CN109883950A - The positioning observing method of two-dimensional material growth - Google Patents
The positioning observing method of two-dimensional material growth Download PDFInfo
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- CN109883950A CN109883950A CN201910129446.7A CN201910129446A CN109883950A CN 109883950 A CN109883950 A CN 109883950A CN 201910129446 A CN201910129446 A CN 201910129446A CN 109883950 A CN109883950 A CN 109883950A
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- dimensional material
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Abstract
The present invention provides a kind of positioning observing method of two-dimensional material growth, includes the following steps: 1) to obtain label graphene；2) growth substrates, and the upper surface that graphene will be marked to be transferred to growth substrates are provided；3) two-dimensional material is grown in the upper surface of growth substrates；4) to mark graphene to carry out location observation to two-dimensional material for label.The positioning observing method of two-dimensional material growth of the invention may be implemented to the growing state of two-dimensional material to carry out that observation is precisely located；The growing state that atomic force microscope location observation two-dimensional material is used in the present invention, does not have strict requirements to the growth conditions of two-dimensional material layer, operation is simple, and testing cost is lower；When the upper surface of growth substrates carries out the multiple growth of two-dimensional material, the growth conditions of the every secondary growth of two-dimensional material can be different, may be implemented to carry out location observation in the growing state of the same area under different growth conditions to two-dimensional material.
Description
Technical field
The invention belongs to measuring technology inventions, more particularly to a kind of positioning observing method of two-dimensional material growth.
Background technique
Graphene is all the time deep by industry and science as a kind of two-dimensional material with excellent physical chemical property
The extensive concern on boundary.Two kinds of mechanism: (1) solution modeling mechanism can be broadly divided by preparing graphene by CVD method:
Main substrate has this very high metal of carbon capacity such as nickel, cobalt, and hydrocarbon resolves into carbon atom at high temperature and incorporates substrate
Inside, when fast cooling, the solubility of carbon sharply declines, and internal carbon is precipitated in substrate surface, to form graphene.(2) table
Surface catalysis mechanism: the substrate for mainly having the carbon capacity such as copper, platinum and germanium low, in high-temperature heating, hydrocarbon dehydrogenation shape
At a large amount of active carbon-based groups, graphene domain is decomposed to form after catalytic type substrate surface.Except different material discussed above serves as a contrast
The mechanism of graphene growth forming core has differences outer on bottom, and graphene growth shows on same substance different crystal orientations or polycrystalline substrates
Form is also completely different.Therefore, graphene forming core and growth have research graphene growth mechanism on location observation various substrates
Extremely important meaning.Meanwhile the method that the two-dimensional materials such as graphene are observed during the growth process in prior art
There is observation higher cost, the problems such as harsh is required to the growth conditions of the two-dimensional materials such as graphene, to be difficult to obtain general
And.For this purpose, the means of testing for developing a kind of inexpensive location observation graphene forming core and growth has very important significance.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of positioning of two-dimensional material growth
Observation method, for solve the two-dimensional materials such as graphene are observed during the growth process in the prior art when it is existing observation at
The problems such as this is higher, harsh to the growth conditions requirement of the two-dimensional materials such as graphene.
In order to achieve the above objects and other related objects, the present invention provides a kind of location observation side of two-dimensional material growth
The positioning observing method of method, the two-dimensional material growth includes the following steps:
1) label graphene is obtained；
2) growth substrates are provided, and the label graphene is transferred to the upper surface of the growth substrates；
3) upper surface of Yu Suoshu growth substrates grows two-dimensional material；
It 4) is that label carries out location observation to the two-dimensional material with the label graphene.
Optionally, in step 1), the label graphene is obtained from highly oriented pyrolytic graphite alkene using mechanical stripping method.
Optionally, the label graphene includes multi-layer graphene.
Optionally, the material for stating growth substrates includes monocrystalline silicon, polysilicon, germanium, copper, nickel or platinum.
Optionally, further include the steps that making annealing treatment the growth substrates between step 2) and step 3).
It optionally, include annealing under vacuum annealing or normal pressure protective atmosphere to the method for growth substrates annealing.
It optionally, after being made annealing treatment to the growth substrates and further include that the growth substrates are carried out clearly before step 3)
The step of washing.
Optionally, the method cleaned to the growth substrates includes that the growth substrates are respectively placed in acetone and wine
Successively it is cleaned by ultrasonic in essence.
Optionally, the time being cleaned by ultrasonic to the growth substrates includes 5~15 minutes.
Optionally, the two-dimensional material includes two chalcogenide of graphene, boron nitride or transition metal.
Optionally, in step 4), the two-dimensional material is observed under lateral force mode using atomic force microscope.
Optionally, further include the steps that repeating step 3)~step 4) at least once after step 4).
Optionally, in multiple observation process, the growing state of described two-dimensional material the same area is observed.
As described above, the positioning observing method that two-dimensional material of the invention is grown, has the advantages that of the invention first
In the upper surface metastatic marker graphene of growth substrates, the multiple life of two-dimensional material is especially carried out in the upper surface of growth substrates
When long, label graphene can mark the observation area after two-dimensional material growth each time well, may be implemented to two-dimentional material
The growing state of material carries out that observation is precisely located；The growth of atomic force microscope location observation two-dimensional material is used in the present invention
Situation does not have strict requirements to the growth conditions of two-dimensional material layer, and operation is simple, and testing cost is lower；It is served as a contrast in growth
When the upper surface at bottom carries out the multiple growth of two-dimensional material, the growth conditions of the every secondary growth of two-dimensional material can be different, Ke Yishi
Location observation now is carried out in the growing state of the same area under different growth conditions to two-dimensional material.
Detailed description of the invention
Fig. 1 is shown as the flow chart of the positioning observing method of two-dimensional material growth provided by the invention.
Fig. 2 to Fig. 7 is shown as each step resulting structures in the positioning observing method of two-dimensional material growth provided by the invention
Schematic cross-section.
Component label instructions
10 label graphenes
101 highly oriented pyrolytic graphite alkene
20 growth substrates
30 two-dimensional materials
S1~S4 step
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Fig. 1 is please referred to Fig. 7.It should be noted that diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, though only show in diagram with related component in the present invention rather than package count when according to actual implementation
Mesh, shape and size are drawn, when actual implementation form, quantity and the ratio of each component can arbitrarily change for one kind, and its
Assembly layout form may also be increasingly complex.
Referring to Fig. 1, the present invention provides a kind of positioning observing method of two-dimensional material growth, the two-dimensional material growth
Positioning observing method includes the following steps:
1) label graphene is obtained；
2) growth substrates are provided, and the label graphene is transferred to the upper surface of the growth substrates；
3) upper surface of Yu Suoshu growth substrates grows two-dimensional material；
It 4) is that label carries out location observation to the two-dimensional material with the label graphene.
In step 1), S1 step and Fig. 2 in Fig. 1 are please referred to, obtains label graphene 10.
As an example, the label graphene 10 will not deform under the conditions of the growth temperature of subsequent two-dimensional material or
It disappears, for example, when the subsequent two-dimensional material is graphene, under the conditions of 900 DEG C~1200 DEG C of graphene growth temperature,
The label graphene 10 will not deform or disappear.
As an example, the label graphene 10 may include highly oriented pyrolytic graphite alkene, specifically, can be using machinery
Stripping method is torn from a bulk of highly oriented pyrolytic graphite alkene takes a fritter highly oriented pyrolytic graphite alkene as the label graphene.
As an example, the label graphene 10 includes multi-layer graphene, single-layer graphene, in the present embodiment, it is preferred that
The label graphene 10 is multi-layer graphene.
In step 2), the S2 step and Fig. 3 to Fig. 4 in Fig. 1 are please referred to, growth substrates 20 are provided, and by the label
Graphene 10 is transferred in the growth substrates 20.
As an example, the growth substrates 20 may include that can grow including graphene, boron nitride or transition metal two
The substrate of the two-dimensional materials such as chalcogenide.
As an example, the material of the growth substrates 20 may include monocrystalline silicon, polysilicon, germanium, copper, nickel or platinum etc..
As an example, at any position for the upper surface that the target graphene 10 can be located at the growth substrates 20.
As an example, in step 2), after the label graphene 10 is transferred to the upper surface of the growth substrates 20,
Further include the steps that making annealing treatment the growth substrates 20.
As an example, include annealing under vacuum annealing or normal pressure protective atmosphere to the method for the growth substrates 20 annealing,
The growth substrates 20 can be placed under vacuum environment and be annealed, the growth substrates 20 can also be placed in protection gas
It anneals under condition of normal pressure under atmosphere (for example, inert gas shielding atmosphere or nitrogen protection atmosphere etc.).
As an example, further including the step cleaned to the growth substrates 20 after annealing to the growth substrates 20
Suddenly.
As an example, the method cleaned to the growth substrates 20 includes that the growth substrates 20 are respectively placed in third
Successively it is cleaned by ultrasonic in ketone and alcohol；First the growth substrates 20 can be placed in acetone and be cleaned by ultrasonic, so
The growth substrates 20 after acetone cleaning are placed in alcohol again afterwards and are cleaned by ultrasonic.
As an example, the time being cleaned by ultrasonic to the growth substrates 20 can set according to actual needs,
The growth substrates 20 are placed in the time being cleaned by ultrasonic in the acetone and are placed in the growth substrates 20 described
The time being cleaned by ultrasonic in alcohol can be set according to actual needs；Preferably, in the present embodiment, by the life
The total time that long substrate 20 is cleaned by ultrasonic may include 5~15 minutes.Certainly, in other examples, or by institute
Stating growth substrates 20 and being placed in time for being cleaned by ultrasonic in the acetone is 5~15 minutes, and the growth substrates 20 are set
The time being cleaned by ultrasonic in the alcohol is 5~15 minutes.
In step 3), S3 step and Fig. 5 in Fig. 1 are please referred to, the upper surface of Yu Suoshu growth substrates 10 grows two dimension
Material 30.
As an example, the two-dimensional material 30 may include two chalcogenide of graphene, boron nitride and transition metal；It is preferred that
Ground, in the present embodiment, the two-dimensional material 30 is graphene.
It is grown as an example, can use but be not limited only to chemical vapour deposition technique in the upper surface of the growth substrates 10
The two-dimensional material 30.
In step 4), the S4 step in Fig. 1 is please referred to, is label to the two-dimensional material with the label graphene 10
30 carry out location observation.
As an example, location observation can be carried out using growing state of the atomic force microscope to the two-dimensional material 30；
Preferably, in the present embodiment, using the atomic force microscope to the growth feelings of the two-dimensional material 30 under lateral force mode
Condition is observed.
It further include repeating step 3)~step 4) at least once after step 4) as an example, please referring to Fig. 6~Fig. 7
Step.Specifically, step 3)~step 4) can be repeated repeatedly after step 4), until the two-dimensional material 30 of growth is complete
Cover the exposed upper surface of the growth substrates 20.Fig. 6 is to carry out the two-dimensional material in the upper surface of the growth substrates 20
The schematic perspective view of resulting structures after 30 the second secondary growth, Fig. 7 is in the upper surface of the growth substrates 20 progress institute
The multiple growth of two-dimensional material 30 is stated after the exposed upper surface of the growth substrates 20 is completely covered in the two-dimensional material 30
The schematic perspective view of resulting structures.
As an example, during carrying out the multiple growth of the two-dimensional material 30 in the growth substrates 20, it is described
The growth conditions of the every secondary growth of two-dimensional material 30 can be different.Certainly, the growth conditions of the every secondary growth of the two-dimensional material 30
It can be identical.
As an example, being repeatedly observed to the growing state of described 30 the same area of two-dimensional material, i.e., in observation process
To the two-dimensional material 30 when after every secondary growth to the growing state progress location observation of the two-dimensional material 30
The growing state of the same area carries out location observation.
In conclusion the positioning observing method of two-dimensional material growth of the present invention, the location observation of the two-dimensional material growth
Method includes the following steps: 1) to obtain label graphene；2) growth substrates are provided, and described in the label graphene is transferred to
The upper surface of growth substrates；3) upper surface of Yu Suoshu growth substrates grows two-dimensional material；It 4) is mark with the label graphene
Note carries out location observation to the two-dimensional material.The positioning observing method of two-dimensional material growth of the invention is prior to growth substrates
Upper surface metastatic marker graphene marks stone especially when the upper surface of growth substrates carries out the multiple growth of two-dimensional material
Black alkene can mark the observation area after two-dimensional material growth each time well, and the growing state to two-dimensional material may be implemented
It carries out that observation is precisely located；The growing state that atomic force microscope location observation two-dimensional material is used in the present invention, to two dimension
The growth conditions of material layer does not have strict requirements, and operation is simple, and testing cost is lower；The upper surface of growth substrates into
When the multiple growth of row two-dimensional material, the growth conditions of the every secondary growth of two-dimensional material can be different, may be implemented to two-dimensional material
Location observation is carried out in the growing state of the same area under different growth conditions.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (13)
1. a kind of positioning observing method of two-dimensional material growth, which is characterized in that the location observation side of the two-dimensional material growth
Method includes the following steps:
1) label graphene is obtained；
2) growth substrates are provided, and the label graphene is transferred to the upper surface of the growth substrates；
3) upper surface of Yu Suoshu growth substrates grows two-dimensional material；
It 4) is that label carries out location observation to the two-dimensional material with the label graphene.
2. the positioning observing method of two-dimensional material growth according to claim 1, which is characterized in that in step 1), use
Mechanical stripping method obtains the label graphene from highly oriented pyrolytic graphite alkene.
3. the positioning observing method of two-dimensional material growth according to claim 1, which is characterized in that the label graphene
Including multi-layer graphene.
4. the positioning observing method of two-dimensional material growth according to claim 1, which is characterized in that the growth substrates
Material includes monocrystalline silicon, polysilicon, germanium, copper, nickel or platinum.
5. the positioning observing method of two-dimensional material growth according to claim 1, which is characterized in that step 2) and step 3)
Between further include the steps that making annealing treatment the growth substrates.
6. the positioning observing method of two-dimensional material growth according to claim 5, which is characterized in that the growth substrates
The method of annealing includes annealing under vacuum annealing or normal pressure protective atmosphere.
7. the positioning observing method of two-dimensional material growth according to claim 5, which is characterized in that the growth substrates
Further include the steps that cleaning the growth substrates after annealing and before step 3).
8. the positioning observing method of two-dimensional material growth according to claim 7, which is characterized in that the growth substrates
The method cleaned includes that the growth substrates are respectively placed in acetone and alcohol to be successively cleaned by ultrasonic.
9. the positioning observing method of two-dimensional material growth according to claim 8, which is characterized in that the growth substrates
The time being cleaned by ultrasonic includes 5~15 minutes.
10. the positioning observing method of two-dimensional material growth according to claim 1, which is characterized in that the two-dimensional material
Including two chalcogenide of graphene, boron nitride or transition metal.
11. the positioning observing method of two-dimensional material growth according to claim 1, which is characterized in that in step 4), use
Atomic force microscope is observed the two-dimensional material under lateral force mode.
12. the positioning observing method of two-dimensional material growth according to claim 1, which is characterized in that after step 4) also
Include the steps that repeating step 3)~step 4) at least once.
13. the positioning observing method of two-dimensional material growth according to claim 12, which is characterized in that multiple observation process
In, the growing state of described two-dimensional material the same area is observed.
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Application publication date: 20190614 |