CN112678810A - Method for preparing high-mobility n-type single-layer sulfur-doped graphene film - Google Patents
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Abstract
The invention discloses a method for preparing an n-type single-layer sulfur-doped graphene film with high mobility, and belongs to the technical field of semiconductor material preparation. The preparation method takes dibenzyl disulfide as a carbon source and a sulfur source at the same time, takes hydrogen/argon as carrier gas, and adopts a chemical vapor deposition method of a double-temperature zone to prepare a single-layer sulfur-doped graphene film on a copper foil substrate; the single-layer sulfur-doped graphene film prepared by the invention has a typical n-type transport characteristic in air and has excellent mobility.
Description
1. Field of the invention
The invention belongs to the technical field of semiconductor material preparation, and particularly relates to a method for preparing an n-type single-layer sulfur-doped graphene film with high mobility.
2. Background of the invention
Among the current numerous two-dimensional materials, graphene has been the focus of research due to its unique structure and properties. Graphene is a zero-forbidden-band semiconductor, and shows p-type transport characteristics due to the adsorption (hole doping) of oxygen/water molecules in the air, so that the stable n-type graphene in the air obtained by adjusting a band gap structure can effectively promote the application of the graphene in the fields of electrons, electrochemistry and the like.
Among many attempts, substitutional doping is considered as an effective and stable method for regulating the energy band structure of graphene. In the current development, nitrogen-doped graphene has been widely studied. Compared with nitrogen, sulfur theoretically means stronger electron donating ability (electron doping) for graphene structure, but experimental studies are still less, which is mainly that the diameters of sulfur and carbon atoms are more different than those of nitrogen atom, which means that more energy is needed to replace carbon atom in six-membered ring, which brings difficulty to growth, especially thin film growth. More noteworthy, the sulfur-doped graphene thin film (mainly existing in a thiophenic sulfur structure) reported so far still exhibits p-type transport characteristics in air, which means that electrons given by the thiophenic sulfur-doped structure are not enough to counteract holes given by adsorbed oxygen/water molecules.
Therefore, a sulfur-doped structure with stronger electron donating capability is researched, the controllable preparation of the stable n-type sulfur-doped graphene in the air is realized, and the method has important research significance in both basic research and practical application.
3. Summary of the invention
The invention aims to: the method for preparing the n-type single-layer sulfur-doped graphene film with high mobility is provided, so that the physical characteristics of graphene are enriched, and the application of the graphene in the fields of electronics, electrochemistry and the like is expanded.
The technical scheme adopted by the invention is as follows:
a method for preparing an n-type single-layer sulfur-doped graphene thin film with high mobility comprises the following steps:
(1) cleaning the copper foil: soaking the copper foil in 10 percent (volume fraction) hydrochloric acid solution for 2min, and then placing the copper foil in deionized water for cleaning; replacing the deionized water for many times to remove the residual hydrochloric acid on the surface of the copper foil; then the copper foil is placed in ethanol to remove water on the surface of the copper foil, and finally, the copper foil is dried by dry nitrogen.
(2) Placing dibenzyl disulfide and copper foil in a first temperature zone and a second temperature zone of a tube furnace respectively, and vacuumizing the back to 7x10-4And Pa, carrying out sulfur-doped graphene growth.
(3) Heating the second temperature zone to 700 ℃ in a hydrogen/argon atmosphere, and preserving heat for 20 min;
(4) in the atmosphere of hydrogen/argon, the first temperature zone is heated to 150-1050 ℃, and the second temperature zone is heated to 900-300 ℃;
(5) in a hydrogen/argon atmosphere, keeping the temperature of the two temperature zones for 30min to perform sulfur-doped graphene growth, and then naturally cooling to room temperature to obtain the sulfur-doped graphene material;
(6) and transferring the prepared graphene from the copper foil to a silicon dioxide/silicon substrate by a traditional PMMA wet method for further structural and electrical characterization. The method comprises the following specific steps: cutting the copper foil with the graphene into a required shape, sealing the edge of the copper foil with the graphene by using an adhesive tape, fixing the copper foil on PET (polyethylene terephthalate), and spin-coating the copper foil with a PMMA (polymethyl methacrylate) solution (PMMA powder with the mass ratio of about 3 percent is dissolved in ethyl lactate) on the front surface of the graphene/copper foil; spin-coating at 1000rpm for 10s and spin-coating at 3000rpm for 30s, hardening at 120 deg.C for 10min, cutting off the tapes on the four sides of the copper foil, and taking off the PET at the bottom; putting the copper foil into 1mol/L ferric chloride aqueous solution for surface treatment for 5min, clamping the copper foil by using a forceps, washing the bottom by using deionized water, and removing bottom graphene; putting the substrate in the ferric chloride aqueous solution again to corrode the copper substrate, wherein the corrosion time is generally 1.5-6 h; washing the film with deionized water for 3 times, and soaking for 10min each time; finally, the film is fished up by a silicon chip and is dried by a hot plate in sequence according to the conditions of 50-15 min, 80-5 min and 100-5 min; and (3) removing the PMMA glue by changing acetone twice, soaking the acetone twice for 10min, respectively soaking the acetone twice for 10min in isopropanol and deionized water for 10min, and drying the soaked acetone by using a nitrogen gun.
The invention adopts dibenzyl disulfide as a carbon source and a sulfur source at the same time so as to allow sulfur-doped graphene to grow.
Further, in the step (2), the amount of dibenzyldisulfide is 0 to 5 mg.
Further, in the step (2), the copper foil has a size of 1x1cm2。
Further, in step (3), the hydrogen/argon gas flow rate was 500/500 sccm.
Further, in step (4), the hydrogen/argon gas flow rate was 500/500 sccm.
Further, in step (5), the hydrogen/argon gas flow rate was 500/500 sccm.
Further, in the step (6), the silicon dioxide/silicon substrate transferred with the graphene is annealed for 10-60min at the low temperature of 300-450 ℃, so that PMMA is removed more cleanly, and subsequent characterization tests and application are facilitated.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. in the invention, dibenzyl disulfide is used as a carbon source and a sulfur source at the same time, and a preparation mode of a double-temperature zone is adopted, wherein dibenzyl disulfide is placed in a first temperature zone, and a growing copper foil is placed in a second temperature zone; compared with an independent carbon source and an independent sulfur source, the method is simpler and is more convenient to operate.
2. The single-layer sulfur-doped graphene film prepared by the method disclosed by the invention has a typical n-type transport characteristic in air, and the sulfur-doped structure synthesized by the growth method is mainly a thiol Structure (SH).
3. The single-layer sulfur-doped graphene film prepared by the method has excellent mobility reaching 750cm below zero2V- 1S-1。
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic view of an apparatus for preparing a single-layer sulfur-doped graphene film according to the present invention;
fig. 2 is an optical microscope image of a single layer sulfur-doped graphene thin film prepared in example 1, with a scale of 100 μm;
fig. 3 is a raman spectrum of the single-layer sulfur-doped graphene thin film prepared in example 1;
fig. 4 is a high resolution S2pXPS spectrum of the single layer sulfur-doped graphene thin film prepared in example 1;
fig. 5 is a transfer characteristic curve diagram of the field-effect transistor of the single-layer sulfur-doped graphene film prepared in example 1, wherein the source-drain voltage is 1V.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The method for preparing the n-type single-layer sulfur-doped graphene film with high mobility, provided by the preferred embodiment of the invention, comprises the following specific steps:
cleaning the copper foil: soaking the copper foil in 10 percent (volume fraction) hydrochloric acid solution for 2min, and then placing the copper foil in deionized water for cleaning; replacing the deionized water for many times to remove the residual hydrochloric acid on the surface of the copper foil; then the copper foil is placed in ethanol to remove water on the surface of the copper foil, and finally, the copper foil is dried by dry nitrogen.
Dibenzyl disulfide (1mg) and copper foil were placed in the first and second temperature zones, respectively, in a tube furnace as shown in fig. 1. Back vacuum was pulled to 7x10-4And Pa, carrying out sulfur-doped graphene growth.
The second temperature zone was heated to 700 ℃ under hydrogen/argon atmosphere (500/500sccm) and held for 20 min.
The first temperature zone was heated to 250 ℃ and the second temperature zone to 1000 ℃ under a hydrogen/argon atmosphere (500/500 sccm).
And (3) keeping the two temperature zones at the temperature of 500/500sccm for 30min under a hydrogen/argon atmosphere to grow the sulfur-doped graphene, and naturally cooling to room temperature to obtain the sulfur-doped graphene.
And transferring the prepared graphene from the copper foil to a silicon dioxide/silicon substrate by a traditional PMMA wet method for further structural and electrical characterization. The method comprises the following specific steps: cutting the copper foil with the graphene into a required shape, sealing the edge of the copper foil with the graphene by using an adhesive tape, fixing the copper foil on PET (polyethylene terephthalate), and spin-coating the copper foil with a PMMA (polymethyl methacrylate) solution (PMMA powder with the mass ratio of about 3 percent is dissolved in ethyl lactate) on the front surface of the graphene/copper foil; spin-coating at 1000rpm for 10s and spin-coating at 3000rpm for 30s, hardening at 120 deg.C for 10min, cutting off the tapes on the four sides of the copper foil, and taking off the PET at the bottom; putting the copper foil into 1mol/L ferric chloride aqueous solution for surface treatment for 5min, clamping the copper foil by using a forceps, washing the bottom by using deionized water, and removing bottom graphene; putting the substrate in the ferric chloride aqueous solution again to corrode the copper substrate, wherein the corrosion time is generally 1.5-6 h; washing the film with deionized water for 3 times, and soaking for 10min each time; finally, the film is fished up by a silicon chip and is dried by a hot plate in sequence according to the conditions of 50-15 min, 80-5 min and 100-5 min; changing acetone twice to remove PMMA glue, soaking the acetone twice for 10min respectively, soaking the acetone twice for 10min in isopropanol and soaking the acetone twice in deionized water for 10min, and drying the acetone twice by using a nitrogen gun; and finally, annealing the silicon dioxide/silicon substrate with the graphene at the low pressure of 350 ℃ for 30 min.
Example 1 typical optical microscopy pictures of single layer sulfur doped graphene thin films grown as shown in fig. 2, show good uniformityAnd (5) consistency. Fig. 3 is a raman spectrum of a typical single-layer sulfur-doped graphene film, where the D and G' peaks are caused by sulfur doping, and the intensity ratio of the G and 2D peaks is-0.5, showing a single-layer graphene structure. Fig. 4 is a high resolution S2pXPS spectrum of a typical single layer sulfur doped graphene film with a total sulfur doping concentration of-2.4 at%, where the thiol Structure (SH) reaches-79%. FIG. 5 is a transfer characteristic curve (air room temperature test) of a field effect transistor with a single-layer sulfur-doped graphene film as a channel, wherein the Dirac point is-15V, which shows that the film is a typical n-type transport characteristic in air, and further, the mobility of the film can reach 750cm2V-1S-1。
Example 2
The method for preparing the n-type single-layer sulfur-doped graphene film with high mobility, provided by the preferred embodiment of the invention, comprises the following specific steps:
cleaning the copper foil: soaking the copper foil in 10 percent (volume fraction) hydrochloric acid solution for 2min, and then placing the copper foil in deionized water for cleaning; replacing the deionized water for many times to remove the residual hydrochloric acid on the surface of the copper foil; then the copper foil is placed in ethanol to remove water on the surface of the copper foil, and finally, the copper foil is dried by dry nitrogen.
Dibenzyl disulfide (1mg) and copper foil were placed in the first and second temperature zones, respectively, in a tube furnace as shown in fig. 1. Back vacuum was pulled to 7x10-4And Pa, carrying out sulfur-doped graphene growth.
The second temperature zone was heated to 700 ℃ under hydrogen/argon atmosphere (500/500sccm) and held for 20 min.
The first temperature zone was heated to 250 ℃ and the second temperature zone was heated to 950 ℃ under a hydrogen/argon atmosphere (500/500 sccm).
And (3) keeping the two temperature zones at the temperature of 500/500sccm for 30min under a hydrogen/argon atmosphere to grow the sulfur-doped graphene, and naturally cooling to room temperature to obtain the sulfur-doped graphene.
And transferring the prepared graphene from the copper foil to a silicon dioxide/silicon substrate by a traditional PMMA wet method for further structural and electrical characterization. The method comprises the following specific steps: cutting the copper foil with the graphene into a required shape, sealing the edge of the copper foil with the graphene by using an adhesive tape, fixing the copper foil on PET (polyethylene terephthalate), and spin-coating the copper foil with a PMMA (polymethyl methacrylate) solution (PMMA powder with the mass ratio of about 3 percent is dissolved in ethyl lactate) on the front surface of the graphene/copper foil; spin-coating at 1000rpm for 10s and spin-coating at 3000rpm for 30s, hardening at 120 deg.C for 10min, cutting off the tapes on the four sides of the copper foil, and taking off the PET at the bottom; putting the copper foil into 1mol/L ferric chloride aqueous solution for surface treatment for 5min, clamping the copper foil by using a forceps, washing the bottom by using deionized water, and removing bottom graphene; putting the substrate in the ferric chloride aqueous solution again to corrode the copper substrate, wherein the corrosion time is generally 1.5-6 h; washing the film with deionized water for 3 times, and soaking for 10min each time; finally, the film is fished up by a silicon chip and is dried by a hot plate in sequence according to the conditions of 50-15 min, 80-5 min and 100-5 min; changing acetone twice to remove PMMA glue, soaking the acetone twice for 10min respectively, soaking the acetone twice for 10min in isopropanol and soaking the acetone twice in deionized water for 10min, and drying the acetone twice by using a nitrogen gun; and finally, annealing the silicon dioxide/silicon substrate with the graphene at the low pressure of 350 ℃ for 30 min.
The sulfur doping concentration of the single-layer sulfur-doped graphene thin film grown in the embodiment 2 is-1.1 at%, which means that the sulfur doping concentration of the graphene can be adjusted and controlled by the change of the growth temperature.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A method for preparing an n-type single-layer sulfur-doped graphene film with high mobility is characterized by comprising the following steps:
(1) cleaning the copper foil: soaking the copper foil in 10 percent (volume fraction) hydrochloric acid solution for 2min, and then placing the copper foil in deionized water for cleaning; replacing the deionized water for many times to remove the residual hydrochloric acid on the surface of the copper foil; then the copper foil is placed in ethanol to remove water on the surface of the copper foil, and finally, the copper foil is dried by dry nitrogen.
(2) Placing dibenzyl disulfide and copper foil in a first temperature zone and a second temperature zone of a tube furnace respectively, and vacuumizing the back to 7x10-4And Pa, carrying out sulfur-doped graphene growth.
(3) Heating the second temperature zone to 700 ℃ in a hydrogen/argon atmosphere, and preserving heat for 20 min;
(4) in the atmosphere of hydrogen/argon, the first temperature zone is heated to 150-1050 ℃, and the second temperature zone is heated to 900-300 ℃;
(5) in a hydrogen/argon atmosphere, keeping the temperature of the two temperature zones for 30min to perform sulfur-doped graphene growth, and then naturally cooling to room temperature to obtain the sulfur-doped graphene material;
(6) and transferring the prepared graphene from the copper foil to a silicon dioxide/silicon substrate by a traditional PMMA wet method for further structural and electrical characterization. The method comprises the following specific steps: cutting the copper foil with the graphene into a required shape, sealing the edge of the copper foil with the graphene by using an adhesive tape, fixing the copper foil on PET (polyethylene terephthalate), and spin-coating the copper foil with a PMMA (polymethyl methacrylate) solution (PMMA powder with the mass ratio of about 3 percent is dissolved in ethyl lactate) on the front surface of the graphene/copper foil; spin-coating at 1000rpm for 10s and spin-coating at 3000rpm for 30s, hardening at 120 deg.C for 10min, cutting off the tapes on the four sides of the copper foil, and taking off the PET at the bottom; putting the copper foil into 1mol/L ferric chloride aqueous solution for surface treatment for 5min, clamping the copper foil by using a forceps, washing the bottom by using deionized water, and removing bottom graphene; putting the substrate in the ferric chloride aqueous solution again to corrode the copper substrate, wherein the corrosion time is generally 1.5-6 h; washing the film with deionized water for 3 times, and soaking for 10min each time; finally, the film is fished up by a silicon chip and is dried by a hot plate in sequence according to the conditions of 50-15 min, 80-5 min and 100-5 min; and (3) removing the PMMA glue by changing acetone twice, soaking the acetone twice for 10min, respectively soaking the acetone twice for 10min in isopropanol and deionized water for 10min, and drying the soaked acetone by using a nitrogen gun.
2. The method for preparing the high-mobility n-type single-layer sulfur-doped graphene thin film according to claim 1, wherein: in the step (2), dibenzyl disulfide is simultaneously used as a carbon source and a sulfur source, and the mass of the dibenzyl disulfide is 0-5 mg.
3. The method for preparing the high-mobility n-type single-layer sulfur-doped graphene thin film according to claim 1, wherein: in the step (2), the size of the copper foil substrate is 1x1cm2。
4. The method for preparing the high-mobility n-type single-layer sulfur-doped graphene thin film according to claim 1, wherein: in the step (3), the hydrogen/argon flow rate was 500/500 sccm.
5. The method for preparing the high-mobility n-type single-layer sulfur-doped graphene thin film according to claim 1, wherein: in the step (4), the flow rate of hydrogen/argon gas was 500/500 sccm.
6. The method for preparing the high-mobility n-type single-layer sulfur-doped graphene thin film according to claim 1, wherein: in the step (5), the hydrogen/argon flow rate was 500/500 sccm.
7. The method for preparing the high-mobility n-type single-layer sulfur-doped graphene thin film according to claim 1, wherein: in the step (6), the silicon dioxide/silicon substrate transferred with the graphene is annealed for 10-60min at the low temperature of 300-450 ℃, so that PMMA is removed more cleanly, and subsequent characterization test and application are facilitated.
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| CN102597336A (en) * | 2009-08-07 | 2012-07-18 | 格尔德殿工业公司 | Large area deposition and doping of graphene, and products including the same |
| US20140234200A1 (en) * | 2010-03-08 | 2014-08-21 | William Marsh Rice University | Growth of graphene films from non-gaseous carbon sources |
| CN103172057A (en) * | 2013-03-07 | 2013-06-26 | 华南理工大学 | Preparation method of nitrogen and sulfur co-doped graphene |
| CN104528699A (en) * | 2014-12-22 | 2015-04-22 | 中国科学院重庆绿色智能技术研究院 | Stable doping method for graphene thin film |
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Application publication date: 20210420 |