CN106323867B - The preparation method of graphene film ball - Google Patents
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- CN106323867B CN106323867B CN201610670006.9A CN201610670006A CN106323867B CN 106323867 B CN106323867 B CN 106323867B CN 201610670006 A CN201610670006 A CN 201610670006A CN 106323867 B CN106323867 B CN 106323867B
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Abstract
The present invention provides a kind of preparation method of graphene film ball, comprising: silicon oxide microsphere is dispersed in substrate surface, the silicon oxide microsphere is monolayer distribution on the surface of the substrate；The substrate for being dispersed with silicon oxide microsphere is placed into reacting furnace；It is passed through protective gas, the air in reacting furnace is discharged；Reducibility gas and heating reaction furnace are passed through to reaction temperature；Under the protection of protective gas and reducibility gas, it is passed through carbon-source gas to reacting furnace, by predetermined reaction time, graphene is directly grown on the surface of silicon oxide microsphere, forms graphene layer.The preparation method simple process of graphene film ball provided by the invention, and there is longer service life.
Description
Technical field
The present invention relates to the preparation methods of a kind of graphene film ball more particularly to a kind of for atomic force microscope probe
The preparation method of graphene film ball.
Background technique
Atomic force microscope (AFM) is a kind of dividing for surface topography acquisition, electromagnetic performance with atomic resolution
The important instrument of analysis is the important characterization tool in the fields such as Surface Science, nanotechnology.Wherein, AFM probe is that atomic force is aobvious
Important component in micro mirror, belongs to the common consumptive material of the high technology equipment, and main manufacturer is distributed in German, auspicious
Scholar, the U.S., Japan and other countries.Common AFM probe, which mainly passes through, processes silicon or silicon nitride using micro electro mechanical system (MEMS) technology means
It prepares, and conductive AFM probe is metal platinum (and other raising binding force of cladding material in average probe surface plating 10-50nm thickness
Metal, such as titanium, chromium, platinum and iridium etc.) obtain.
However, its conductive coating is prone to wear out conductive AFM probe in use, its electric conductivity is caused to be difficult to have for a long time
Effect is kept, so the associated mechanisms of many countries all are being dedicated to researching and developing the novel spy with high-resolution and more long life
Needle.Currently, the new product of conductive afm tip has the needle point based on carbon nanotube, diamond coating needle point and all-metal silk needle point
Deng, although these new technologies overcome to a certain extent, the common conductive afm tip service life is shorter and the not high disadvantage of resolution ratio,
But its preparation process is sufficiently complex, and production cost is higher.
Summary of the invention
In conclusion a kind of with the spy of the atomic force microscope of more long life and simple process it is necessory to provide
Needle, and the preparation method of the graphene film ball suitable for the probe.
A kind of preparation method of graphene film ball, comprising: silicon oxide microsphere is dispersed in substrate surface, the silica is micro-
Ball is monolayer distribution on the surface of the substrate；The substrate for being dispersed with silicon oxide microsphere is placed into reacting furnace；It is passed through protection
The air in reacting furnace is discharged in gas；Reducibility gas and heating reaction furnace are passed through to reaction temperature；In protective gas and reduction
Property gas protection under, be passed through carbon-source gas to reacting furnace, it is directly raw on the surface of silicon oxide microsphere by predetermined reaction time
Long graphene forms graphene layer.
The partial size of the silicon oxide microsphere is 1 micron to 50 microns in one of the embodiments,.
The silicon oxide microsphere is spaced apart from each other setting in one of the embodiments, between arbitrary silicon oxide microsphere not
It stacks.
The silicon oxide microsphere is formed in the surface of the substrate by following steps in one of the embodiments:
Organic solvent is provided；
Formation silicon oxide microsphere suspension in organic solution is dispersed by the silicon oxide microsphere；
The silicon oxide microsphere suspension is coated on substrate surface；
The substrate of dry coating silica suspension forms dispersion to remove organic solvent, on the surface of the substrate
Silicon oxide microsphere.
The flow-rate ratio of the carbon-source gas, reducibility gas and protective gas is 3.0 in one of the embodiments:
50:50 to 7.0:50:50, reaction time are 1.5 hours to 4 hours.
The carbon-source gas is methane in one of the embodiments, and the reducibility gas is hydrogen, the protection gas
Body is argon gas.
A kind of preparation method of graphene film ball, comprising:
Silicon oxide microsphere is dispersed in a substrate surface, the silicon oxide microsphere is single layer point on the surface of the substrate
Cloth；
The substrate for being dispersed with silicon oxide microsphere is placed into reacting furnace；
It is passed through protective gas with first flow, the air in reacting furnace is discharged；
While heating reaction furnace, reducibility gas is passed through with second flow, until reaction temperature；
The flow of protective gas is adjusted to third flow, adjusts the flow of reducibility gas to the 4th flow, the third
Flow is less than first flow, and the 4th flow is less than second flow；
Under the protection of protective gas and reducibility gas, carbon-source gas is passed through to reacting furnace with the 5th flow, by pre-
Determine the reaction time, directly grows graphene on the surface of silicon oxide microsphere, form a graphene layer.
The first flow is more than or equal to 200sccm in one of the embodiments, and the second flow is more than or equal to
100sccm。
In one of the embodiments, the 5th flow, third flow, the 4th flow flow-rate ratio meet 3.0:
50:50 to 7.0:50:50.
The third flow is 50sccm in one of the embodiments, and the 4th flow is 50sccm, the 5th flow
For 6.3sccm, the reaction time is 30 minutes.
Relative to current technology, the preparation method of graphene film ball provided in an embodiment of the present invention, by the way that silica is micro-
Then ball Monolayer Dispersion directly grows graphene on the silicon oxide microsphere surface with chemical vapour deposition technique, obtains graphene
Film ball, preparation method is simpler, and the graphene film ball prepared has excellent wear resistance, and has extraordinary
Moisture resistance performance, so that there is very high measurement essence when measuring interfacial friction as probe using the graphene film ball
Degree and service life, adaptability are good.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method for the graphene film ball that first embodiment of the invention provides.
Fig. 2 is the flow chart of the preparation method for the graphene film ball that second embodiment of the invention provides.
Fig. 3 is the structural representation that the graphene film ball that second embodiment of the invention provides is applied to atomic force microscope probe
Figure.
Fig. 4 is the electromicroscopic photograph for the graphene film ball that second embodiment of the invention provides.
Fig. 5 is the wear resistance schematic diagram of graphene film talent scout needle provided in an embodiment of the present invention and conventional probe.
Fig. 6 is frictional force of the embodiment of the present invention between the graphene film talent scout needle measured under different humidity and graphite
Schematic diagram.
Main element symbol description
Cantilever 10
Graphene film ball 20
Silicon oxide microsphere 21
Graphene layer 22
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned attached drawing.
Specific embodiment
Below with reference to the attached drawing graphene film ball for atomic force microscope probe that the present invention will be described in detail provides
Preparation method.
Also referring to Fig. 1, first embodiment of the invention, which provides, utilizes process for preparing graphenes by chemical vapour deposition film ball
Preparation method includes the following steps:
Silicon oxide microsphere is dispersed in a substrate surface by step S10；
The substrate for being dispersed with silicon oxide microsphere is placed into reacting furnace by step S20；
Step S30 is passed through protective gas, and the air in reacting furnace is discharged；
Step S40 is passed through reducibility gas and heating reaction furnace to reaction temperature；
Step S50 is passed through carbon-source gas to reacting furnace under the protection of protective gas and reducibility gas, by predetermined
Reaction time directly grows graphene on the surface of silicon oxide microsphere, forms a graphene layer.
In step slo, the partial size of the silicon oxide microsphere can be 100 nanometers to 500 microns.Preferably, the oxidation
The partial size of silicon microballoon is 1 micron to 50 microns, so that on the one hand the silicon oxide microsphere is conducive to graphene in silicon oxide microsphere
Formation, be on the other hand more favorable to the graphene film talent scout's needle being subsequently applied in atomic force microscope.The silica
The shape of microballoon can be spheroidal or elliposoidal, can according to need and selected.The silicon oxide microsphere is pure silica,
Without containing other impurities and functional group.
The material of the substrate can be silicon, silica etc..In the present embodiment, the silicon oxide microsphere is spheroidal,
Partial size is 8 microns, and the substrate is quartz boat.
In step S20, the silicon oxide microsphere is dispersed in substrate surface, and further, the silicon oxide microsphere exists
The surface of the substrate is monolayer distribution, space set between adjacent silicon oxide microsphere, between arbitrary silicon oxide microsphere
It does not stack.The distribution density of the silicon oxide microsphere, which can according to need, to be selected, as long as guaranteeing silicon oxide microsphere described
Substrate surface is monolayer distribution.The silicon oxide microsphere can be formed in the table of the substrate in such a way that solution disperses
Face.
Specifically, the silicon oxide microsphere is formed in the surface of the substrate by following steps:
Step S21 provides an organic solvent；
The silicon oxide microsphere is dispersed formation silicon monoxide microballoon suspension in organic solution by step S22；
The silicon oxide microsphere suspension is coated on substrate surface by step S23；
Step S24, the substrate of dry coating silica suspension is to remove organic solvent, in the surface shape of the substrate
At the silicon oxide microsphere of dispersion.
In the step s 21, for the organic solvent for dispersing the silicon oxide microsphere, the organic solvent can be according to need
It is selected, as long as guaranteeing that the organic solvent is not reacted with substrate and silicon oxide microsphere.The organic solvent can be
Alcohols.In the present embodiment, the organic solvent is ethyl alcohol.
In step S22, the silicon oxide microsphere is put into the organic solvent and carries out ultrasound, the silica is micro-
Ball is evenly dispersed in the organic solvent, forms silicon oxide microsphere suspension.And in the silicon oxide microsphere suspension only
Containing organic solvent and silicon oxide microsphere, other impurities are not contained, the subsequent influence to growth course can be further reduced, improved
The quality of the graphene of growth, to be suitable for.In the silicon oxide microsphere suspension, the distribution density of the silicon oxide microsphere can
To be selected as needed, as long as guaranteeing that subsequent oxidation silicon microballoon can be distributed in substrate surface in monolayer fashion, avoid
It stacks.
In step S23, the silicon oxide microsphere suspension uniformly coats on the surface of the substrate, so that oxidation
Silicon microballoon is dispersed in the surface of substrate.
In step s 24, the substrate can be dried by way of heating or natural evaporation, it is organic molten to remove
Silicon oxide microsphere is dispersed in the surface of substrate by agent.
Further, described is only a specific embodiment, the silicon oxide microsphere in the way of suspension dispersion
It can be directly laid in the substrate surface by the modes such as shedding, smearing, as long as guaranteeing that the silicon oxide microsphere does not stack.
In step s 30, the optional inert gas of the protective gas, specifically, the protective gas can be passed through stone
Ying Guanzhong, the air in quartz ampoule is discharged.The flow of the protective gas is unlimited, as long as the sky in quartz ampoule can be discharged
Gas.It is appreciated that flow is bigger, it is shorter the time required to discharge air plankton etc.；Flow is smaller, then is discharged needed for air etc.
Time it is longer.In the present embodiment, the protective gas is argon gas, and being passed through flow is 50sccm, to be discharged in quartz ampoule
Air and other foreign gases.
In step s 40, the substrate in the reacting furnace and reacting furnace is heated to reaction temperature, and in the mistake of heating
Reducibility gas is continually fed into journey, so as to guarantee in temperature-rise period, substrate is in a reducing atmosphere, favorably
In the reduction and removal of the carbons impurity of silicon oxide microsphere adsorption, to be conducive to obtain clean silica bead table
Face, this helps to improve the quality of the graphene of growth.The reaction temperature can be carried out according to reducibility gas and carbon-source gas
Reaction, as long as guaranteeing that the carbon-source gas can be reacted with reducibility gas.The intake of the reducibility gas can
More than or equal to 30sccm, it is more than or equal to 100sccm etc..In the present embodiment, the reaction temperature is 1130 degree, the 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, the carbon-source gas are reacted with reducibility gas, grow graphene on the surface of the silicon oxide microsphere.The carbon-source gas
It can be the gases such as methane, ethane.The flow of the carbon-source gas can be selected according to the flow of protective gas and reducing gas.
Specifically, the flow-rate ratio of the carbon-source gas, reducibility gas and protective gas can be 3.0:50:50 to 7.0:50:50, reaction
Time is -4 hours 1.5 hours, thus on the one hand guarantee that graphene can completely be coated on the whole surface of silicon oxide microsphere,
On the other hand, also avoid graphene thickness blocked up.In the present embodiment, the carbon-source gas is methane, then methane, hydrogen, argon gas
Flow be respectively 6.3sccm, 50sccm, 50sccm.If the excessively high thickness that will increase graphene of methane, too low to will lead to
It is imperfect to graphene.Temperature, gas flow, reaction time are the principal elements for determining graphene growth.Exist between three
Dependence.Wherein, at a certain temperature, by keeping the methane selected, hydrogen, argon flow to can be obtained by corresponding pattern
Graphene.
When after the reaction was completed, opening reacting furnace makes reacting furnace be reduced rapidly to room temperature in 30 minutes, graphite can be obtained
Alkene film ball, can shorten the etch period of graphene in this way, to reduce gas to the etching of graphene, improve silicon oxide microsphere
The quality of surface graphene.
The graphene layer can directly be coated on the surface of the silicon oxide microsphere, and directly connect with the spherical substrate
Touching.Specifically, the graphene layer can be directly grown in the surface of the spherical substrate, thus the surface with the spherical substrate
Directly contact.The graphene layer includes an at least single layer graphene film, and the number of plies of the graphene layer can be 3-10 layers, described
The thickness of graphene layer can be 1 nanometer to 3 nanometers, so that the graphene layer is easier to prepare, and reduce the shape of probe
Becoming influences.The graphene film is a continuous single layer of carbon atom layer, i.e. single-layer graphene, with a thickness of 0.34 nanometer.Further,
The graphene layer is a pure graphene-structured, and the pure graphene-structured refers in the graphene layer to be pure graphene and only
Only contain carbon atom containing graphene, and in the graphene, other impurities and functional group is free of, so as to reduce other
The influence of impurity avoids the suction-operated of functional group and other impurities, improves subsequent measurement accuracy.Further, due to described
Graphene layer is a pure graphene-structured, therefore the graphene layer can firmly be coated on the surface of the spherical substrate, energy
It is enough effectively to avoid falling off in subsequent measurement process.
Referring to Fig. 2, the system using process for preparing graphenes by chemical vapour deposition film ball that second embodiment of the invention provides
Preparation Method includes the following steps:
Silicon oxide microsphere is dispersed in a substrate surface by step S10；
The substrate for being dispersed with silicon oxide microsphere is placed into reacting furnace by step S20；
Step S30 is passed through protective gas with first flow, the air in reacting furnace is discharged；
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 third flow, adjusts the flow of reducibility gas to the 4th flow,
The third flow is less than first flow, and the 4th flow is less than second flow；
Step S60 is passed through carbon source gas to reacting furnace with the 5th flow under the protection of protective gas and reducibility gas
Body directly grows graphene on the surface of silicon oxide microsphere, forms a graphene layer by predetermined reaction time.
The preparation method and first embodiment of graphene film ball provided by the invention are essentially identical, and difference is, into one
Step includes the steps that an adjustment protective gas and reducibility gas flow.
In step s 30, the first flow can be more than or equal to 200sccm, the air in reacting furnace to be discharged as soon as possible.
In step s 40, the second flow can be more than or equal to 100sccm, to guarantee the quartz ampoule in temperature-rise period
It is inside in a reducing atmosphere, is conducive to the reduction and removal of the carbons impurity of silica bead surface absorption, to have
Conducive to clean silica bead surface is obtained, this helps to improve the quality of the graphene of growth.
In step s 50, the third flow, the 4th flow are selected as needed, specifically, the third flow
Less than first flow, the 4th flow is less than second flow, and the third flow, the 4th flow can be equal or different, to guarantee stone
Black alkene can completely be coated on the whole surface of silicon oxide microsphere, while avoid graphene thickness blocked up.In the present embodiment, institute
Stating third flow is 50sccm, and the 4th flow is 50sccm.
In step S60, the 5th flow of intake and third flow, the 4th flow of the carbon-source gas are interrelated,
To obtain the graphene layer of high quality.Specifically, the flow-rate ratio of the 5th flow, third flow, the 4th flow meets 3.0:
50:50 to 7.0:50:50, to form the graphene layer of high quality on silicon oxide microsphere surface, to avoid to having grown
The etching of graphene layer.In the present embodiment, the 5th flow is 6.3sccm.
Embodiment: the silicon oxide microsphere that average grain diameter is 8um is dispersed on quartz boat, is placed into quartz ampoule.Adding
It is first passed through in quartz ampoule with the argon gas of 1000sccm before hot, the air in quartz ampoule is discharged.Then extremely by diamond heating
1130 degrees Celsius, the pure hydrogen gas of 200sccm is passed through in heating process.After being heated to target temperature, while by hydrogen
The flow of gas and the flow of argon gas are adjusted to 50sccm.Finally, being passed through the methane gas growth graphene of 6.3sccm.Two hours
Afterwards, opening CVD tube furnace makes temperature drop to room temperature rapidly in 30 minutes.
Also referring to Fig. 3 and Fig. 4, the graphene layer 22 that second embodiment of the invention provides continuously is coated on institute
The surface of silicon oxide microsphere 21 is stated, and is directly contacted with the silicon oxide microsphere 21, thus by 21 gapless of silicon oxide microsphere
Cladding get up.The graphene film ball 20 is attached at one end of the cantilever 10.Specifically, the graphene film ball 20 can lead to
Cross the surface that an adhesive layer (not shown) is attached at the cantilever 10.Since in graphene film ball 20, the graphene layer 22 is whole
The surface for being coated on silicon oxide microsphere 21 of body, therefore the graphene layer 22 passes through the surface of adhesive layer and the cantilever 10
It is in close contact, thus by the whole one end for being firmly fixed to the cantilever 10 of graphene film ball 20.
Please refer to fig. 5, the present embodiment is further to the steady of graphene film talent scout's needle using the graphene film ball
It is qualitative to be tested.Same position of the graphene film talent scout needle with the contact stress of 1Gpa in graphite rubs repeatedly, long
Superslide just fails after up to two hours, it was demonstrated that the graphene film talent scout can be realized stable superslide state for graphite.
In addition, can still be obtained when the graphene film talent scout needle is moved to new position after the superslide state failure of the position
Superslide is obtained, to prove that the graphene film talent scout needle especially needle point has very excellent wear resistance.
In addition, referring to Fig. 6, the present embodiment further surveys the moisture resistance performance of the graphene film talent scout needle
Examination.By the way that vapor and nitrogen are passed through environmental chamber with predetermined ratio, different humidity is obtained, to the resistance to of graphene film talent scout's needle
Psychometric performance is tested.The graphene film talent scout needle is in the environment that humidity is 31.8% it can be seen from Fig. 6, phase
When moving distance for graphite is 1 micron to 10 microns, it is able to maintain that superslide state；In addition, the graphene film talent scout
Between needle and graphite when humidity is up to 51%, it still is able to maintain superslide state, to prove the graphene film talent scout needle
With extraordinary moisture resistance, and still there is excellent wear resistance in the case where high humility.
The preparation method of graphene film ball provided by the invention, by dispersing silicon oxide microsphere, then directly in dispersion
Prepared by the mode of silicon oxide microsphere surface growth graphene, preparation process is simpler, and the graphene quality obtained is high, therefore
The graphene film ball is more wear-resisting, therefore uses the longevity with longer with the atomic force microscope probe of the graphene film ball
Life.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot 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, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (8)
1. a kind of preparation method of graphene film ball, comprising:
Silicon oxide microsphere is dispersed in substrate surface, the silicon oxide microsphere is monolayer distribution on the surface of the substrate；
The substrate for being dispersed with silicon oxide microsphere is placed into reacting furnace；
It is passed through protective gas, the air in reacting furnace is discharged；
Reducibility gas and heating reaction furnace are passed through to reaction temperature；
Under the protection of protective gas and reducibility gas, it is passed through carbon-source gas to reacting furnace, by predetermined reaction time, in oxygen
The surface of SiClx microballoon directly grows graphene, forms graphene layer；
The partial size of the silicon oxide microsphere is 1 micron to 50 microns, the stream of the carbon-source gas, reducibility gas and protective gas
Amount is than being 3.0:50:50 to 7.0:50:50.
2. the preparation method of graphene film ball as described in claim 1, which is characterized in that the silicon oxide microsphere is spaced apart from each other
Setting.
3. the preparation method of graphene film ball as described in claim 1, which is characterized in that the silicon oxide microsphere passes through following
Step is formed in the surface of the substrate:
Organic solvent is provided；
Formation silicon oxide microsphere suspension in organic solution is dispersed by the silicon oxide microsphere；
The silicon oxide microsphere suspension is coated on substrate surface；
The substrate of dry coating silica suspension forms the oxidation of dispersion to remove organic solvent, on the surface of the substrate
Silicon microballoon.
4. the preparation method of graphene film ball as described in claim 1, which is characterized in that the reaction time is 1.5 hours to 4 small
When.
5. the preparation method of graphene film ball as claimed in claim 4, which is characterized in that the carbon-source gas is methane, institute
Stating reducibility gas is hydrogen, and the protective gas is argon gas.
6. a kind of preparation method of graphene film ball, comprising:
Silicon oxide microsphere is dispersed in a substrate surface, the silicon oxide microsphere is monolayer distribution on the surface of the substrate；
The substrate for being dispersed with silicon oxide microsphere is placed into reacting furnace；
It is passed through protective gas with first flow, the air in reacting furnace is discharged；
While heating reaction furnace, reducibility gas is passed through with second flow, until reaction temperature；
The flow of protective gas is adjusted to third flow, adjusts the flow of reducibility gas to the 4th flow, the third flow
Less than first flow, the 4th flow is less than second flow；
Under the protection of protective gas and reducibility gas, carbon-source gas is passed through to reacting furnace with the 5th flow, by predetermined anti-
Between seasonable, graphene is directly grown on the surface of silicon oxide microsphere, forms a graphene layer；
5th flow, third flow, the 4th flow flow-rate ratio meet 3.0:50:50 to 7.0:50:50.
7. the preparation method of graphene film ball as claimed in claim 6, which is characterized in that the first flow is more than or equal to
200sccm, the second flow are more than or equal to 100sccm.
8. the preparation method of graphene film ball as claimed in claim 7, which is characterized in that the third flow is 50sccm,
4th flow is 50sccm, and the 5th flow is 6.3sccm, and the reaction time is 30 minutes.
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| 石墨烯的纳米摩擦与磨损性质;朱齐荣等;《物理化学学报》;20130503;第29卷(第7期);第1582-1587页 * |
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