CN106323867A - Preparation method of graphene membrane spheres - Google Patents
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- CN106323867A CN106323867A CN201610670006.9A CN201610670006A CN106323867A CN 106323867 A CN106323867 A CN 106323867A CN 201610670006 A CN201610670006 A CN 201610670006A CN 106323867 A CN106323867 A CN 106323867A
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Abstract
The invention provides a preparation method of graphene membrane spheres. The preparation method includes the steps that silicon oxide microspheres are dispersed on the surface of a substrate, wherein the silicon oxide microspheres are distributed on the surface of the substrate in a single layer; the substrate with the silicon oxide microspheres dispersed is put into a reaction furnace; protective gas is introduced, and air in the reaction furnace is discharged; reducing gas is introduced, and the reaction furnace is heated to the reaction temperature; carbon source gas is introduced into the reaction furnace under protection of the protective gas and the reducing gas, graphene directly grows on the surfaces of the silicon oxide microspheres after preset reaction time, and a graphene layer is formed. The preparation method of the graphene membrane spheres is simple in process, and the prepared graphene membrane spheres have a longer service life.
Description
Technical field
The present invention relates to the preparation method of a kind of graphene film ball, particularly relate to a kind of for atomic force microscope probe
The preparation method of graphene film ball.
Background technology
Atomic force microscope (AFM) is a kind of to have dividing for surface topography collection, electromagnetic performance of atomic resolution
The important instrument of analysis, is the important characterization tool in the field such as Surface Science, nanotechnology.Wherein, AFM probe is atomic force microscopy
Important component part in mirror, belongs to the conventional consumptive material of this high technology equipment, and its main manufacturer is distributed in Germany, auspicious
Scholar, the U.S., Japan and other countries.Common AFM probe is mainly by utilizing micro electro mechanical system (MEMS) technology means processing silicon or silicon nitride
Prepare, and conducting electricity AFM probe is that (and other improve binding force of cladding material in thick for average probe plated surface 10-50nm metal platinum
Metal, such as titanium, chromium, platinum and iridium etc.) obtain.
But, conduction AFM probe in use its conductive coating is prone to wear out, and causing its electric conductivity to be difficult to for a long time has
Effect keeps, so the associated mechanisms of a lot of country all has the novel spy of high-resolution and more long life being devoted to research and develop
Pin.At present, the new product of conduction afm tip has needle point based on CNT, diamond coating needle point and all-metal silk needle point
Deng, although these new techniques overcome the shortcoming that the common conductive afm tip life-span is shorter and resolution is the highest to a certain extent,
But its preparation process is sufficiently complex, and production cost is higher.
Summary of the invention
In sum, necessary offer one has the more long life and the simple atomic force microscope of technique is visited
Pin, and it is applicable to the preparation method of the graphene film ball of this probe.
A kind of preparation method of graphene film ball, including: silicon oxide microsphere is dispersed in substrate surface, and described silicon oxide is micro-
Ball is monolayer distribution on the surface of described substrate；The substrate being dispersed with silicon oxide microsphere is placed in reacting furnace；It is passed through protection
Gas, discharges the air in reacting furnace；It is passed through reducibility gas heating reaction furnace to reaction temperature；In protective gas and reduction
Under the protection of property gas, it is passed through carbon-source gas to reacting furnace, through predetermined reaction time, directly gives birth on the surface of silicon oxide microsphere
Long Graphene, forms graphene layer.
Wherein in an embodiment, the particle diameter of described silicon oxide microsphere is 1 micron to 50 microns.
Wherein in an embodiment, the spaced setting of described silicon oxide microsphere, between arbitrary silicon oxide microsphere not
Stacking.
Wherein in an embodiment, described silicon oxide microsphere is formed at the surface of described substrate by following steps:
Organic solvent is provided；
Described silicon oxide microsphere is scattered in organic solution formation silicon oxide microsphere suspension；
Described silicon oxide microsphere suspension is coated on substrate surface；
It is dried and is coated with the substrate of silicon oxide suspension to remove organic solvent, formed scattered on the surface of described substrate
Silicon oxide microsphere.
Wherein in an embodiment, the flow-rate ratio of described carbon-source gas, reducibility gas and protective gas is 3.0:50:
50 to 7.0:50:50, the response time is 1.5 hours to 4 hours.
Wherein in an embodiment, described carbon-source gas is methane, and described reducibility gas is hydrogen, described protection gas
Body is argon.
A kind of preparation method of graphene film ball, including:
Silicon oxide microsphere is dispersed in a substrate surface, and described silicon oxide microsphere is that monolayer divides on the surface of described substrate
Cloth；
The substrate being dispersed with silicon oxide microsphere is placed in reacting furnace；
It is passed through protective gas with first flow, discharges the air in reacting furnace；
While heating reaction furnace, it is passed through reducibility gas with second flow, until reaction temperature；
Adjust the flow of protective gas to the 3rd flow, adjust the flow of reducibility gas to the 4th flow, the described 3rd
Flow is less than first flow, and described 4th flow is less than second flow；
Under the protection of protective gas and reducibility gas, it is passed through carbon-source gas with the 5th flow to reacting furnace, through pre-
Determine the response time, at the surface direct growth Graphene of silicon oxide microsphere, form a graphene layer.
Wherein in an embodiment, described first flow is more than or equal to 200sccm, and described second flow is more than or equal to
100sccm。
Wherein in an embodiment, described 5th flow, the 3rd flow, the flow-rate ratio of the 4th flow meet 3.0:
50:50 to 7.0:50:50.
Wherein in an embodiment, described 3rd flow is 50sccm, and described 4th flow is 50sccm, the 5th flow
For 6.3sccm, the response time is 30 minutes.
Relative to current technology, the preparation method of the graphene film ball that the embodiment of the present invention provides, by micro-by silicon oxide
Ball Monolayer Dispersion, then with chemical vapour deposition technique directly at described silicon oxide microsphere superficial growth Graphene, obtains Graphene
Film ball, preparation method is simpler, and the graphene film ball of preparation has the wear resistance of excellence, and has extraordinary
Moisture resistance performance, during so that utilize this graphene film ball as probe measurement interfacial friction, has the highest measurement essence
Degree and service life, adaptability is good
Accompanying drawing explanation
The flow chart of the preparation method of the graphene film ball that Fig. 1 provides for first embodiment of the invention.
The flow chart of the preparation method of the graphene film ball that Fig. 2 provides for second embodiment of the invention.
Fig. 3 is applied to the structural representation of atomic force microscope probe for the graphene film ball that second embodiment of the invention provides
Figure.
The electromicroscopic photograph of the graphene film ball that Fig. 4 provides for second embodiment of the invention.
Graphene film talent scout's pin that Fig. 5 provides for the embodiment of the present invention and the wear resistance schematic diagram of conventional probe.
Fig. 6 is the frictional force between graphene film talent scout's pin and the graphite that the embodiment of the present invention records under different humidity
Schematic diagram.
Main element symbol description
Cantilever 10
Graphene film ball 20
Silicon oxide microsphere 21
Graphene layer 22
Specific examples below will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Detailed description of the invention
The graphene film ball for atomic force microscope probe of present invention offer is provided in detail below with reference to accompanying drawing
Preparation method.
Seeing also Fig. 1, first embodiment of the invention provides and utilizes process for preparing graphenes by chemical vapour deposition film ball
Preparation method, comprises the steps:
Step S10, is dispersed in a substrate surface by silicon oxide microsphere；
Step S20, is placed into the substrate being dispersed with silicon oxide microsphere in reacting furnace；
Step S30, is passed through protective gas, discharges the air in reacting furnace；
Step S40, is passed through reducibility gas heating reaction furnace to reaction temperature；
Step S50, under the protection of protective gas and reducibility gas, is passed through carbon-source gas to reacting furnace, through predetermined
In the response time, at the surface direct growth Graphene of silicon oxide microsphere, form a graphene layer.
In step slo, the particle diameter of described silicon oxide microsphere can be that 100 nanometers are to 500 microns.Preferably, described oxidation
The particle diameter of silicon microsphere is 1 micron to 50 microns so that on the one hand described silicon oxide microsphere is conducive to Graphene at silicon oxide microsphere
Formation, on the other hand be more favorable to the graphene film talent scout's pin being subsequently applied in atomic force microscope.Described silicon oxide
The shape of microsphere can be spheroidal or elliposoidal, can select as required.Described silicon oxide microsphere is pure silicon oxide,
Do not contain other impurity and functional group.
The material of described substrate can be silicon, silicon dioxide etc..In the present embodiment, described silicon oxide microsphere for spheroidal,
Particle diameter is 8 microns, and described substrate is quartz boat.
In step S20, described silicon oxide microsphere is dispersed in substrate surface, and further, described silicon oxide microsphere exists
The surface of described substrate is monolayer distribution, space set between adjacent silicon oxide microsphere, between arbitrary silicon oxide microsphere
Do not stack.The distribution density of described silicon oxide microsphere can select as required, as long as ensureing that silicon oxide microsphere is described
Substrate surface is monolayer distribution.Described silicon oxide microsphere can be formed at the table of described substrate by the scattered mode of solution
Face.
Concrete, described silicon oxide microsphere is formed at the surface of described substrate by following steps:
Step S21 a, it is provided that organic solvent；
Step S22, is scattered in organic solution formation silicon monoxide microsphere suspension by described silicon oxide microsphere；
Step S23, is coated on substrate surface by described silicon oxide microsphere suspension；
Step S24, is dried and is coated with the substrate of silicon oxide suspension to remove organic solvent, in the surface shape of described substrate
Become scattered silicon oxide microsphere.
In the step s 21, described organic solvent is used for disperseing described silicon oxide microsphere, and described organic solvent can be according to need
Select, as long as ensureing that described organic solvent does not reacts with substrate and silicon oxide microsphere.Described organic solvent can be
Alcohols.In the present embodiment, described organic solvent is ethanol.
In step S22, being put in described organic solvent by described silicon oxide microsphere and carry out ultrasonic, described silicon oxide is micro-
Ball is dispersed in described organic solvent, forms silicon oxide microsphere suspension.And in described silicon oxide microsphere suspension only
Containing organic solvent and silicon oxide microsphere, do not contain other impurity, the follow-up impact on growth course can be reduced further, improve
The quality of the Graphene of growth, to be applicable to.In described silicon oxide microsphere suspension, the distribution density of described silicon oxide microsphere can
To select as required, as long as ensureing that subsequent oxidation silicon microsphere can be distributed in substrate surface in monolayer fashion, it is to avoid
Stacking.
In step S23, described silicon oxide microsphere suspension uniformly coats on the surface of described substrate, so that oxidation
Silicon microsphere is dispersed in the surface of substrate.
In step s 24, by the way of heating or natural evaporation, described substrate can be dried, organic molten to remove
Agent, is dispersed in the surface of substrate by silicon oxide microsphere.
Further, described utilize the scattered mode of suspension be only a specific embodiment, described silicon oxide microsphere is also
Described substrate surface can be directly laid in, as long as ensureing that described silicon oxide microsphere does not stacks by the mode such as shedding, smear.
In step s 30, the optional noble gas of described protective gas, concrete, described protective gas can be passed through stone
Ying Guanzhong, to discharge the air in quartz ampoule.The flow of described protective gas does not limits, if the sky can discharged in quartz ampoule
Gas.Being appreciated that flow is the biggest, the required time such as air-out impurity is the shortest；Flow is the least, then air-out etc. are required
Time the longest.In the present embodiment, described protective gas is argon, and being passed through flow is 50sccm, to discharge in quartz ampoule
Air and other foreign gas.
In step s 40, the substrate in described reacting furnace and reacting furnace is heated to reaction temperature, and in the mistake of heating
Being continually fed into reducibility gas in journey such that it is able to ensure in temperature-rise period, substrate is in a reducing atmosphere, favorably
In the reduction of carbons impurity and the removal of silicon oxide microsphere surface adsorption, thus be conducive to obtaining clean silicon oxide bead table
Face, this is favorably improved the quality of Graphene of growth.Described reaction temperature can be carried out according to reducibility gas and carbon-source gas
Reaction, as long as ensureing that described carbon-source gas can carry out reacting with reducibility gas.The intake of described reducibility gas can
More than or equal to 30sccm, more than or equal to 100sccm etc..In the present embodiment, described reaction temperature is 1130 degree, described reproducibility gas
Body is hydrogen, and the flow of hydrogen is 50sccm.
In step s 50, it is passed through at the same time under the protection of protective gas and reducibility gas, is passed through carbon source gas to reacting furnace
Body, described carbon-source gas reacts with reducibility gas, at the superficial growth Graphene of described silicon oxide microsphere.Described carbon-source gas
Can be the gas such as methane, ethane.The flow of described carbon-source gas can select according to the flow of protective gas and reducing gas.
Concrete, the flow-rate ratio of described carbon-source gas, reducibility gas and protective gas can be 3.0:50:50 to 7.0:50:50, reaction
Time is 1.5 hours-4 hours, thus on the one hand ensures the whole surface being coated on silicon oxide microsphere that Graphene can be complete,
On the other hand, also avoid Graphene thickness blocked up.In the present embodiment, described carbon-source gas is methane, then methane, hydrogen, argon
Flow be respectively 6.3sccm, 50sccm, 50sccm.If the too high thickness that can increase Graphene of methane, too low meeting causes
Imperfect to Graphene.Temperature, gas flow, response time are the principal elements determining graphene growth.Exist between three
Dependence.Wherein, at a certain temperature, by keeping the methane selected, hydrogen, argon flow amount to can be obtained by corresponding pattern
Graphene.
After reaction completes, open reacting furnace, make reacting furnace be reduced rapidly to room temperature in 30 minutes, i.e. can get graphite
Alkene film ball, so can shorten the etch period of Graphene, thus reduce the gas etching to Graphene, improves silicon oxide microsphere
The quality of surface Graphene.
Described graphene layer can directly be coated on the surface of described silicon oxide microsphere, and directly connects with described spherical substrate
Touch.Concrete, described graphene layer can be directly grown in the surface of described spherical substrate, thus with the surface of described spherical substrate
Directly contact.Described graphene layer includes at least one single layer graphene film, and the number of plies of described graphene layer can be 3-10 layer, described
The thickness of graphene layer can be 1 nanometer to 3 nanometers so that described graphene layer is easier to preparation, and reduce the shape of probe
Become impact.Described graphene film is a continuous print monolayer carbon atomic layer, i.e. single-layer graphene, and thickness is 0.34 nanometer.Further,
Described graphene layer is a pure graphene-structured, and described pure graphene-structured refers in described graphene layer as pure Graphene and only
Containing Graphene, and described Graphene contains only carbon atom, without other impurity and functional group such that it is able to reduce other
The impact of impurity, it is to avoid the adsorption of other impurity such as functional group, improves follow-up certainty of measurement.Further, due to described
Graphene layer is a pure graphene-structured, and the most described graphene layer can firmly be coated on the surface of described spherical substrate, energy
Enough it is prevented effectively from coming off during follow-up measurement.
Refer to Fig. 2, the system utilizing process for preparing graphenes by chemical vapour deposition film ball that second embodiment of the invention provides
Preparation Method, comprises the steps:
Step S10, is dispersed in a substrate surface by silicon oxide microsphere；
Step S20, is placed into the substrate being dispersed with silicon oxide microsphere in reacting furnace；
Step S30, is passed through protective gas with first flow, discharges the air in reacting furnace；
Step S40, while heating reaction furnace, is passed through reducibility gas with second flow, until reaction temperature；
Step S50, adjusts the flow of protective gas to the 3rd flow, adjusts the flow of reducibility gas to the 4th flow,
Described 3rd flow is less than first flow, and described 4th flow is less than second flow；
Step S60, under the protection of protective gas and reducibility gas, is passed through carbon source gas with the 5th flow to reacting furnace
Body, through predetermined reaction time, at the surface direct growth Graphene of silicon oxide microsphere, forms a graphene layer.
The preparation method of the graphene film ball that the present invention provides is essentially identical with first embodiment, and its difference is, enters one
Step includes an adjustment protective gas and the step of reducibility gas flow.
In step s 30, described first flow can be more than or equal to 200sccm, to discharge the air in reacting furnace as soon as possible.
In step s 40, described second flow can be more than or equal to 100sccm, thus ensures quartz ampoule in temperature-rise period
Inside it is in a reducing atmosphere, the reduction of carbons impurity of beneficially silicon oxide bead surface absorption and removal, thus has
Being beneficial to obtain clean silicon oxide bead surface, this is favorably improved the quality of Graphene of growth.
In step s 50, described 3rd flow, the 4th flow select as required, concrete, described 3rd flow
Less than first flow, the 4th flow is less than second flow, and described 3rd flow, the 4th flow can be equal or different, to ensure stone
Ink alkene can be complete the whole surface being coated on silicon oxide microsphere, avoid Graphene thickness blocked up simultaneously.In the present embodiment, institute
Stating the 3rd flow is 50sccm, and described 4th flow is 50sccm.
In step S60, described carbon-source gas to be passed through flow control five flow and the 3rd flow, the 4th flow interrelated,
To obtain high-quality graphene layer.Concrete, described 5th flow, the 3rd flow, the flow-rate ratio of the 4th flow meet 3.0:
50:50 to 7.0:50:50, thus form high-quality graphene layer on silicon oxide microsphere surface, to avoid having grown
The etching of graphene layer.In the present embodiment, described 5th flow is 6.3sccm.
Embodiment: the silicon oxide microsphere that mean diameter is 8um is dispersed on quartz boat, is placed in quartz ampoule.Adding
First it is passed through in quartz ampoule by the argon gas of 1000sccm before heat, discharges the air in quartz ampoule.Then by diamond heating extremely
1130 degrees Celsius, in the middle of heating process, it is passed through the pure hydrogen gas of 200sccm.After being heated to target temperature, simultaneously by hydrogen
The flow of gas and the flow of argon are adjusted to 50sccm.Finally, the methane gas growth Graphene of 6.3sccm it is passed through.Two hours
After, open CVD tube furnace and make temperature drop to rapidly room temperature in 30 minutes.
Seeing also Fig. 3 and Fig. 4, described graphene layer 22 continuous print that second embodiment of the invention provides is coated on institute
State the surface of silicon oxide microsphere 21, and directly contact with described silicon oxide microsphere 21, thus by silicon oxide microsphere 21 gapless
Cladding get up.Described graphene film ball 20 is attached at one end of described cantilever 10.Concrete, described graphene film ball 20 can lead to
Cross a tack coat (not shown) and be attached at the surface of described cantilever 10.Owing to, in graphene film ball 20, described graphene layer 22 is whole
The surface being coated on silicon oxide microsphere 21 of body, the most described graphene layer 22 is tight with the surface of described cantilever 10 by tack coat
Contiguity is touched, thus graphene film ball 20 entirety is firmly fixed to one end of described cantilever 10.
Seeing also Fig. 5, the present embodiment is further to graphene film talent scout's pin steady using described graphene film ball
Qualitative it is tested.Described graphene film talent scout's pin rubs at the same position of graphite repeatedly with the contact stress of 1Gpa, long
After reaching two hours, superslide just lost efficacy, it was demonstrated that described graphene film talent scout is capable of stable superslide state for graphite.
It addition, after the superslide state of this position lost efficacy, still can obtain when described graphene film talent scout's pin is moved to new position
Obtain superslide, thus prove that described graphene film talent scout's pin especially needle point has the most excellent wear resistance.
It addition, refer to Fig. 6, the moisture resistance performance of described graphene film talent scout's pin is surveyed by the present embodiment further
Examination.By steam and nitrogen are passed through environmental chamber with predetermined ratio, obtain different humidity, resistance to graphene film talent scout's pin
Psychometric performance is tested.By in Fig. 6 it can be seen that described graphene film talent scout's pin is in the environment that humidity is 31.8%, phase
When being 1 micron to 10 microns for the displacement of graphite, all it is able to maintain that superslide state；It addition, described graphene film talent scout
Between pin and graphite when humidity is up to 51%, remain able to maintain superslide state, thus prove described graphene film talent scout's pin
There is extraordinary moisture resistance, and still there is in the case of high humility the wear resistance of excellence.
The preparation method of the graphene film ball that the present invention provides, by dispersion silicon oxide microsphere, then directly scattered
Prepared by the mode of silicon oxide microsphere superficial growth Graphene, preparation technology is simpler, and the Graphene quality obtained is high, therefore
Described graphene film ball is more wear-resisting, and the atomic force microscope probe therefore with this graphene film ball has the longer use longevity
Life.
Each technical characteristic of embodiment described above can combine arbitrarily, for making description succinct, not to above-mentioned reality
The all possible combination of each technical characteristic executed in example is all described, but, as long as the combination of these technical characteristics is not deposited
In contradiction, all it is considered to be the scope that this specification is recorded.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for graphene film ball, including:
Silicon oxide microsphere is dispersed in substrate surface, and described silicon oxide microsphere is monolayer distribution on the surface of described substrate；
The substrate being dispersed with silicon oxide microsphere is placed in reacting furnace；
It is passed through protective gas, discharges the air in reacting furnace；
It is passed through reducibility gas heating reaction furnace to reaction temperature；
Under the protection of protective gas and reducibility gas, it is passed through carbon-source gas to reacting furnace, through predetermined reaction time, at oxygen
The surface direct growth Graphene of SiClx microsphere, forms graphene layer.
2. the preparation method of graphene film ball as claimed in claim 1, it is characterised in that the particle diameter of described silicon oxide microsphere is
1 micron to 50 microns.
3. the preparation method of graphene film ball as claimed in claim 1, it is characterised in that described silicon oxide microsphere is spaced
Arrange.
4. the preparation method of graphene film ball as claimed in claim 1, it is characterised in that described silicon oxide microsphere is by following
Step is formed at the surface of described substrate:
Organic solvent is provided；
Described silicon oxide microsphere is scattered in organic solution formation silicon oxide microsphere suspension；
Described silicon oxide microsphere suspension is coated on substrate surface；
It is dried and is coated with the substrate of silicon oxide suspension to remove organic solvent, form scattered oxidation on the surface of described substrate
Silicon microsphere.
5. the preparation method of graphene film ball as claimed in claim 1, it is characterised in that described carbon-source gas, reproducibility gas
The flow-rate ratio of body and protective gas is 3.0:50:50 to 7.0:50:50, and the response time is 1.5 hours to 4 hours.
6. the preparation method of graphene film ball as claimed in claim 5, it is characterised in that described carbon-source gas is methane, institute
Stating reducibility gas is hydrogen, and described protective gas is argon.
7. a preparation method for graphene film ball, including:
Silicon oxide microsphere is dispersed in a substrate surface, and described silicon oxide microsphere is monolayer distribution on the surface of described substrate；
The substrate being dispersed with silicon oxide microsphere is placed in reacting furnace；
It is passed through protective gas with first flow, discharges the air in reacting furnace；
While heating reaction furnace, it is passed through reducibility gas with second flow, until reaction temperature；
The flow of adjustment protective gas, to the 3rd flow, adjusts the flow of reducibility gas to the 4th flow, described 3rd flow
Less than first flow, described 4th flow is less than second flow；
Under the protection of protective gas and reducibility gas, it is passed through carbon-source gas with the 5th flow to reacting furnace, through predetermined anti-
Between Ying Shi, at the surface direct growth Graphene of silicon oxide microsphere, form a graphene layer.
8. the preparation method of graphene film ball as claimed in claim 7, it is characterised in that described first flow is more than or equal to
200sccm, described second flow is more than or equal to 100sccm.
9. the preparation method of graphene film ball as claimed in claim 7, it is characterised in that described 5th flow, the 3rd
Flow, the flow-rate ratio of the 4th flow meet 3.0:50:50 to 7.0:50:50.
10. the preparation method of graphene film ball as claimed in claim 9, it is characterised in that described 3rd flow is 50sccm,
Described 4th flow is 50sccm, and the 5th flow is 6.3sccm, and the response time is 30 minutes.
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| CN110423017A (en) * | 2019-09-06 | 2019-11-08 | 安徽凯盛基础材料科技有限公司 | Graphene coats light hollow bead particles and preparation method completely |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423017A (en) * | 2019-09-06 | 2019-11-08 | 安徽凯盛基础材料科技有限公司 | Graphene coats light hollow bead particles and preparation method completely |
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