
The present invention has the advantage that
(1) the method for the invention is using graphene oxide as covering material, and compare high-quality graphene, and having can
Largely prepare single layer and few layer material, good dispersion, can the various strength solutions of quantitative configuration, be more advantageous to that be attached at atomic force aobvious
Micro mirror detecting probe surface coats the advantages that close, uniform.
(2) the method for the invention can not only make remaining solution using qualitative filter paper for adsorbing extra solution
Quick removal, graphene oxide can be adjacent to rapidly probe, avoid the presence of solution that material is desorbed, and can also avoid droplets from stream
To other positions of atomic force microscope probe, causes cladding area excessive, influence probe performance.Due to the presence of filter paper, i.e.,
Make the solvent for being not easy to volatilize also due to content is less and quickly disposes.
(3) the method for the invention use hydrogen reduction method redox graphene, compare high temperature reduction method, can compared with
Low temperature removes oxygen-containing group, avoids the dirt of destruction and exogenous impurity that metal layer is brought using high temperature and strong reductant
Dye.
(4) present invention can reduce scientific research cost, extend the service life of probe, many experiments can be carried out, to reduce
The loss of probe, increases the reliability of test data, graphene AFM probe will not contaminated samples, be capable of providing true figure
Picture.
(5) the method for the invention preparation process is simple, and material therefor is easy to get, and the requirement to equipment is lower, may be implemented
On a large scale, batch coats, and greatly improves production efficiency, and is conducive to reduce error, is suitable for industry or laboratory operation, tool
There is huge application prospect.
Detailed description of the invention
Fig. 1 is the Raman figure that the method for the present invention prepares graphene oxide.
Fig. 2 is the XPS figure that the method for the present invention prepares graphene oxide.
Fig. 3 is the XPS figure that the method for the present invention hydrogen reduction graphene oxide powder prepares graphene.
Fig. 4 is the structural schematic diagram of the method for the present invention graphene coated atomic force microscope probe.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) Hummers method is obtained into graphene oxide composite material and is put into aqueous solution, ultrasonic 30min configures 0.1mg/mL's
Graphene oxide water solution.
(2) atomic force microscope probe is placed on smooth qualitative filter paper, probe tip direction is upward.
(3) graphene oxide water solution of 100uL is pipetted using pipettor, drop coating is on the cantilever and needle point of probe, In
Dry 10min at a temperature of 60 DEG C.
(4) atomic force microscope probe is transferred on silicon wafer, is put into tube furnace, be passed through nitrogen and exclude air, heating
To 400 DEG C, and it is passed through hydrogen reducing graphene oxide, time 0.5h.
Embodiment 2
(1) Hummers method is obtained into graphene oxide composite material and is put into aqueous solution, ultrasonic 30min configures the oxygen of 1mg/mL
Graphite aqueous solution.
(2) atomic force microscope probe is placed on smooth qualitative filter paper, probe tip direction is upward.
(3) graphene oxide water solution of 100uL is pipetted using pipettor, drop coating is on the cantilever and needle point of probe, In
Dry 10min at a temperature of 60 DEG C.
(4) atomic force microscope probe is transferred on silicon wafer, is put into tube furnace, be passed through nitrogen and exclude air, heating
To 400 DEG C, and it is passed through hydrogen reducing graphene oxide, time 0.5h.
Embodiment 3
(1) Hummers method is obtained into graphene oxide composite material and is put into ethanol solution, ultrasonic 30min configures 0.1mg/mL
Graphene oxide ethanol solution.
(2) atomic force microscope probe is placed on smooth qualitative filter paper, probe tip direction is upward.
(3) the graphene oxide ethanol solution of 100uL is pipetted using pipettor, drop coating on the cantilever and needle point of probe,
Dry 10min at a temperature of 20 DEG C.
(4) atomic force microscope probe is transferred on silicon wafer, is put into tube furnace, be passed through nitrogen and exclude air, heating
To 400 DEG C, and it is passed through hydrogen reducing graphene oxide, time 0.5h.
Embodiment 4
(1) Hummers method is obtained into graphene oxide composite material and is put into aqueous solution, ultrasonic 30min configures 0.1mg/mL's
Graphene oxide water solution.
(2) atomic force microscope probe is placed on smooth qualitative filter paper, probe tip direction is upward.
(3) graphene oxide water solution of 100uL is pipetted using pipettor, drop coating is on the cantilever and needle point of probe, In
Dry 10min at a temperature of 60 DEG C.
(4) atomic force microscope probe is transferred on silicon wafer, is put into tube furnace, be passed through nitrogen and exclude air, heating
To 450 DEG C, and it is passed through hydrogen reducing graphene oxide, time 0.5h.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (5)
1. a kind of hydrogen reduction method prepares graphene coated atomic force microscope probe, include the following steps:
(1) graphene oxide composite material is obtained using Hummers method, is configured to graphene oxide solution；
(2) atomic force microscope probe is placed on smooth qualitative filter paper, probe tip direction is upward；
(3) use pipettor or dropper by graphene oxide solution drop coating on cantilever and needle point, qualitative filter paper quickly sponges
Liquid, it is dry；
(4) atomic force microscope probe is transferred on silicon wafer, is put into tube furnace, be passed through nitrogen and exclude air, heat and lead to
Enter hydrogen reducing graphene oxide.
2. preparation method according to claim 1, which is characterized in that the graphene oxide solution concentration in step (1) is
0.001-10mg/mL。
3. preparation method according to claim 1, which is characterized in that molten used in the graphene oxide solution in step (1)
Agent is water, ethyl alcohol, propyl alcohol, methylene chloride, gasoline, butanol, acetone, ether, acetaldehyde, petroleum ether, benzene,toluene,xylene, penta
Alkane, hexane, octane, hexamethylene, cyclohexanone, toluene cyclohexanone, chlorobenzene, dichloro-benzenes, methylene chloride, methanol, isopropanol, epoxy third
Alkane, methyl acetate, ethyl acetate, propyl acetate, espeleton, methylisobutylketone, glycol monoethyl ether, ethylene glycol monoethyl ether,
Ethylene glycol monobutyl ether, acetonitrile, pyridine, phenol and its mixed solution.
4. preparation method according to claim 1, which is characterized in that pipettor or dropper in step (3) can drip every time
Painting liquor capacity is 1uL-1mL, and drying time 1s-1800s, drying temperature is 0-80 DEG C.
5. preparation method according to claim 1, which is characterized in that the heating temperature in step (4) is 350-450 DEG C,
Heating time is 0.5-2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910732594.8A CN110514873A (en) | 2019-08-04 | 2019-08-04 | A kind of hydrogen reduction method prepares graphene coated atomic force microscope probe |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112762835A (en) * | 2021-01-18 | 2021-05-07 | 华东师范大学 | Micro-control platform for non-destructive fixed-point transfer of two-dimensional material by solid-liquid method |
| CN114217097A (en) * | 2021-11-19 | 2022-03-22 | 国家纳米科学中心 | Preparation method of graphene functionalized silicon-based probe |
-
2019
- 2019-08-04 CN CN201910732594.8A patent/CN110514873A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112762835A (en) * | 2021-01-18 | 2021-05-07 | 华东师范大学 | Micro-control platform for non-destructive fixed-point transfer of two-dimensional material by solid-liquid method |
| CN112762835B (en) * | 2021-01-18 | 2021-10-15 | 华东师范大学 | Micro-control platform for non-destructive fixed-point transfer of two-dimensional material by solid-liquid method |
| CN114217097A (en) * | 2021-11-19 | 2022-03-22 | 国家纳米科学中心 | Preparation method of graphene functionalized silicon-based probe |
| CN114217097B (en) * | 2021-11-19 | 2024-03-05 | 国家纳米科学中心 | Preparation method of graphene functionalized silicon-based probe |
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Application publication date: 20191129 |
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