CN105129789B - A kind of preparation method of black phosphorus alkene graphene composite material tiny balloon - Google Patents
A kind of preparation method of black phosphorus alkene graphene composite material tiny balloon Download PDFInfo
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- CN105129789B CN105129789B CN201510624711.0A CN201510624711A CN105129789B CN 105129789 B CN105129789 B CN 105129789B CN 201510624711 A CN201510624711 A CN 201510624711A CN 105129789 B CN105129789 B CN 105129789B
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 106
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 150000001336 alkenes Chemical class 0.000 title abstract description 8
- -1 black phosphorus alkene Chemical class 0.000 claims abstract description 87
- 239000007788 liquid Substances 0.000 claims abstract description 52
- 239000006185 dispersion Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000007710 freezing Methods 0.000 claims abstract description 11
- 230000008014 freezing Effects 0.000 claims abstract description 11
- 239000002096 quantum dot Substances 0.000 claims abstract description 11
- 239000001307 helium Substances 0.000 claims abstract description 10
- 229910052734 helium Inorganic materials 0.000 claims abstract description 10
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 8
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims 1
- 239000011806 microball Substances 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 3
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 description 1
- AWSCOTJIASXILV-UHFFFAOYSA-O 3-butyl-2,4,5-trimethyl-1H-imidazol-3-ium Chemical compound CCCC[n+]1c(C)[nH]c(C)c1C AWSCOTJIASXILV-UHFFFAOYSA-O 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of black phosphorus alkene graphene composite material tiny balloon, black phosphorus alkene nanometer sheet or black phosphorus alkene quantum dot dispersion liquid are added in stannic oxide/graphene nano piece dispersion liquid first, using churned mechanically method both black phosphorus alkene and graphene oxide are mixed；Then it is microballoon black phosphorus alkene and graphene oxide mixed dispersion liquid to be injected into quick freeze in liquid helium by spray-on process, then resulting black phosphorus alkene and graphene oxide composite material freezing microballoon are placed in freeze drier and is freeze-dried, obtain black phosphorus alkene and graphene oxide composite material tiny balloon；Last is under nitrogen or argon graphene by graphene oxide high temperature reduction, finally gives black phosphorus alkene and graphene composite material tiny balloon.Black phosphorus alkene and graphene composite material tiny balloon prepared by the present invention has potential application foreground in fields such as lithium ion battery, ultracapacitor, sensor, filtration, purifications.
Description
Technical field
The present invention relates to a kind of preparation method of black phosphorus alkene-graphene composite material tiny balloon, by freeze forming with
Thermal reduction prepares tiny balloon on a large scale, belongs to composite technology of preparing.
Background technology
Two-dimension nano materials such as graphene, transient metal sulfide etc., are existed with its excellent physics and architectural characteristic
Electronics, sensing and photoelectric device etc. are multi-field to show outstanding application potential.Wherein, graphene is used as most representational two
Dimension material has been widely studied.It has the carrier mobility of superelevation, but shortage band gap seriously hinders graphene and existed
Application in logic semiconductor devices such as field-effect transistor.And as transient metal sulfide semiconductor family representative into
Member, molybdenum disulfide (MoS2) there is obvious band gap, and show in n-type transistor excellent switch ratio characteristic (>108)。
However, MoS2There is the reduction that may result in electron mobility in middle fault of construction, so as to influence its electric property.Therefore,
Explore more new function two-dimensional semiconductor materials still significant.In recent years, with individual layer or few layer black phosphorus atom
The black phosphorus alkene of Rotating fields, with its higher carrier mobility (200~1000cm2V-1s-1), adjustable direct band gap, compared with
Big switch ratio characteristic (104~105) and anisotropy etc., it is increasingly becoming and most potential is applied to high-performance electronic and photoelectricity
The two-dimensional semiconductor material of sub- device.Therefore, need a kind of synthesis preparation method, can be by two kinds of two dimensions of black phosphorus alkene and graphene
Material combines, and forms the composite with both excellent physical characteristics, will widen black phosphorus alkene and graphene is multiple
Potential application of the condensation material in numerous areas such as lithium ion battery, ultracapacitor, sensor, filtration, purifications.
The content of the invention
Goal of the invention：In order to overcome the deficiencies in the prior art, the present invention provides a kind of black phosphorus alkene-graphene and is combined
The preparation method of material tiny balloon, this method freeze forming comes to prepare tiny balloon on a large scale with thermal reduction, and this method will
Black phosphorus alkene and graphene both two-dimensional materials combine so that composite can give play to both respective optimal materializations
Characteristic, field is more widely applied in electronics and optoelectronic areas developing.
Technical scheme：To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of black phosphorus alkene-graphene composite material tiny balloon, first by black phosphorus alkene nanometer sheet or black
Phosphorus alkene quantum dot dispersion liquid is added in stannic oxide/graphene nano piece dispersion liquid, using churned mechanically method cause black phosphorus alkene and
Both graphene oxides are well mixed to form mixed dispersion liquid；Then mixed dispersion liquid is injected to by spray-on process fast in liquid helium
Quickly cooling is frozen as black phosphorus alkene and graphene oxide composite material freezing microballoon；Then it is black phosphorus alkene and graphene oxide composite material is cold
Freeze microballoon and be placed in freeze-drying in freeze drier, obtain black phosphorus alkene and graphene oxide composite material tiny balloon；Finally exist
It is by the graphene oxide high temperature reduction in black phosphorus alkene and graphene oxide composite material tiny balloon under nitrogen or argon gas protection
Graphene, finally gives black phosphorus alkene and graphene composite material tiny balloon.
The above method specifically includes following steps：
(1) black phosphorus alkene nanometer sheet or black phosphorus alkene quantum dot dispersion liquid are added to stannic oxide/graphene nano piece dispersion liquid
In, cause both black phosphorus alkene and graphene oxide are well mixed to form mixed dispersion liquid using churned mechanically method, by 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 and stannic oxide/graphene nano piece
Dispersion liquid uses identical solvent, and both volume ratios are 1:1；The solvent be ethanol, water, dimethyl sulfoxide (DMSO) (DMSO),
1-METHYLPYRROLIDONE (NMP), isopropanol (IPA), N,N-dimethylformamide (DMF), 1- butyl -3- methylimidazole tetrafluoro boron
Hydrochlorate [BMIM] [BF4], ethylene carbonate (EC), acetonitrile, 1- butyl-tri-methylimidazolium cdicynanmide [BMIM] [N (CN2)], N- rings
One kind in ethyl -2- pyrrolidines, and the concentration of stannic oxide/graphene nano piece dispersion liquid is 0.01~1mg/mL；
(2) it is that black phosphorus alkene and graphene oxide are combined mixed dispersion liquid to be injected into quick freeze in liquid helium by spray-on process
The caliber size that material freezes the nozzle bore used in microballoon, spray-on process is 0.05~0.5mm；
(3) by black phosphorus alkene and graphene oxide composite material freezing microballoon be placed in freeze drier freeze-drying 6~
48h, obtains black phosphorus alkene and graphene oxide composite material tiny balloon；
(4) under nitrogen or argon by the graphite oxide in black phosphorus alkene and graphene oxide composite material tiny balloon
Alkene high temperature reduction is graphene, finally gives black phosphorus alkene and graphene composite material tiny balloon, temperature during high temperature reduction is
500~1200 DEG C.
Beneficial effect：The preparation method for black phosphorus alkene-graphene composite material tiny balloon that the present invention is provided, utilizes machinery
Black phosphorus alkene is compound to surface of graphene oxide by the method for stirring, and black phosphorus alkene and graphene oxide are mixed into scattered by spray-on process
It is microballoon that liquid, which is injected in liquid helium quick freeze, then removes the solvent in microballoon using freeze-drying, obtain black phosphorus alkene and
Graphene oxide composite material tiny balloon；Last is under nitrogen or argon graphite by graphene oxide high temperature reduction
Alkene, finally gives black phosphorus alkene and graphene composite material tiny balloon.Difference can obtain by the caliber size for adjusting nozzle bore
The microballoon of size, to meet different application demands.It is subject to follow-up freeze-drying and high temperature heat treatment step, black phosphorus can be achieved
The prepare with scale of the graphene hollow ball of alkene quantum dot modification.Black phosphorus alkene and stone are crossed currently without any document and patent report
The preparation and application of black alkene composite material hollow microballoon, thus the present invention preparation method filled up this blank, will lithium from
The fields such as sub- battery, ultracapacitor, sensor, filtration, purification have potential application prospect.
Brief description of the drawings
Fig. 1 is the optical photograph of the black phosphorus alkene-graphene composite material tiny balloon prepared using the inventive method；
Fig. 2 is sweeping for the microstructure of the black phosphorus alkene-graphene composite material tiny balloon prepared using the inventive method
Retouch electron micrograph.
Embodiment
The present invention is further described with reference to embodiment.
Embodiment 1
(1) alcohol dispersion liquid of 0.01mg/mL black phosphorus alkene nanometer sheets is added into 0.5mg/mL graphene oxides first to receive
In the alcohol dispersion liquid of rice piece, using churned mechanically method both black phosphorus alkene and graphene oxide are mixed.Black phosphorus alkene and
Graphene should use homogeneous solvent when mixing, and both volume ratios are 1:1.
(2) and then by nozzle diameter black phosphorus alkene and graphene oxide mixed dispersion liquid are sprayed into for 0.05mm sprayer
Into liquid helium, quick freeze is microballoon, is then placed in resulting black phosphorus alkene and graphene oxide composite material freezing microballoon cold
6h is freeze-dried in lyophilizer, black phosphorus alkene and graphene oxide composite material tiny balloon is obtained.
(3) last is graphene by graphene oxide high temperature reduction under 500 DEG C and nitrogen protective condition, is finally given black
Phosphorus alkene and graphene composite material tiny balloon.
Embodiment 2
(1) the dimethyl sulfoxide (DMSO) dispersion liquid of 1mg/mL black phosphorus alkene quantum dots is added to 0.5mg/mL graphene oxides first
In the dimethyl sulfoxide (DMSO) dispersion liquid of nanometer sheet, using churned mechanically method both 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) and then by nozzle diameter black phosphorus alkene and graphene oxide mixed dispersion liquid are sprayed into for 0.2mm sprayer
Into liquid helium, quick freeze is microballoon, is then placed in resulting black phosphorus alkene and graphene oxide composite material freezing microballoon cold
24h is freeze-dried in lyophilizer, black phosphorus alkene and graphene oxide composite material tiny balloon is obtained.
(3) last is graphene by graphene oxide high temperature reduction under 800 DEG C and argon gas protective condition, is finally given black
Phosphorus alkene and graphene composite material tiny balloon.
The optical photograph of Fig. 1 black phosphorus alkene-graphene composite material tiny balloons manufactured in the present embodiment.Can from figure
Arrive, prepared microballoon is the hollow ball of opening, size is 0.5~3mm or so.Fig. 2 be black phosphorus alkene manufactured in the present embodiment-
The electron scanning micrograph of the microstructure of graphene composite material tiny balloon.From the figure, it can be seen that microballoon is by three
The nanometer sheet skeleton for tieing up structure is constituted, and porous morphology is presented.
Embodiment 3
(1) the 1-METHYLPYRROLIDONE dispersion liquid of 2mg/mL black phosphorus alkene quantum dots is added to 1mg/mL graphite oxides first
In the 1-METHYLPYRROLIDONE dispersion liquid of alkene nanometer sheet, both black phosphorus alkene and graphene oxide are caused using churned mechanically method
Mixing.Homogeneous solvent should be used when black phosphorus alkene and graphene mixing, and both volume ratios are 1:1.
(2) and then by nozzle diameter black phosphorus alkene and graphene oxide mixed dispersion liquid are sprayed into for 0.3mm sprayer
Into liquid helium, quick freeze is microballoon, is then placed in resulting black phosphorus alkene and graphene oxide composite material freezing microballoon cold
36h is freeze-dried in lyophilizer, black phosphorus alkene and graphene oxide composite material tiny balloon is obtained.
(3) last is graphene by graphene oxide high temperature reduction under 1000 DEG C and argon gas protective condition, is finally given
Black phosphorus alkene and graphene composite material tiny balloon.
Embodiment 4
(1) the N- ring ethyl -2- pyrrolidines dispersion liquids of 5mg/mL black phosphorus alkene quantum dots are added to 1mg/mL oxidations first
In the N- ring ethyl -2- pyrrolidines dispersion liquids of graphene nanometer sheet, black phosphorus alkene and oxidation stone are caused using churned mechanically method
Both black alkene is mixed.Homogeneous solvent should be used when black phosphorus alkene and graphene mixing, and both volume ratios are 1:1.
(2) and then by nozzle diameter black phosphorus alkene and graphene oxide mixed dispersion liquid are sprayed into for 0.5mm sprayer
Into liquid helium, quick freeze is microballoon, is then placed in resulting black phosphorus alkene and graphene oxide composite material freezing microballoon cold
48h is freeze-dried in lyophilizer, black phosphorus alkene and graphene oxide composite material tiny balloon is obtained.
(3) last is graphene by graphene oxide high temperature reduction under 1200 DEG C and argon gas protective condition, is finally given
Black phosphorus alkene and graphene composite material tiny balloon.
Described above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (1)
1. a kind of preparation method of black phosphorus alkene-graphene composite material tiny balloon, it is characterised in that：First by black phosphorus alkene nanometer
Piece or black phosphorus alkene quantum dot dispersion liquid are added in stannic oxide/graphene nano piece dispersion liquid, are caused using churned mechanically method
Both black phosphorus alkene and graphene oxide are well mixed to form mixed dispersion liquid；Then mixed dispersion liquid is injected to by spray-on process
Quick freeze is black phosphorus alkene and graphene oxide composite material freezing microballoon in liquid helium；Then black phosphorus alkene and graphene oxide are answered
Condensation material freezing microballoon, which is placed in freeze drier, to be freeze-dried, and obtains black phosphorus alkene and graphene oxide composite material is hollow micro-
Ball；It is finally under nitrogen or argon that the graphene oxide in black phosphorus alkene and graphene oxide composite material tiny balloon is high
Temperature is reduced to graphene, finally gives black phosphorus alkene and graphene composite material tiny balloon；This method specifically includes following steps：
(1) black phosphorus alkene nanometer sheet or black phosphorus alkene quantum dot dispersion liquid are added in stannic oxide/graphene nano piece dispersion liquid, adopted
Cause both black phosphorus alkene and graphene oxide are well mixed to form mixed dispersion liquid with churned mechanically method, by black phosphorus alkene nanometer
Piece and black phosphorus alkene quantum dot dispersion liquid are referred to as black phosphorus alkene dispersion liquid, black phosphorus alkene dispersion liquid and stannic oxide/graphene nano piece dispersion liquid
Using identical solvent, and both volume ratios are 1:1；The solvent is ethanol, water, dimethyl sulfoxide (DMSO), N- crassitudes
Ketone, isopropanol, N,N-dimethylformamide, 1- butyl -3- methyl imidazolium tetrafluoroborates, ethylene carbonate, acetonitrile, 1- fourths
One kind in base-tri-methylimidazolium cdicynanmide, N- ring ethyl -2- pyrrolidines, and the concentration of stannic oxide/graphene nano piece dispersion liquid
For 0.01~1mg/mL；
(2) it is black phosphorus alkene and graphene oxide composite material mixed dispersion liquid to be injected into quick freeze in liquid helium by spray-on process
The caliber size for freezing the nozzle bore used in microballoon, spray-on process is 0.05~0.5mm；
(3) black phosphorus alkene and graphene oxide composite material freezing microballoon are placed in 6~48h of freeze-drying in freeze drier, obtained
To black phosphorus alkene and graphene oxide composite material tiny balloon；
(4) it is under nitrogen or argon that the graphene oxide in black phosphorus alkene and graphene oxide composite material tiny balloon is high
Temperature is reduced to graphene, finally gives black phosphorus alkene and graphene composite material tiny balloon, temperature during high temperature reduction be 500~
1200℃。
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| CN103432992A (en) * | 2013-08-23 | 2013-12-11 | 中国科学院东北地理与农业生态研究所 | Method for preparing graphene coated nanometer material composite |
| CN103579616A (en) * | 2013-10-31 | 2014-02-12 | 浙江工业大学 | Graphene coated lead powder composite material and application thereof |
| CN103877971A (en) * | 2014-03-07 | 2014-06-25 | 中国科学院东北地理与农业生态研究所 | Efficient visible-light-induced photocatalyst and preparation method thereof |
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