CN109987597B - Preparation method of heterogeneously stacked graphene - Google Patents
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 178
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B2204/00—Structure or properties of graphene
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Abstract
The invention discloses a preparation method of heterosexual stacked graphene, which comprises the following steps: preparing an insulating or semiconductor substrate; preparing a nickel layer and a doped carbon source layer which are distributed in a layered manner on the surface of a substrate, and enabling the nickel layer to be in direct contact with the doped carbon source layer; heating the doped carbon source layer to enable carbon to be fused into the nickel layer, and then cooling the doped carbon source layer to enable doped graphene to grow on one side of the nickel layer and pure graphene to grow on the other side of the nickel layer; and annealing and evaporating the nickel layer to ensure that the doped graphene and the pure graphene are distributed in a layered manner and are in contact with each other. Layered doped graphene and pure graphene grow on an insulating or semiconductor substrate, so that the subsequent transfer step is avoided, and the doped graphene and the pure graphene are prevented from being damaged.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to a preparation method of heterosexual stacked graphene, and belongs to the field of graphene production.
[ background of the invention ]
In 2004, two scientists at manchester university, uk, discovered graphene using a micromechanical lift-off method and obtained a nobel prize in 2010. Graphene is a carbon atom through sp2The new two-dimensional honeycomb carbonaceous material which is tightly arranged in a regular hexagon in a hybridization mode has the single-layer thickness of only 0.335 nm. Theoretically, graphene exhibits excellent electronic stability, thermal conductivity, optical properties, mechanical properties, and the like. Since the discovery of graphene, the research in the fields of physics and material science has been hot due to its excellent performance and huge market application prospects. Graphene is the thinnest and the hardest nano material at present, has the properties which are not possessed by a plurality of common materials such as good light transmittance, high heat conductivity coefficient, high electron mobility, low resistivity, high mechanical strength and the like, is expected to be widely applied to a plurality of fields such as electrodes, batteries, transistors, touch screens, solar energy, sensors, ultra-light materials, medical treatment, seawater desalination and the like in the future, and is one of the most promising advanced new materials.
The preparation method of the graphene comprises a chemical vapor deposition method, a redox method, a liquid phase stripping method, a mechanical stripping method and the like, but the methods have the defects of complex process, difficult control of process conditions, high requirement on a substrate, poor repeatability, pollution and the like, and are not beneficial to the industrial production of the graphene. The chemical vapor deposition method is one of the most conventional using methods, the traditional preparation method inevitably comprises subsequent transfer, impurity defects and pollution are introduced unavoidably in the transfer process, damage and fracture are caused, the stability, the electrical property and the like of graphene are reduced, and therefore, the subsequent application and preparation of devices are influenced; while lacking precise control over the number of graphene layers and the manner in which they are stacked, control of the doping of foreign heteroatoms into the lattice structure of graphene is particularly difficult. The application of graphene in semiconductor devices requires that the preparation technology of graphene is compatible with a semiconductor process, and doping can improve the performance of graphene, which makes the requirements on the preparation technology of doping more severe.
Therefore, a preparation method which is compatible with a semiconductor process, free of transfer, doping and controllable in the number of layers is urgently needed, the industrial application of graphene is realized, and material and technical support is provided for the microelectronic technology in China to enter the non-silicon CMOS era.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provide a preparation method of heterosexual stacked graphene with controllable layer number.
The technical scheme adopted by the invention is as follows:
a preparation method of stacked graphene with opposite polarities comprises the following steps:
the method comprises the following steps: preparing an insulating or semiconductor substrate;
step two: preparing a nickel layer and a doped carbon source layer which are distributed in a layered manner on the surface of a substrate, and enabling the nickel layer to be in direct contact with the doped carbon source layer;
step three: heating and annealing the doped carbon source layer to enable carbon to be fused into the nickel layer, and then cooling to enable doped graphene to grow on one side of the nickel layer and pure graphene to grow on the other side of the nickel layer;
step IV: and annealing and evaporating the nickel layer to ensure that the doped graphene and the pure graphene are distributed in a layered manner and are in contact with each other.
The invention has the beneficial effects that: layered doped graphene and pure graphene grow on an insulating or semiconductor substrate, so that the subsequent transfer step is avoided, and the doped graphene and the pure graphene are prevented from being damaged. Meanwhile, by utilizing the permeation effect of the nickel layer on carbon atoms and the barrier effect on other non-metal doping elements, part of carbon atoms in the doped carbon source layer penetrate through the nickel layer to reach the other side of the nickel layer, the nickel layer is used as separation, the doped graphene and the pure graphene independently grow in the subsequent growth process without mutual interference, the mutual interference between the doped graphene and the pure graphene is avoided, and the process compatibility is improved.
Summarizing, the present invention has the following advantages:
1. the transfer-free preparation is realized, the excellent performance of the graphene is not damaged, and the graphene can be directly applied to the related field;
2. simultaneously, the controllable preparation of doped and undoped graphene is realized;
3. the preparation technology is compatible with the existing mature semiconductor process, and is beneficial to realizing the industrial application of the graphene material;
4. by continuously superposing the configuration, the continuous and alternate multilayer controllable preparation between doped graphene and undoped graphene is hopefully realized;
5. the preparation method is green, pollution-free, low in cost and high in efficiency.
After the step (IV) is finished, the step (III), and the step (IV) are repeated.
In the second step of the invention, the doped carbon source layer comprises a carbon source layer and a doping layer, and the carbon source layer is positioned between the doping layer and the nickel layer.
In the second step of the invention, the surface of the substrate is firstly coated with doping liquid in a spin mode to form a doping layer, then coated with carbon source liquid to form a carbon source layer, and finally electron beam evaporation Ni is carried out on the surface of the carbon source layer to form a nickel layer, so that a layered distribution structure of the substrate, the doping layer, the carbon source layer and the nickel layer is formed.
In the second step of the invention, electron beam evaporation is carried out on the surface of the substrate to form a nickel layer, and then chemical vapor deposition is carried out on a gaseous carbon source and a gaseous doping source to form a carbon source layer on the surface of the nickel layer.
In the second step of the invention, the doping liquid and the carbon source liquid are mixed and spin-coated on the surface of the nickel layer to form a doping carbon source layer.
The doping element in the doping carbon source layer is one or more of N, S, P and B.
In the step III of the invention, the heating temperature of the doped carbon source layer is 800-900 ℃, and the temperature is kept at 800-900 ℃ for 2-15min, and the cooling rate is 25-30 ℃/min.
The carbon source liquid is PMMA.
Other features and advantages of the present invention will be disclosed in more detail in the following detailed description of the invention and the accompanying drawings.
[ description of the drawings ]
The invention is further described below with reference to the accompanying drawings:
fig. 1 is a diagram of the working steps of a method for preparing heteroleptic stacked graphene according to embodiment 1 of the present invention;
fig. 2 is a photograph of a sample of heteroleptic stacked graphene according to example 1 of the present invention;
fig. 3 is a second photograph of a sample of heteroleptic stacked graphene according to example 1 of the present invention;
fig. 4 is a photograph of three samples of anisotropically stacked graphene in accordance with example 1 of the present invention;
fig. 5 shows raman spectra of samples one, two and three of the heteroleptic stacked graphene of example 1 of the present invention.
[ detailed description ] embodiments
The technical solutions of the embodiments of the present invention are explained and illustrated below with reference to the drawings of the embodiments of the present invention, but the following embodiments are only preferred embodiments of the present invention, and not all embodiments. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative effort belong to the protection scope of the present invention.
In the following description, the appearances of the indicating orientation or positional relationship such as the terms "inner", "outer", "upper", "lower", "left", "right", etc. are only for convenience in describing the embodiments and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and are not to be construed as limiting the present invention.
Example 1:
referring to fig. 1, this embodiment shows a method for preparing stacked heterotropically graphene, including the following steps:
the method comprises the following steps: an insulating or semiconductor substrate is prepared.
Step two: preparing a nickel layer and a doped carbon source layer which are distributed in a layered mode on the surface of the substrate, and enabling the nickel layer and the doped carbon source layer to be in direct contact.
The doped carbon source layer in the embodiment comprises a carbon source layer and a doping layer, and the carbon source layer is positioned between the doping layer and the nickel layer.
The specific preparation method of the nickel layer and the doped carbon source layer comprises the following steps: the surface of the substrate is firstly coated with doping liquid in a spin mode to form a doping layer, then coated with carbon source liquid in a spin mode to form a carbon source layer, and finally electron beams are evaporated on the surface of the carbon source layer to form a nickel layer, so that a layered distribution structure of the substrate, the doping layer, the carbon source layer and the nickel layer is formed.
In this example, the carbon source liquid is PMMA.
The doping element in the doped carbon source layer is one or more of N, S, P and B. For example, the doping liquid may be selected as a nitrogen and sulfur co-doped graphene quantum dot.
Step three: in the presence of Ar: h2Heating the doped carbon source layer to 800-900 ℃ in a gas atmosphere of 10(sccm), preserving heat for 2-15min to enable carbon to be fused into the nickel layer, and then cooling at a speed of 25-30 ℃/min to enable doped graphene to grow on one side of the nickel layer and pure graphene to grow on the other side of the nickel layer.
The heating temperature is not too high, and the too high heating temperature can cause the speed of growing the doped graphene on the doped carbon source layer to be too high, so that the growing speed is far higher than the speed of melting carbon into the nickel layer, and the content of pure graphene in the subsequent segregation growth process is too low, or even the layered pure graphene with an effective structure cannot be formed. In addition, the heating temperature is not suitable to be too low, and the carbon is difficult to enter the nickel layer due to the too low heating temperature, and the PMMA is difficult to grow into graphene. Therefore, in this embodiment, under the condition that the temperature condition that carbon can be fused into the nickel layer is ensured, the temperature and the long heat preservation time are as low as possible, so that enough carbon can be fused into the nickel layer under the condition that the early growth of graphene is inhibited as much as possible, and further, enough carbon can form pure graphene in the subsequent temperature reduction process. In addition, the cooling rate should not be too large or too small. Too fast a cooling rate is difficult to provide enough time to separate out carbon elements in the nickel layer, and the mechanical strength of the doped graphene and the pure graphene is damaged. The too slow cooling rate causes the too fast growth of the pure graphene on the surface of the nickel layer at the early stage, and inhibits the precipitation of carbon element in the subsequent nickel layer.
Step IV: and annealing and evaporating the nickel layer to ensure that the doped graphene and the pure graphene are distributed in a layered manner and are in contact with each other.
In this embodiment, because the separation of nickel layer, the doping element in the doping layer can't cross the nickel layer, and because the nickel layer is to the dissolution of carbon element, in the heating heat preservation process, carbon element in the carbon source layer can move gradually to the nickel layer, later the carbon element in the nickel layer in the cooling process oozes out gradually to the nickel layer and keeps away from one side of doping layer and carries out the segregation growth. Meanwhile, the carbon source layer is in direct contact with the nickel layer, so that the carbon source layer is less hindered by the doping layer in the process of being fused into the nickel layer, and the doping layer and the nickel layer are also hindered by the carbon source layer. And then evaporating the nickel layer at a high temperature to realize the preparation of the layered assembly of the doped graphene and the pure graphene, wherein the pure graphene can be physically settled onto the doped graphene in the evaporation process of the nickel layer, and the pure graphene and the doped graphene are thinner, so that the pure graphene can not be separated after being settled onto the doped graphene to form a physical layered stacked structure, thereby avoiding the formation of chemical bonds between the pure graphene and the doped graphene and generating unnecessary interface effect, and further influencing the respective physicochemical properties of the pure graphene and the doped graphene. In addition, in the evaporation process of nickel, carbon which is not subjected to segregation growth in the nickel layer can be subjected to secondary growth through the space left by the evaporated nickel, so that pure graphene is formed and is combined with the graphene subjected to segregation growth.
Referring to fig. 2 to 5, in order to confirm that the present example can reliably perform the preparation of the layered structures of the doped graphene and the pure graphene, a first sample with a heating temperature of 800 ℃, a second sample with a heating temperature of 850 ℃, and a third sample with a heating temperature of 900 ℃ were respectively prepared, and the raman spectra of the three samples were measured to be 1350cm-1、1575cm-1And 2700cm-1Characteristic peak positions are formed, indicating the effective formation of graphene.
Example 2:
the embodiment shows a preparation method of heterosexual stacked graphene, which comprises the following steps:
the method comprises the following steps: an insulating or semiconductor substrate is prepared.
Step two: preparing a nickel layer and a doped carbon source layer which are distributed in a layered mode on the surface of the substrate, and enabling the nickel layer and the doped carbon source layer to be in direct contact.
The specific preparation method of the nickel layer and the doped carbon source layer comprises the following steps: and performing electron beam evaporation on the surface of the substrate to form a nickel layer. And mixing the doping liquid and the carbon source liquid, and spin-coating the mixture on the surface of the nickel layer to form a doping carbon source layer.
Step three: and heating the doped carbon source layer to enable carbon to be fused into the nickel layer, and then cooling the doped carbon source layer to enable doped graphene to grow on one side of the nickel layer and pure graphene to grow on the other side of the nickel layer.
Step IV: and annealing and evaporating the nickel layer to ensure that the doped graphene and the pure graphene are distributed in a layered manner and are in contact with each other.
The difference between this embodiment and embodiment 1 is that, since the doping liquid and the carbon source liquid are uniformly in contact with the nickel layer, although the doping element has a certain effect on hindering carbon during the penetration of carbon into the nickel layer, a relatively low distance is maintained between carbon and the nickel layer, and thus the penetration rate of carbon is not greatly affected. Meanwhile, the method is more beneficial to the contact of the doping element and the nickel layer, and is more beneficial to the growth of the doped graphene in the follow-up process.
Example 3:
this example differs from example 1 in that: and fourthly, repeating the third step, the fourth step and the fourth step after the fourth step is finished. The above steps are repeated to form a periodic layered structure of the substrate, the doped graphene, the pure graphene, the doped graphene and the pure graphene.
Example 4:
the embodiment shows a preparation method of heterosexual stacked graphene, which comprises the following steps:
the method comprises the following steps: an insulating or semiconductor substrate is prepared.
Step two: preparing a nickel layer and a doped carbon source layer which are distributed in a layered mode on the surface of the substrate, and enabling the nickel layer and the doped carbon source layer to be in direct contact.
The specific preparation method of the nickel layer and the doped carbon source layer comprises the following steps: and performing electron beam evaporation on the surface of the substrate to form a nickel layer, and then performing chemical vapor deposition on a gaseous carbon source and a gaseous doping source to form a doped carbon source layer on the surface of the nickel layer. Meanwhile, nickel can catalyze the growth of graphene in the chemical vapor deposition process.
In addition, since the substrate is made of insulating or semiconductor material, if the surface of the nickel layer cannot be ensured to form graphene by vapor deposition on the substrate surface, and then the nickel layer is prepared, the result is uncontrollable, so that the nickel layer is prepared first in the case of vapor deposition.
Step three: and heating the doped carbon source layer to enable carbon to be fused into the nickel layer, and then cooling the doped carbon source layer to enable doped graphene to grow on one side of the nickel layer and pure graphene to grow on the other side of the nickel layer.
Step IV: and annealing and evaporating the nickel layer to ensure that the doped graphene and the pure graphene are distributed in a layered manner and are in contact with each other.
While the invention has been described with reference to specific embodiments thereof, it will be understood by those skilled in the art that the invention is not limited thereto, and may be embodied in many different forms without departing from the spirit and scope of the invention as set forth in the following claims. Any modification which does not depart from the functional and structural principles of the present invention is intended to be included within the scope of the claims.
Claims (4)
1. A preparation method of heterosexual stacked graphene is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: preparing an insulating or semiconductor substrate;
step two: preparing a nickel layer and a doped carbon source layer which are distributed in a layered manner on the surface of a substrate, and enabling the nickel layer to be in direct contact with the doped carbon source layer;
step three: heating and annealing the doped carbon source layer to enable carbon to be fused into the nickel layer, and then cooling to enable doped graphene to grow on one side of the nickel layer and pure graphene to grow on the other side of the nickel layer;
step IV: annealing and evaporating the nickel layer to ensure that the doped graphene and the pure graphene are distributed in a layered manner and are mutually contacted;
in the third step, the heating temperature of the doped carbon source layer is 800-900 ℃, and the temperature is kept at 800-900 ℃ for 2-15min, and the cooling rate is 25-30 ℃/min;
in the second step, the doped carbon source layer comprises a carbon source layer and a doping layer, and the carbon source layer is positioned between the doping layer and the nickel layer;
and secondly, spin-coating doping liquid on the surface of the substrate to form a doping layer, spin-coating carbon source liquid to form a carbon source layer, and finally performing electron beam evaporation on Ni on the surface of the carbon source layer to form a nickel layer so as to form a layered distribution structure of the substrate, the doping layer, the carbon source layer and the nickel layer.
2. The method for preparing stacked anisotropic graphene according to claim 1, wherein: and fourthly, repeating the third step, the fourth step and the fourth step after the fourth step is finished.
3. The method for preparing stacked anisotropic graphene according to claim 1, wherein: the doping element in the doped carbon source layer is one or more of N, S, P and B.
4. The method for preparing stacked anisotropic graphene according to claim 1, wherein: the carbon source liquid is PMMA.
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Effective date of registration: 20220831 Address after: Room 2202, 22 / F, Wantong building, No. 3002, Sungang East Road, Sungang street, Luohu District, Shenzhen City, Guangdong Province Patentee after: Shenzhen dragon totem technology achievement transformation Co.,Ltd. Address before: 315211, Fenghua Road, Jiangbei District, Zhejiang, Ningbo 818 Patentee before: Ningbo University |
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Effective date of registration: 20240710 Address after: 442000 Unit 201, Building 1, Group 2, Xiaochangpo Village, Chengguan Town, Yunxi County, Shiyan City, Hubei Province Patentee after: Yunxi Mineng Biological Group Co.,Ltd. Country or region after: China Address before: Room 2202, 22 / F, Wantong building, No. 3002, Sungang East Road, Sungang street, Luohu District, Shenzhen City, Guangdong Province Patentee before: Shenzhen dragon totem technology achievement transformation Co.,Ltd. Country or region before: China |