CN109081316A - A kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process - Google Patents
A kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process Download PDFInfo
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- CN109081316A CN109081316A CN201710444138.4A CN201710444138A CN109081316A CN 109081316 A CN109081316 A CN 109081316A CN 201710444138 A CN201710444138 A CN 201710444138A CN 109081316 A CN109081316 A CN 109081316A
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- QIHHYQWNYKOHEV-UHFFFAOYSA-N 4-tert-butyl-3-nitrobenzoic acid Chemical compound CC(C)(C)C1=CC=C(C(O)=O)C=C1[N+]([O-])=O QIHHYQWNYKOHEV-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 39
- 239000002904 solvent Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000010410 layer Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000006228 supernatant Substances 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 238000002604 ultrasonography Methods 0.000 claims abstract description 14
- 239000002356 single layer Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000010792 warming Methods 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000009830 intercalation Methods 0.000 claims description 9
- 230000002687 intercalation Effects 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 7
- 239000011669 selenium Substances 0.000 claims description 7
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 229910052711 selenium Inorganic materials 0.000 claims description 6
- 239000004065 semiconductor Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000000527 sonication Methods 0.000 claims description 3
- 241000446313 Lamella Species 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims 1
- 238000004528 spin coating Methods 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000012512 characterization method Methods 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 2
- 238000000703 high-speed centrifugation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910005543 GaSe Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/24—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only semiconductor materials not provided for in groups H01L29/16, H01L29/18, H01L29/20, H01L29/22
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
Abstract
The invention discloses a kind of preparations of Germanium selenide two-dimensional material based on solvent heat graft process: including the following steps: that Germanium selenide powder is put into reaction kettle by (1), solvent is added, be warming up to 100-200 DEG C, keep the temperature 8-48h；(2) the Germanium selenide dispersion liquid after step (1) solvent heat is put into cell disruptor, is ultrasonically treated；(3) centrifugal treating is carried out to the Germanium selenide dispersion liquid after ultrasound, obtains the supernatant liquor of grey black, single layer or few layer Germanium selenide are dispersed in the supernatant liquor of the grey black.The beneficial effects of the present invention are: preparation method is simple, it is easy to operate.
Description
Technical field
The present invention relates to two-dimensional material preparation technical fields, more particularly to a kind of Germanium selenide based on solvent heat graft process
The preparation method of two-dimensional material.
Background technique
Two-dimensional layer semiconductor material has the excellent property such as specific surface area of adjustable band gap, superelevation, possesses solely
Optics, the electrical properties of spy, cause extensive research boom in scientific circles.Since graphene in 2004 is successfully removed, more
Come more two-dimensional semiconductor materials, such as Transition-metal dichalcogenide (MoS2、MoSe2、WS2) and III-IVA semiconductor
Material (GaS, GaSe, In2Se3, InSe), in photodetector, field effect transistor, solar battery and flexible device etc.
Field shows the application prospect of great potential.Document report, Germanium selenide are a kind of layered crystals similar with black phosphorus structure, are
A kind of p-type semiconductor material of narrow band gap (1.08ev) has air, humidity stability, the pole in terms of the following opto-electronic device
It is with potential applications.(Mukherjee B,Cai Y,Tan H R,et al.NIR Schottkyphotodetectors based
on individual single-crystalline GeSenanosheet.[J].Acs Applied Materials&
Interfaces, 2013,5 (19): 9594.) currently, the preparation of Germanium selenide two-dimensional material include micromechanics stripping method, ultrasound it is auxiliary
Help stripping method.But peeling effect is undesirable, cannot combine the requirement of lateral dimension and thickness.
Summary of the invention
In view of the technical drawbacks of the prior art, it is an object of the present invention to provide one kind to be based on solvent heat graft process
Germanium selenide two-dimensional material preparation method.
The technical solution adopted to achieve the purpose of the present invention is:
A kind of preparation of the Germanium selenide two-dimensional material based on solvent heat graft process: include the following steps:
(1) Germanium selenide powder is put into reaction kettle, organic solvent is added, be warming up to 100-200 DEG C, keep the temperature 8-48h, it is described
Organic solvent chooses ethyl alcohol, methanol, dimethylformamide or chloroform；
(2) the Germanium selenide dispersion liquid after step (1) solvent heat is put into cell disruptor, is ultrasonically treated, in which: is super
The sonication time is 2-20h, ultrasonic power 50-300W；
(3) centrifugal treating is carried out to the Germanium selenide dispersion liquid after ultrasound, obtains the supernatant liquor of grey black, the grey black
Supernatant liquor in be dispersed with single layer or few layer Germanium selenide, wherein layer Germanium selenide is layer 2-3 less, wherein the speed being centrifugated is
1000r/min-8000r/min, centrifugation time 5-60min.
Preferably, the Germanium selenide powder in the step (1) is prepared by following steps: weighing the selenium and germanium of equimolar ratio
Powder is placed in Vacuum Package in quartz glass tube, is heated slowly to 600 DEG C~1000 DEG C, keeps the temperature 12-72h, naturally cools to room
Temperature obtains Germanium selenide dusty material.
Preferably, organic solvent chooses ethyl alcohol or methanol in the step (1).
Preferably, sonication treatment time is 15-20h, ultrasonic power 100-300W in the step (2).
Preferably, the speed being centrifugated in the step (3) is 5000r/min-8000r/min, centrifugation time 30-
60min。
Preferably, by adjusting solvent type, temperature, time during solvent heat intercalation, uniform Germanium selenide is prepared
Two-dimensional nano piece.
Another aspect of the present invention further includes that the supernatant for being dispersed with single layer or lacking layer Germanium selenide is preparing semiconductor
Application in material.
Preferably, the supernatant for being dispersed with single layer or few layer Germanium selenide is spun on silicon wafer, it is suitable to find under light microscopic
Sheet layer material obtain FET device in lamella both ends electrode evaporation.
Compared with prior art, the beneficial effects of the present invention are:
Germanium selenide body material is distributed to progress solvent heat intercalation in a variety of organic reagents for the first time by the present invention, then uses cell powder
Broken machine is ultrasonically treated and is carried out high speed centrifugation, finally obtains two-dimensional slice Germanium selenide.Ethyl alcohol, methanol, two are selected in experiment
The organic reagents such as methylformamide, chloroform are as solvent, and preparation method is simple, easy to operate, insert by adjusting solvent heat
Solvent type, temperature, time etc., factors prepared uniform Germanium selenide two-dimensional nano piece during layer.
Detailed description of the invention
The X-ray diffraction phenogram of the Germanium selenide body material of Fig. 1 sintering；
The scanning electron microscope phenogram of the Germanium selenide body material of Fig. 2 sintering；
Germanium selenide surface sweeping Electronic Speculum phenogram after Fig. 3 solvent heat intercalation processing；
The transmission electron microscope phenogram of the Germanium selenide nanometer sheet obtained after the removing of Fig. 4 ultrasound；
Specific embodiment
The present invention is described in further detail below in conjunction with the drawings and specific embodiments.It should be appreciated that described herein
Specific embodiment be only used to explain the present invention, be not intended to limit the present invention.
Embodiment 1
(1) selenium and 72.6mg germanium powder for weighing 79mg are placed in Vacuum Package in quartz glass tube, are heated slowly to 600
DEG C, 12h is kept the temperature, room temperature is naturally cooled to, obtains Germanium selenide body material；
(2) Germanium selenide body material obtained in step (1) is put into reaction kettle, ethyl alcohol is added, is put into Muffle furnace, is warming up to
150 DEG C, heat preservation is for 24 hours；
(3) the Germanium selenide dispersion liquid after solvent heat in step (2) is put into cell disruptor, is ultrasonically treated, ultrasound
Power be 50W, ultrasonic time 20h；
(4) centrifugal treating, centrifugation rate 8000r/min are carried out to the Germanium selenide dispersion liquid after ultrasound, centrifugation time is
5min obtains the supernatant liquor of grey black；
X-ray diffraction, scanning electron microscope characterization are carried out to gray solid obtained in step (1), by Fig. 1 and standard Germanium selenide
Card compares, it was demonstrated that sintering has obtained Germanium selenide, scans electricity according to solvent heat intercalation Germanium selenide obtained in step (2)
The characterization of mirror, it can be seen that the spacing of piece interlayer becomes larger, and has a small amount of monolayer material to be formed, on obtained in step (4)
The characterization of clear liquid progress transmission electron microscope, it was demonstrated that obtained the Germanium selenide of two-dimensional layer.
Embodiment 2
(1) selenium and 72.6mg germanium powder for weighing 79mg are placed in Vacuum Package in quartz glass tube, are heated slowly to 900
DEG C, 48h is kept the temperature, room temperature is naturally cooled to, obtains Germanium selenide body material；
(2) Germanium selenide body material obtained in step (1) is put into reaction kettle, methanol is added, is put into Muffle furnace, is warming up to
100 DEG C, keep the temperature 48h；
(3) the Germanium selenide dispersion liquid after solvent heat in step (2) is put into cell disruptor, is ultrasonically treated, ultrasound
Power be 150W, ultrasonic time 10h；
(4) centrifugal treating, centrifugation rate 5000r/min are carried out to the Germanium selenide dispersion liquid after ultrasound, centrifugation time is
20min obtains the supernatant liquor of grey black；
(5) X-ray diffraction, scanning electron microscope characterization are carried out to gray solid obtained in step (1), is obtained in step (2)
The characterization of the solvent heat intercalation Germanium selenide scanning electron microscope arrived carries out the characterization of transmission electron microscope to supernatant obtained in step (3),
Obtain result same as Example 1.
Embodiment 3
(1) selenium and 72.6mg germanium powder for weighing 79mg are placed in Vacuum Package in quartz glass tube, are heated slowly to 750
DEG C, 72h is kept the temperature, room temperature is naturally cooled to, obtains Germanium selenide body material；
(2) Germanium selenide body material obtained in step (1) is put into reaction kettle, dimethylformamide is added, is put into Muffle
Furnace is warming up to 200 DEG C, keeps the temperature 8h, is scanned Electronic Speculum characterization；
(3) the Germanium selenide dispersion liquid after solvent heat in step (2) is put into cell disruptor, is ultrasonically treated, ultrasound
Power be 300W, ultrasonic time 2h；
(4) centrifugal treating, centrifugation rate 1000r/min are carried out to the Germanium selenide dispersion liquid after ultrasound, centrifugation time is
60min obtains the supernatant liquor of grey black；
(5) X-ray diffraction, scanning electron microscope characterization are carried out to gray solid obtained in step (1), is obtained in step (2)
The characterization of the solvent heat intercalation Germanium selenide scanning electron microscope arrived carries out the characterization of transmission electron microscope to supernatant obtained in step (3),
Obtain result same as Example 1.
Embodiment 4
(1) selenium and 72.6mg germanium powder for weighing 79mg are placed in Vacuum Package in quartz glass tube, are heated slowly to 800
DEG C, 18h is kept the temperature, room temperature is naturally cooled to, obtains Germanium selenide body material；
(2) Germanium selenide body material obtained in step (1) is put into reaction kettle, chloroform is added, is put into Muffle furnace, is warming up to
120 DEG C, keep the temperature 10h；
(3) the Germanium selenide dispersion liquid after solvent heat in step (2) is put into cell disruptor, is ultrasonically treated, ultrasound
Power be 100W, ultrasonic time 10h；
(4) centrifugal treating, centrifugation rate 4000r/min are carried out to the Germanium selenide dispersion liquid after ultrasound, centrifugation time is
20min obtains the supernatant liquor of grey black；
(5) X-ray diffraction, scanning electron microscope characterization are carried out to gray solid obtained in step (1), is obtained in step (2)
The characterization of the solvent heat intercalation Germanium selenide scanning electron microscope arrived carries out the characterization of transmission electron microscope to supernatant obtained in step (3),
Obtain result same as Example 1.
The present invention discloses and proposes for Germanium selenide body material to be distributed to progress solvent heat intercalation processing in a variety of organic reagents,
It is ultrasonically treated with cell disruptor, then carries out high speed centrifugation, finally obtain two-dimensional slice Germanium selenide, those skilled in the art
It can be by using for reference present disclosure, the links such as appropriate feed change and process route are realized, although method of the invention and preparation skill
Art is described by preferred embodiment, and related technical personnel can obviously not depart from the content of present invention, spirit and model
Enclose it is interior methods and techniques described herein route is modified or is reconfigured, to realize final technology of preparing.Especially need
It is noted that all similar replacements and change are apparent to those skilled in the art, they are regarded
To be included in spirit of that invention, range and content.
Claims (8)
1. a kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process, which comprises the steps of:
(1) Germanium selenide powder is put into reaction kettle, organic solvent is added, be warming up to 100-200oC, keep the temperature 8-48h, it is described organic
Solvent chooses ethyl alcohol, methanol, dimethylformamide or chloroform；
(2) the Germanium selenide dispersion liquid after step (1) solvent heat is put into cell disruptor, is ultrasonically treated, in which: at ultrasound
The reason time is 2-20h, ultrasonic power 50-300W；
(3) centrifugal treating is carried out to the Germanium selenide dispersion liquid after ultrasound, obtains the supernatant liquor of grey black, the grey black it is upper
Single layer or few layer Germanium selenide are dispersed in layer clear liquid, wherein layer Germanium selenide is layer 2-3 less, wherein the speed being centrifugated is
1000r/min-8000r/min, centrifugation time 5-60min.
2. a kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process as described in claim 1, feature
It is, the Germanium selenide powder in the step (1) is prepared by following steps: the selenium and germanium powder for weighing equimolar ratio are placed in stone
Vacuum Package in English glass tube is heated slowly to 600 DEG C~1000 DEG C, keeps the temperature 12-72h, naturally cools to room temperature, obtain selenizing
Germanium dusty material.
3. a kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process as described in claim 1, feature
It is, organic solvent chooses ethyl alcohol or methanol in the step (1).
4. a kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process as described in claim 1, feature
It is, sonication treatment time is 15-20h, ultrasonic power 100-300W in the step (2).
5. a kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process as described in claim 1, feature
It is, the speed being centrifugated in the step (3) is 5000r/min-8000r/min, centrifugation time 30-60min.
6. a kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process as described in claim 1, feature
It is, by adjusting solvent type, temperature, time during solvent heat intercalation, prepares uniform Germanium selenide two-dimensional nano piece.
7. a kind of preparation method of the Germanium selenide two-dimensional material based on solvent heat graft process as described in claim 1 is obtained
The supernatant for being dispersed with single layer or few layer Germanium selenide is preparing the application in semiconductor material.
8. application according to claim 7, it is characterised in that: the supernatant spin coating of single layer or few layer Germanium selenide will be dispersed with
Onto silicon wafer, suitable sheet layer material is found under light microscopic, in lamella both ends electrode evaporation, obtains FET device.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113181936A (en) * | 2021-04-28 | 2021-07-30 | 东南大学 | Heterojunction GeSe/TiO2Composite photocatalyst and preparation method thereof |
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Application publication date: 20181225 |