CN105239136A - Electrophoretic deposition preparation method for graphene thin film modified by black phosphorus quantum dots - Google Patents
Electrophoretic deposition preparation method for graphene thin film modified by black phosphorus quantum dots Download PDFInfo
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- CN105239136A CN105239136A CN201510587559.3A CN201510587559A CN105239136A CN 105239136 A CN105239136 A CN 105239136A CN 201510587559 A CN201510587559 A CN 201510587559A CN 105239136 A CN105239136 A CN 105239136A
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- black phosphorus
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Abstract
The invention discloses an electrophoretic deposition preparation method for a graphene thin film modified by black phosphorus quantum dots. Firstly, the black phosphorus quantum dots prepared through liquid phase ultrasound are added to organic solvent dispersion liquid of graphene oxide, and the black phosphorus quantum dots are fully absorbed onto the surface of the graphene oxide by adopting water bath ultrasonic mixing. Then a conducting substrate and a graphite rod serving as an anode and a cathode respectively are placed in the mixed dispersion liquid with the addition of constant direct voltage, and the graphene oxide with electronegativity is electrophoretically deposited onto the substrate to form a graphene oxide thin film modified by the black phosphorus quantum dots. Finally, after the substrate for depositing the graphene oxide thin film is taken out, the graphene oxide thin film is rinsed thoroughly with ethyl alcohol, and under the protection of argon or nitrogen, the graphene oxide thin film is reduced to the graphene thin film modified by the black phosphorus quantum dots at the high temperature (500 DEG C-1200 DEG C). The electrophoretic deposition preparation method for the graphene thin film modified by the black phosphorus quantum dots has the potential of being simple and easy to operate, and capable of achieving scale preparation.
Description
Technical field
The present invention relates to the electrophoretic deposition preparation method of the graphene film that a kind of black phosphorus alkene quantum dot is modified, belong to nanometer thin films.
Background technology
Two-dimension nano materials, as Graphene, transient metal sulfide etc., shows outstanding application potential electronics, sensing and photoelectric device etc. are multi-field with the physics of its excellence and structural performance.Wherein, Graphene is widely studied as the representational two-dimensional material of most.It has the carrier mobility of superelevation, but shortage band gap seriously hinders Graphene at logic semiconductor devices as the application in field-effect transistor.And as the line-up of delegates of transient metal sulfide semi-conductor family, molybdenumdisulphide (MoS
2) there is obvious band gap, and in n-type transistor, show excellent on-off ratio characteristic (>10
8).But, MoS
2there is the reduction that may cause electronic mobility in middle textural defect, thus affects its electric property.Therefore, more new function two-dimensional semiconductor material is explored still significant.In recent years, there is the black phosphorus alkene of individual layer or few layer black phosphorus atomic shell structure, with carrier mobility (200 ~ 1000cm that it is higher
2v
-1s
-1), adjustable direct band gap, larger on-off ratio characteristic (10
4~ 10
5) and anisotropy etc., become the two-dimensional semiconductor material being applicable to high-performance electronic and opto-electronic device of most potentiality gradually.Therefore, need a kind of synthesis preparation method, black phosphorus alkene and Graphene two kinds of two-dimensional material can be combined, form the matrix material simultaneously with both excellent physical characteristics, the potential application at numerous areas such as electronics, photoelectric device and optics of black phosphorus alkene and graphene composite material will be widened.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art; the invention provides the electrophoretic deposition preparation method of the graphene film that a kind of black phosphorus alkene quantum dot is modified; utilize electrophoretic deposition method as film technique; in addition follow-up reduction step; can realize the graphene film that black phosphorus alkene quantum dot modifies simple, prepare fast, there is low cost, potential prepared by mass-producing.
Technical scheme: for achieving the above object, the technical solution used in the present invention is:
The electrophoretic deposition preparation method of the graphene film that a kind of black phosphorus alkene quantum dot is modified, first the black phosphorus alkene quantum dot of liquid phase ultrasonic preparation is joined in the dispersion in organic solvent containing graphene oxide, adopt the method for water bath sonicator mixing to make black phosphorus alkene quantum dot fully be adsorbed onto the surface of graphene oxide, finally form mixed dispersion liquid; Then be positive pole with conductive substrates, take graphite rod as negative pole, conductive substrates and graphite rod are placed in mixed dispersion liquid, to conductive substrates and the additional constant volts DS of graphite rod, make the graphene oxide electrophoretic deposition of negatively charged on conductive substrates, form the graphene oxide film of black phosphorus alkene quantum dot modification; Finally the conductive substrates of deposited oxide graphene film taken out and clean with alcohol flushing, under argon gas or nitrogen protection, graphene oxide film is reduced to the graphene film that black phosphorus alkene quantum dot is modified by high temperature, and described high temperature is 500 ~ 1200 DEG C.
The method comprises the steps:
(1) the black phosphorus alkene quantum dot of liquid phase ultrasonic preparation is joined in the dispersion in organic solvent containing graphene oxide, adopt the method for water bath sonicator mixing to make black phosphorus alkene quantum dot fully be adsorbed onto the surface of graphene oxide, finally form mixed dispersion liquid; Described organic solvent is dimethyl sulfoxide (DMSO) (DMSO), DMF (DMF), N-Methyl pyrrolidone (NMP), Virahol (IPA), 1-butyl-3-methyl imidazolium tetrafluoroborate [BMIM] [BF
4], NSC 11801 (EC), acetonitrile, 1-butyl-tri-methylimidazolium dicyanamide [BMIM] [N (CN
2)], one in N-ring ethyl-2-tetramethyleneimine;
(2) take conductive substrates as positive pole, take graphite rod as negative pole, conductive substrates and graphite rod are placed in mixed dispersion liquid, to conductive substrates and the additional constant volts DS of graphite rod, make the graphene oxide electrophoretic deposition of negatively charged on conductive substrates, form the graphene oxide film of black phosphorus alkene quantum dot modification; Described volts DS is 0.1 ~ 36V; Described conductive substrates is the one in metal titanium, silicon chip, conductive glass, silicon carbide, goldleaf; Depositing time is 1 ~ 30min;
(3) conductive substrates of deposited oxide graphene film to be taken out and clean with alcohol flushing, under argon gas or nitrogen protection, graphene oxide film is reduced to the graphene film that black phosphorus alkene quantum dot is modified by high temperature, and described high temperature is 500 ~ 1200 DEG C.
Beneficial effect: the electrophoretic deposition preparation method of the graphene film that black phosphorus alkene quantum dot provided by the invention is modified; utilize electrophoretic deposition method as film technique; in addition follow-up reduction step; can realize the graphene film that black phosphorus alkene quantum dot modifies simple, prepare fast, there is low cost, potential prepared by mass-producing.This preparation method utilizes two electrode galvanic deposit systems under liquid phase environment, under additional DC constant voltage condition, makes the graphene oxide electrophoretic deposition of negatively charged to substrate, form the graphene oxide film of black phosphorus alkene quantum dot modification.This simple electrophoretic deposition film technique can be amplified to industrially scalableization further and produce, and thus has extendability and the applicability widely of height.Due to the current preparation method having reported black phosphorus alkene quantum dot and graphene composite film without any document and patent, therefore preparation method of the present invention has filled up this blank, has great application prospect.
Accompanying drawing explanation
Fig. 1 is device schematic diagram prepared by the graphene film adopting the inventive method to carry out the modification of black phosphorus alkene quantum dot; In figure, 1 is substrate on earth, and 2 is Graphite Electrodes, and 3 is container, and 4 is the dispersion in organic solvent of black phosphorus alkene quantum dot and graphene oxide, and 5 is voltage source;
Fig. 2 is the transmission electron microscope photo of the graphene film that the black phosphorus alkene quantum dot adopting the inventive method to prepare is modified.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
(1) first the black phosphorus alkene quantum dot of liquid phase ultrasonic preparation is joined in methyl sulfoxide (DMSO) dispersion in organic solvent containing graphene oxide, adopt the method for water bath sonicator mixing to make black phosphorus alkene quantum dot fully be adsorbed onto the surface of graphene oxide.
(2) then conductive glass and graphite rod are placed in mixed dispersion liquid as positive pole and negative pole, the volts DS that additional 3V is constant, make the graphene oxide electrophoretic deposition of negatively charged to conductive glass, form the graphene oxide film of black phosphorus alkene quantum dot modification, depositing time is 1min.
(3) with the clean film of alcohol flushing after finally the conductive glass of this deposit film being taken out, be the graphene film of black phosphorus alkene quantum dot modification at 500 DEG C of high temperature reductions under argon shield.
Embodiment 2
(1) first the black phosphorus alkene quantum dot of liquid phase ultrasonic preparation is joined in N-Methyl pyrrolidone (NMP) dispersion in organic solvent containing graphene oxide, adopt the method for water bath sonicator mixing to make black phosphorus alkene quantum dot fully be adsorbed onto the surface of graphene oxide.
(2) then silicon chip and graphite rod are placed in mixed dispersion liquid as positive pole and negative pole, the volts DS that additional 10V is constant, make the graphene oxide electrophoretic deposition of negatively charged to silicon chip, form the graphene oxide film of black phosphorus alkene quantum dot modification, depositing time is 5min.
(3) finally by after the silicon chip extracting of this deposit film with the clean film of alcohol flushing, under argon shield 1000 DEG C of high temperature reductions be black phosphorus alkene quantum dot modify graphene film.
Embodiment 3
(1) first the black phosphorus alkene quantum dot of liquid phase ultrasonic preparation is joined 1-butyl-3-methyl imidazolium tetrafluoroborate [the BMIM] [BF containing graphene oxide
4] in dispersion in organic solvent, adopt the method for water bath sonicator mixing to make black phosphorus alkene quantum dot fully be adsorbed onto the surface of graphene oxide.
(2) then metal titanium sheet and graphite rod are placed in mixed dispersion liquid as positive pole and negative pole, the volts DS that additional 20V is constant, make the graphene oxide electrophoretic deposition of negatively charged on metal titanium sheet, form the graphene oxide film of black phosphorus alkene quantum dot modification, depositing time is 10min.
(3) with the clean film of alcohol flushing after finally the metal titanium sheet of this deposit film being taken out, be the graphene film of black phosphorus alkene quantum dot modification at 1200 DEG C of high temperature reductions under argon shield.
Embodiment 4
(1) first the black phosphorus alkene quantum dot of liquid phase ultrasonic preparation is joined in the N-ring ethyl-2-tetramethyleneimine dispersion in organic solvent containing graphene oxide, adopt the method for water bath sonicator mixing to make black phosphorus alkene quantum dot fully be adsorbed onto the surface of graphene oxide.
(2) then silicon carbide plate and graphite rod are placed in mixed dispersion liquid as positive pole and negative pole, the volts DS that additional 30V is constant, make the graphene oxide electrophoretic deposition of negatively charged to silicon carbide plate, form the graphene oxide film of black phosphorus alkene quantum dot modification, depositing time is 5min
(3) with the clean film of alcohol flushing after finally the silicon carbide plate of this deposit film being taken out, be the graphene film of black phosphorus alkene quantum dot modification at 1200 DEG C of high temperature reductions under nitrogen protection.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (2)
1. the electrophoretic deposition preparation method of the graphene film of a black phosphorus alkene quantum dot modification, it is characterized in that: first the black phosphorus alkene quantum dot of liquid phase ultrasonic preparation is joined in the dispersion in organic solvent containing graphene oxide, adopt the method for water bath sonicator mixing to make black phosphorus alkene quantum dot be adsorbed onto the surface of graphene oxide, finally form mixed dispersion liquid; Then be positive pole with conductive substrates, take graphite rod as negative pole, conductive substrates and graphite rod are placed in mixed dispersion liquid, to conductive substrates and the additional constant volts DS of graphite rod, make the graphene oxide electrophoretic deposition of negatively charged on conductive substrates, form the graphene oxide film of black phosphorus alkene quantum dot modification; Finally the conductive substrates of deposited oxide graphene film taken out and clean with alcohol flushing, under argon gas or nitrogen protection, graphene oxide film is reduced to the graphene film that black phosphorus alkene quantum dot is modified by high temperature, and described high temperature is 500 ~ 1200 DEG C.
2. the electrophoretic deposition preparation method of the graphene film of black phosphorus alkene quantum dot modification according to claim 1, is characterized in that: the method comprises the steps:
(1) the black phosphorus alkene quantum dot of liquid phase ultrasonic preparation is joined in the dispersion in organic solvent containing graphene oxide, adopt the method for water bath sonicator mixing to make black phosphorus alkene quantum dot be adsorbed onto the surface of graphene oxide, finally form mixed dispersion liquid; Described organic solvent is the one in dimethyl sulfoxide (DMSO), DMF, N-Methyl pyrrolidone, Virahol, 1-butyl-3-methyl imidazolium tetrafluoroborate, NSC 11801, acetonitrile, 1-butyl-tri-methylimidazolium dicyanamide, N-ring ethyl-2-tetramethyleneimine;
(2) take conductive substrates as positive pole, take graphite rod as negative pole, conductive substrates and graphite rod are placed in mixed dispersion liquid, to conductive substrates and the additional constant volts DS of graphite rod, make the graphene oxide electrophoretic deposition of negatively charged on conductive substrates, form the graphene oxide film of black phosphorus alkene quantum dot modification; Described volts DS is 0.1 ~ 36V; Described conductive substrates is the one in metal titanium, silicon chip, conductive glass, silicon carbide, goldleaf; Depositing time is 1 ~ 30min;
(3) conductive substrates of deposited oxide graphene film to be taken out and clean with alcohol flushing, under argon gas or nitrogen protection, graphene oxide film is reduced to the graphene film that black phosphorus alkene quantum dot is modified by high temperature, and described high temperature is 500 ~ 1200 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106018851A (en) * | 2016-05-23 | 2016-10-12 | 济南大学 | Method for preparing steroid immunosensor based on sheet black phosphorus and application |
| CN106479503A (en) * | 2016-09-29 | 2017-03-08 | Tcl集团股份有限公司 | A kind of quantum dot solid film and preparation method thereof |
| CN106744854A (en) * | 2016-12-29 | 2017-05-31 | 深圳大学 | A kind of Graphene/black phosphorus quantum dot/nitrogen containing plasma liquid composite aerogel and preparation method thereof |
| CN107022784A (en) * | 2016-02-02 | 2017-08-08 | 通用汽车环球科技运作有限责任公司 | Electrophoretic deposition for the electrode of lithium-base battery |
| CN107268017A (en) * | 2017-05-23 | 2017-10-20 | 北京工业大学 | A kind of regulatable black phosphorus method for manufacturing thin film of simple thickness |
| CN107601466A (en) * | 2017-10-12 | 2018-01-19 | 青岛科技大学 | A kind of preparation method and applications of the graphene quantum dot of size uniform |
| CN108772079A (en) * | 2018-04-26 | 2018-11-09 | 昆明理工大学 | A kind of preparation method of nanometer of black phosphorus/graphene composite material |
| CN112909097A (en) * | 2021-02-27 | 2021-06-04 | 成都市水泷头化工科技有限公司 | Graphene/black phosphorus alkene composite thin film transistor and preparation method thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107022784A (en) * | 2016-02-02 | 2017-08-08 | 通用汽车环球科技运作有限责任公司 | Electrophoretic deposition for the electrode of lithium-base battery |
| CN106018851B (en) * | 2016-05-23 | 2018-01-30 | 济南大学 | A kind of preparation method and application of the steroids immunosensor based on sheet black phosphorus |
| CN106018851A (en) * | 2016-05-23 | 2016-10-12 | 济南大学 | Method for preparing steroid immunosensor based on sheet black phosphorus and application |
| CN106479503A (en) * | 2016-09-29 | 2017-03-08 | Tcl集团股份有限公司 | A kind of quantum dot solid film and preparation method thereof |
| CN106744854A (en) * | 2016-12-29 | 2017-05-31 | 深圳大学 | A kind of Graphene/black phosphorus quantum dot/nitrogen containing plasma liquid composite aerogel and preparation method thereof |
| CN106744854B (en) * | 2016-12-29 | 2019-04-26 | 深圳大学 | A kind of graphene/black phosphorus quantum dot/nitrogen containing plasma liquid composite aerogel and preparation method thereof |
| CN107268017A (en) * | 2017-05-23 | 2017-10-20 | 北京工业大学 | A kind of regulatable black phosphorus method for manufacturing thin film of simple thickness |
| CN107268017B (en) * | 2017-05-23 | 2019-03-29 | 北京工业大学 | A kind of regulatable black phosphorus method for manufacturing thin film of simple film thickness |
| CN107601466A (en) * | 2017-10-12 | 2018-01-19 | 青岛科技大学 | A kind of preparation method and applications of the graphene quantum dot of size uniform |
| CN107601466B (en) * | 2017-10-12 | 2018-08-03 | 青岛科技大学 | A kind of preparation method and applications of the graphene quantum dot of size uniform |
| CN108772079A (en) * | 2018-04-26 | 2018-11-09 | 昆明理工大学 | A kind of preparation method of nanometer of black phosphorus/graphene composite material |
| CN108772079B (en) * | 2018-04-26 | 2021-03-02 | 昆明理工大学 | Preparation method of nano black phosphorus/graphene composite material |
| CN112909097A (en) * | 2021-02-27 | 2021-06-04 | 成都市水泷头化工科技有限公司 | Graphene/black phosphorus alkene composite thin film transistor and preparation method thereof |
| CN112909097B (en) * | 2021-02-27 | 2023-04-18 | 贵溪穿越光电科技有限公司 | Graphene/black phosphorus alkene composite thin film transistor and preparation method thereof |
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