CN105129789A - Preparation method of black phosphorus alkene-graphene composite material hollow microsphere - Google Patents
Preparation method of black phosphorus alkene-graphene composite material hollow microsphere Download PDFInfo
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- CN105129789A CN105129789A CN201510624711.0A CN201510624711A CN105129789A CN 105129789 A CN105129789 A CN 105129789A CN 201510624711 A CN201510624711 A CN 201510624711A CN 105129789 A CN105129789 A CN 105129789A
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Abstract
The invention discloses a preparation method of a black phosphorus alkene-graphene composite material hollow microsphere. The preparation method comprises the steps of adding a black phosphorus alkene nanosheet or black phosphorus alkene quantum dot dispersion liquid into oxidized graphene nanosheet dispersion liquid firstly, and mixing the black phosphorus alkene and the oxidized graphene by adopting a mechanical agitation method; spraying the mixed dispersion liquid of the black phosphorus and the oxidized graphene into liquid helium by a spraying method and rapidly freezing the mixed dispersion liquid into microballoons; then putting the obtained black phosphorus alkene and oxidized graphene composite material microballoons into a freezer dryer for freeze-drying, so as to obtain the black phosphorus alkene and oxidized graphene composite material hollow microballoons; reducing the oxidized graphene into graphene at high temperature under the protection of nitrogen or argon, so as to obtain the balck phosphorus alkene and graphene composite material hollow miroballoons at last. The prepared black phosphorus alkene and graphene composite material hollow miroballoons have a potential application prospect in the fields such as lithium ion batteries, supercapacitors, sensors and filtration purification.
Description
Technical field
The present invention relates to the preparation method of a kind of black phosphorus alkene-graphene composite material tiny balloon, prepare tiny balloon on a large scale by freeze forming and hot reducing method, belong to matrix material technology of preparing.
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 lithium ion battery, ultracapacitor, sensor, filtration, purifications 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 preparation method of a kind of black phosphorus alkene-graphene composite material tiny balloon, the method freeze forming and hot reducing method prepare tiny balloon on a large scale, black phosphorus alkene and these two kinds of two-dimensional material of Graphene combine by the method, make matrix material can give play to both respective best physicochemical characteristics, open up more wide application field at electronics and optoelectronic areas.
Technical scheme: for achieving the above object, the technical solution used in the present invention is:
A kind of preparation method of black phosphorus alkene-graphene composite material tiny balloon, first black phosphorus alkene nanometer sheet or black phosphorus alkene quantum dot dispersion liquid are joined in stannic oxide/graphene nano sheet dispersion liquid, adopt churned mechanically method to make black phosphorus alkene and graphene oxide mix formation mixed dispersion liquid; Then by spray method, mixed dispersion liquid being injected to quick freeze in liquid helium is black phosphorus alkene and the freezing microballoon of graphene oxide composite material; Then black phosphorus alkene and the freezing microballoon of graphene oxide composite material are placed in freeze drier lyophilize, obtain black phosphorus alkene and graphene oxide composite material tiny balloon; Last is Graphene by the graphene oxide high temperature reduction in black phosphorus alkene and graphene oxide composite material tiny balloon under nitrogen or argon, finally obtains black phosphorus alkene and graphene composite material tiny balloon.
Aforesaid method specifically comprises the steps:
(1) black phosphorus alkene nanometer sheet or black phosphorus alkene quantum dot dispersion liquid are joined in stannic oxide/graphene nano sheet dispersion liquid, churned mechanically method is adopted to make black phosphorus alkene and graphene oxide mix formation mixed dispersion liquid, black phosphorus alkene nanometer sheet and black phosphorus alkene quantum dot dispersion liquid are referred to as black phosphorus alkene dispersion liquid, black phosphorus alkene dispersion liquid uses identical solvent with stannic oxide/graphene nano sheet dispersion liquid, and both volume ratios are 1:1; Described solvent is ethanol, water, dimethyl sulfoxide (DMSO) (DMSO), N-Methyl pyrrolidone (NMP), Virahol (IPA), DMF (DMF), 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, and the concentration of stannic oxide/graphene nano sheet dispersion liquid is 0.01 ~ 1mg/mL;
(2) by spray method, mixed dispersion liquid being injected to quick freeze in liquid helium is black phosphorus alkene and the freezing microballoon of graphene oxide composite material, and the caliber size of the nozzle bore used in spray method is 0.05 ~ 0.5mm;
(3) black phosphorus alkene and the freezing microballoon of graphene oxide composite material are placed in freeze drier lyophilize 6 ~ 48h, obtain black phosphorus alkene and graphene oxide composite material tiny balloon;
(4) be Graphene by the graphene oxide high temperature reduction in black phosphorus alkene and graphene oxide composite material tiny balloon under nitrogen or argon; finally obtain black phosphorus alkene and graphene composite material tiny balloon, temperature during high temperature reduction is 500 ~ 1200 DEG C.
Beneficial effect: the preparation method of black phosphorus alkene-graphene composite material tiny balloon provided by the invention, utilize churned mechanically method that black phosphorus alkene is compound to surface of graphene oxide, by spray method, black phosphorus alkene and graphene oxide mixed dispersion liquid being injected to quick freeze in liquid helium is microballoon, then adopt the solvent in freeze-drying removing microballoon, obtain black phosphorus alkene and graphene oxide composite material tiny balloon; Last is Graphene by graphene oxide high temperature reduction under nitrogen or argon, finally obtains black phosphorus alkene and graphene composite material tiny balloon.By the microballoon regulating the caliber size of nozzle bore can obtain different size, to meet different application demands.In addition follow-up lyophilize and high temperature heat treatment step, can realize the mass-producing preparation of the Graphene hollow ball that black phosphorus alkene quantum dot is modified.The Synthesis and applications of black phosphorus alkene and graphene composite material tiny balloon is crossed at present without any document and patent report, therefore preparation method of the present invention has filled up this blank, has potential application prospect by fields such as lithium ion battery, ultracapacitor, sensor, filtration, purifications.
Accompanying drawing explanation
Fig. 1 is the optical photograph of the black phosphorus alkene-graphene composite material tiny balloon adopting the inventive method to prepare;
Fig. 2 is the electron scanning micrograph of the microtexture of the black phosphorus alkene-graphene composite material tiny balloon adopting the inventive method to prepare.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
(1) first the alcohol dispersion liquid of 0.01mg/mL black phosphorus alkene nanometer sheet is joined in the alcohol dispersion liquid of 0.5mg/mL stannic oxide/graphene nano sheet, adopt churned mechanically method that black phosphorus alkene and graphene oxide are mixed.Homogeneous solvent should be used when black phosphorus alkene and Graphene mixing, and both volume ratios are 1:1.
(2) it is microballoon that black phosphorus alkene and graphene oxide mixed dispersion liquid are injected to quick freeze in liquid helium by the atomizer being then 0.05mm by nozzle diameter, then obtained black phosphorus alkene and the freezing microballoon of graphene oxide composite material are placed in freeze drier lyophilize 6h, obtain black phosphorus alkene and graphene oxide composite material tiny balloon.
(3) be finally Graphene by graphene oxide high temperature reduction under 500 DEG C and nitrogen protection condition, finally obtain black phosphorus alkene and graphene composite material tiny balloon.
Embodiment 2
(1) first the dimethyl sulfoxide (DMSO) dispersion liquid of 1mg/mL black phosphorus alkene quantum dot is joined in the dimethyl sulfoxide (DMSO) dispersion liquid of 0.5mg/mL stannic oxide/graphene nano sheet, adopt churned mechanically method that black phosphorus alkene and graphene oxide are mixed.Homogeneous solvent should be used when black phosphorus alkene and Graphene mixing, and both volume ratios are 1:1.
(2) it is microballoon that black phosphorus alkene and graphene oxide mixed dispersion liquid are injected to quick freeze in liquid helium by the atomizer being then 0.2mm by nozzle diameter, then obtained black phosphorus alkene and the freezing microballoon of graphene oxide composite material are placed in freeze drier lyophilize 24h, obtain black phosphorus alkene and graphene oxide composite material tiny balloon.
(3) be finally Graphene by graphene oxide high temperature reduction under 800 DEG C and argon shield condition, finally obtain black phosphorus alkene and graphene composite material tiny balloon.
The optical photograph of black phosphorus alkene-graphene composite material tiny balloon prepared by Fig. 1 the present embodiment.As we can see from the figure, prepared microballoon is the hollow ball of opening, is of a size of about 0.5 ~ 3mm.Fig. 2 is the electron scanning micrograph of the microtexture of black phosphorus alkene-graphene composite material tiny balloon prepared by the present embodiment.As we can see from the figure, microballoon is made up of the nanometer sheet skeleton of three-dimensional structure, presents the morphology of porous.
Embodiment 3
(1) first the N-Methyl pyrrolidone dispersion liquid of 2mg/mL black phosphorus alkene quantum dot is joined in the N-Methyl pyrrolidone dispersion liquid of 1mg/mL stannic oxide/graphene nano sheet, adopt churned mechanically method that black phosphorus alkene and graphene oxide are mixed.Homogeneous solvent should be used when black phosphorus alkene and Graphene mixing, and both volume ratios are 1:1.
(2) it is microballoon that black phosphorus alkene and graphene oxide mixed dispersion liquid are injected to quick freeze in liquid helium by the atomizer being then 0.3mm by nozzle diameter, then obtained black phosphorus alkene and the freezing microballoon of graphene oxide composite material are placed in freeze drier lyophilize 36h, obtain black phosphorus alkene and graphene oxide composite material tiny balloon.
(3) be finally Graphene by graphene oxide high temperature reduction under 1000 DEG C and argon shield condition, finally obtain black phosphorus alkene and graphene composite material tiny balloon.
Embodiment 4
(1) first the N-ring ethyl-2-tetramethyleneimine dispersion liquid of 5mg/mL black phosphorus alkene quantum dot is joined in the N-ring ethyl-2-tetramethyleneimine dispersion liquid of 1mg/mL stannic oxide/graphene nano sheet, adopt churned mechanically method that black phosphorus alkene and graphene oxide are mixed.Homogeneous solvent should be used when black phosphorus alkene and Graphene mixing, and both volume ratios are 1:1.
(2) it is microballoon that black phosphorus alkene and graphene oxide mixed dispersion liquid are injected to quick freeze in liquid helium by the atomizer being then 0.5mm by nozzle diameter, then obtained black phosphorus alkene and the freezing microballoon of graphene oxide composite material are placed in freeze drier lyophilize 48h, obtain black phosphorus alkene and graphene oxide composite material tiny balloon.
(3) be finally Graphene by graphene oxide high temperature reduction under 1200 DEG C and argon shield condition, finally obtain black phosphorus alkene and graphene composite material tiny balloon.
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 preparation method of black phosphorus alkene-graphene composite material tiny balloon, it is characterized in that: first black phosphorus alkene nanometer sheet or black phosphorus alkene quantum dot dispersion liquid are joined in stannic oxide/graphene nano sheet dispersion liquid, adopt churned mechanically method to make black phosphorus alkene and graphene oxide mix formation mixed dispersion liquid; Then by spray method, mixed dispersion liquid being injected to quick freeze in liquid helium is black phosphorus alkene and the freezing microballoon of graphene oxide composite material; Then black phosphorus alkene and the freezing microballoon of graphene oxide composite material are placed in freeze drier lyophilize, obtain black phosphorus alkene and graphene oxide composite material tiny balloon; Last is Graphene by the graphene oxide high temperature reduction in black phosphorus alkene and graphene oxide composite material tiny balloon under nitrogen or argon, finally obtains black phosphorus alkene and graphene composite material tiny balloon.
2. the preparation method of black phosphorus alkene-graphene composite material tiny balloon according to claim 1, is characterized in that: the method specifically comprises the steps:
(1) black phosphorus alkene nanometer sheet or black phosphorus alkene quantum dot dispersion liquid are joined in stannic oxide/graphene nano sheet dispersion liquid, churned mechanically method is adopted to make black phosphorus alkene and graphene oxide mix formation mixed dispersion liquid, black phosphorus alkene nanometer sheet and black phosphorus alkene quantum dot dispersion liquid are referred to as black phosphorus alkene dispersion liquid, black phosphorus alkene dispersion liquid uses identical solvent with stannic oxide/graphene nano sheet dispersion liquid, and both volume ratios are 1:1; Described solvent is ethanol, water, dimethyl sulfoxide (DMSO), N-Methyl pyrrolidone, Virahol, N, one in dinethylformamide, 1-butyl-3-methyl imidazolium tetrafluoroborate, NSC 11801, acetonitrile, 1-butyl-tri-methylimidazolium dicyanamide, N-ring ethyl-2-tetramethyleneimine, and the concentration of stannic oxide/graphene nano sheet dispersion liquid is 0.01 ~ 1mg/mL;
(2) by spray method, mixed dispersion liquid being injected to quick freeze in liquid helium is black phosphorus alkene and the freezing microballoon of graphene oxide composite material, and the caliber size of the nozzle bore used in spray method is 0.05 ~ 0.5mm;
(3) black phosphorus alkene and the freezing microballoon of graphene oxide composite material are placed in freeze drier lyophilize 6 ~ 48h, obtain black phosphorus alkene and graphene oxide composite material tiny balloon;
(4) be Graphene by the graphene oxide high temperature reduction in black phosphorus alkene and graphene oxide composite material tiny balloon under nitrogen or argon; finally obtain black phosphorus alkene and graphene composite material tiny balloon, temperature during high temperature reduction is 500 ~ 1200 DEG C.
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| CN105944114A (en) * | 2016-04-19 | 2016-09-21 | 首都医科大学 | Black phosphorus-graphene composite nanometer contrast agent and preparation thereof, and application of contrast agent to acupuncture research |
| CN106098399A (en) * | 2016-05-26 | 2016-11-09 | 北京石油化工学院 | Combination electrode, ultracapacitor and preparation method thereof |
| CN106241778A (en) * | 2016-07-15 | 2016-12-21 | 浙江大学 | A kind of high-specific surface area many folds hollow graphite alkene microsphere and preparation method thereof |
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