CN104746144B - A kind of preparation method of stannic disulfide single crystal nanoplate - Google Patents

A kind of preparation method of stannic disulfide single crystal nanoplate Download PDF

Info

Publication number
CN104746144B
CN104746144B CN201510178074.9A CN201510178074A CN104746144B CN 104746144 B CN104746144 B CN 104746144B CN 201510178074 A CN201510178074 A CN 201510178074A CN 104746144 B CN104746144 B CN 104746144B
Authority
CN
China
Prior art keywords
horizontal pipe
heating zone
pipe furnace
sns
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201510178074.9A
Other languages
Chinese (zh)
Other versions
CN104746144A (en
Inventor
孟祥敏
夏静
朱丹丹
王磊
黄奔
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Technical Institute of Physics and Chemistry of CAS
Original Assignee
Technical Institute of Physics and Chemistry of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Technical Institute of Physics and Chemistry of CAS filed Critical Technical Institute of Physics and Chemistry of CAS
Priority to CN201510178074.9A priority Critical patent/CN104746144B/en
Publication of CN104746144A publication Critical patent/CN104746144A/en
Application granted granted Critical
Publication of CN104746144B publication Critical patent/CN104746144B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/46Sulfur-, selenium- or tellurium-containing compounds
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B23/00Single-crystal growth by condensing evaporated or sublimed materials
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/64Flat crystals, e.g. plates, strips or discs

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention discloses a kind of preparation method of stannic disulfide single crystal nanoplate, and this method comprises the following steps:1) substrate is positioned over horizontal pipe furnace heating zone downstream area;2) SnS2 powder is weighed, is placed in high-temperature resistant container, then places it in diamond heating area;3) sulphur powder is weighed, is placed in another high-temperature resistant container, then places it in heating zone upstream region;4) the horizontal tube furnace pressure is reduced;5) inert gas is filled with into the horizontal pipe furnace, the horizontal pipe furnace internal pressure is returned to normal pressure, while keeping the inert gas of certain flow rate;6) the horizontal tube furnace temperature is risen to 650 750 DEG C;7) by horizontal pipe furnace heating zone Temperature fall to room temperature.This method preparation technology is simple, and repeatability is high, and controllability is strong, good crystallinity, be easily transferred to other substrates, is easy to the research and development and application of extensive photoelectric device.

Description

A kind of preparation method of stannic disulfide single crystal nanoplate
Technical field
The present invention relates to nano material technical field of semiconductors.More particularly, to a kind of preparation of single crystal nanoplate.
Background technology
Two-dimensional layer material is the class new material risen in recent years, and this kind of material Van der Waals that are otherwise known as are brilliant Body, it is noteworthy characterized by its molecular layer is combined with stronger covalent bond or ionic bond, and be then between molecular layer rely on compared with Weak van der Waals interaction power is bonded together, therefore these materials are easily formed receiving for monolayer or several molecular layers Rice chip architecture.Wherein, foremost two-dimensional layer material surely belongs to graphene, it be one kind by carbon atom with sp2Hybridized orbit group It is in the flat film of honeycomb lattice, the two-dimensional material of only one of which carbon atom thickness into hexangle type.Graphene is in the quilt of year in 2004 Physicist An Deliegaimu and its student Constant the Ting Nuowoxiao love of Univ Manchester UK) find, this It was found that making the physics Nobel Prize that this two physicists obtain 2010.Because graphene has excellent optics, electricity Learn, mechanics and thermal property, therefore suffer from fields such as electronic information, mechanics of communication, biology, catalysis, sensings huge Potential using value.However, band gap width (the E of grapheneg) it is 0eV, this defect greatly limit graphene in semiconductor Application in electronics and opto-electronics.
Recent studies have indicated that magnesium-yttrium-transition metal disulphide (molybdenum disulfide, tungsten disulfide, two selenizing molybdenums, two tungsten selenides Deng) it is a kind of excellent two-dimensional semiconductor material.Relative to graphene, transition-metal sulphides have preferable band gap knot Structure, this feature makes them have great application potential in microelectronics and optoelectronic areas;With traditional silicon, II-VI and III-V group semi-conductor material is compared, and transition-metal sulphides two-dimensional nanostructure thickness is adjustable, all can be light from individual layer to multilayer Easily obtain, make its be beneficial to device grid modulation and longitudinal direction High Density Integration (R.Cheng, S.Jiang, Y.Chen,Y.Liu,N.Weiss,H.C.Cheng,H.Wu,Y.Huang and X.F.Duan.Few-layer molybdenum disulfide transistors and circuits for high-speed flexible electronics.Nature Communication,2014,5);These two-dimensional material surface unusual lights, no chemical dangling bond, this feature make carrier From the influence of trap states, so as to obtain higher carrier mobility (RadisavljevicB, RadenovicA, BrivioJ,GiacomettiV and KisA.Single-layer MoS2 transistors.Nature Nanotechnology,2011,6,147-150);In addition, natural two-dimensional structure makes it with flexible substrates with simultaneous well Capacitive, is expected to turn into preferable flexible device material (O.Lopez-Sanchez, D.Lembke, M.Kayci, A.Radenovic and A.Kis.Ultrasensitive photodetectors based on monolayer MoS2.Nature Nanotechnology,2013,8,497-501)。
Except transition-metal sulphides, other metal chalcogenide compounds also have excellent physical and chemical performance.Wherein compared with For it is typical be exactly stannic disulfide (SnS2), stannic disulfide has typical CI2Type layer structure, band gap magnitude is in 2.2-2.35eV Between, it is commonly used for the fields such as semiconductor electronics, photoelectrocatalysis, energy storage.For example, the SnS of several molecular layers thicks2 Effect transistor is successfully prepared, its ON/OFF electric current ratio up to 106(D.De,J.Manongdo,S.See,V.Zhang, A.Guloy and H.Peng.High on/off ratio field effect transistors based on exfoliated crystalline SnS2Nano-membranes.Nanotechnology, 2013,24), therefore be expected to more Mend the deficiency that graphene is applied in semiconductor electronics and opto-electronics;In addition, SnS2Excellent catalysis is also equipped with to live Property, it can be used as the catalysis water decomposition of photoelectrochemical cell cathode material, individual layer SnS2Photoelectrolysis water efficiency can reach 38.7% It can be seen that light conversion efficiency, be current maximum (Y.F.Sun, H.Cheng, S.Gao, Z.H.Sun, Q.H.Liu, Q.Liu, F.C.Lei,T.Yao,J.F.He,S.Q.Wei and Y.Xie.Freestanding Tin Disulfide Single- Layers Realizing Efficient Visible-Light Water Splitting.AngewandteChemie- International Edition.2012,51,8727-8731);In addition, research have shown that by with the Material cladding such as graphene, Stannic disulfide can be used in lithium ion battery, and battery whole volume may be up to 650mA h g-1(B.Luo,Y.Fang, B.Wang,J.S.Zhou,H.H.Song and L.J.Zhi.Two dimensional graphene-SnS2hybrids with superior rate capability for lithium ion storage.Energy&Environmental Science,2012,5,5226-5230)。
So far, two dimension SnS is prepared2The method of single crystal nanoplate mainly include physics stripping method (D.De, J.Manongdo,S.See,V.Zhang,A.Guloy and H.Peng.High on/off ratio field effect transistors based on exfoliated crystalline SnS2nano- Membranes.Nanotechnology, 2013,24), hydrothermal synthesis method (B.Luo, Y.Fang, B.Wang, J.S.Zhou, H.H.Song and L.J.Zhi.Two dimensional graphene-SnS2hybrids with superior rate capability for lithium ion storage.Energy&Environmental Science,2012,5,5226- 5230), chemical bath deposition method (S.A.Liu, X.M.Yin, Q.Y.Hao, M.Zhang, L.M.Li, L.B.Chen, Q.H.Li, Y.G.Wang and T.H.Wang.Chemical bath deposition of SnS2nanowall arrays with improved electrochemical performance for lithium ion battery.Materials Letters.2010,64,2350-2353) etc..For semiconductor electronics application, these preparation methods are suffered from each Deficiency.Such as physics stripping method, although high-quality SnS can be obtained2Nanometer sheet, but the method poor repeatability, are prepared Nanometer sheet area is relatively small, quantity is few, be not suitable for extensive electronic device integrated;The SnS that hydrothermal synthesis method is obtained2Nanometer Piece pattern heterogeneity and crystallinity is poor, surface defect is more, can reduce carrier mobility.
Accordingly, it is desirable to provide the SnS that a kind of area is big, crystallite dimension is big, uniformity is good and quality is high2The preparation of nanometer sheet Method.
The content of the invention
The technical problem to be solved of the present invention is to provide that a kind of area is big, crystallite dimension is big, uniformity good and quality height SnS2The preparation method of nanometer sheet.
In order to solve the above technical problems, the present invention is using such as following technical proposals:
A kind of preparation method of stannic disulfide single crystal nanoplate, it comprises the following steps:
1) substrate is positioned over horizontal pipe furnace heating zone downstream area;
2) SnS is weighed2Powder, is placed in high-temperature resistant container, then places it in the horizontal pipe furnace heating zone;
3) sulphur powder is weighed, is placed in another high-temperature resistant container, then places it in the horizontal pipe furnace heating zone Upstream region;
4) the horizontal tube furnace pressure is reduced;
5) inert gas is filled with into the horizontal pipe furnace, the stove internal pressure is returned to normal pressure, while keeping certain The inert gas of flow velocity;
6) the horizontal tube furnace temperature is risen to 650-750 DEG C;
7) by horizontal pipe furnace heating zone Temperature fall to room temperature.
The above method is that normal atmosphere vapor deposition method prepares large area, large scale SnS2Nanometer sheet, it is characterized in that with curing Tin (SnS2) and sulphur powder (S) be source material, with mica sheet (mica) for substrate, inert gas is in cloud under carrier gas, hot conditions Deposition obtains large area, large-sized SnS on master slice2Nanometer sheet.
The high-temperature resistant container can be ceramic boat, corundum boat or quartz boat.
The heating zone refers to the region residing for horizontal pipe furnace heating rod;The heating zone upstream region and downstream area Correspondence flow rate of carrier gas direction, refers to the top and bottom of horizontal pipe furnace heating zone, as shown in Figure 1.
The substrate is high temperature resistant and smooth substrate, such as mica sheet, silica, quartz plate or sapphire sheet Deng the substrate needs to cut into suitable specification.The substrate is positioned over the heating zone downstream area (as shown in Figure 1), Apart from heating region 5-20cm position.Preferably, the substrate is mica sheet, it is highly preferred that the substrate is fluorophologopite Piece.In one embodiment, mica sheet is cut into 2cm × 3.5cm specification.SnS2Nanometer sheet is grown to the clear of backing material Cleanliness requires higher, it is preferable that the upper layer being exposed to mica sheet in air is removed.
Preferably, SnS2Powder is high-purity SnS2Powder, purity is not less than 99%.
The sulphur powder and SnS2Mol ratio be more than 300.High-temperature resistant container equipped with sulphur powder is positioned over apart from horizontal tube The heating zone upstream region 15-30cm of stove position.
Preferably, vacuumized to reduce horizontal tube furnace pressure with mechanical pump, it is preferable that pressure is down to below 0.1Pa, Being filled with high-purity inert gas makes pressure in stove be returned to atmospheric pressure.The inert gas is argon gas, nitrogen, helium or neon Gas, preferably argon gas.The flow velocity of the inert gas is maintained between 20-200sccm.
Preferably, between the heating rate of the horizontal pipe furnace is 10-25 DEG C/min, the heating response time is 5-30 points Clock.After heating terminates, treat that horizontal pipe furnace heating zone Temperature fall, to room temperature, takes out mica sheet substrate.
The SnS that the present invention is prepared2Nanometer sheet is in the fields such as solar cell, field-effect transistor, photocatalysis hydrogen production With important researching value and being widely applied prospect.
Beneficial effects of the present invention are as follows:
(1) preparation technology is simple, this experiment source material need to be put into horizontal pipe furnace horizontal pipe furnace, carrier gas of having friendly relations, Mix up heating program just can, a step heating response, therefore preparation process is comparatively simple;
(2) repeatability is high, i.e., prepare large area, large scale SnS in this way2The success rate of nanometer sheet is high;
(3) controllability is strong, i.e., control SnS by changing the conditions such as sedimentation time, evaporating temperature, source material quality2Receive Thickness, size, pattern of rice piece etc.;
(4) synthesis cycle is short, and this method is sampled from being heated to be reacted to finally cooling, it is only necessary to four or five hours, is taken few;
(5) good crystallinity, because we use thermal evaporation, the SnS prepared under the high temperature conditions2Nanometer sheet, so The material arrived has higher crystallinity.
(6) other substrates are easily transferred to, are easy to the research and development and application of extensive photoelectric device.
Brief description of the drawings
The embodiment to the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows SnS2The grower schematic diagram of nanometer sheet.
Fig. 2 shows to grown SnS2The mica sheet optical photograph of nanometer sheet.
Fig. 3 shows large area SnS2The optical imagery of nanometer sheet.
Fig. 4 shows SnS2Nanometer sheet AFM (AFM) image and elevation information.
Fig. 5 shows SnS2X ray diffracting data.
Fig. 6 shows SnS2Raman spectrum.
Fig. 7 shows the SnS of (a) hexagon shape2Nanometer sheet transmission electron microscope (TEM) bright field image;(b)SnS2Nanometer sheet low power is high Resolution Transmission Electron microscope (HRTEM) photo, illustration is SEAD (SAED), a set of six sub-symmetries diffraction spot card This bright nanometer sheet is monocrystalline;(c) high power HRTEM images;(d) energy dispersion X-ray spectrometer (EDX).
Embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings It is bright.Similar part is indicated with identical reference in accompanying drawing.It will be appreciated by those skilled in the art that institute is specific below The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
1. the preparation of mica sheet substrate:
1) specification of the cutting mica sheet into 2cm × 3.5cm.
2) layer on mica sheet is removed with the tapering tweezers in top, it is standby using intermediate layer as substrate.
2. prepare SnS2Nanometer sheet:
(1) the mica sheet substrate is put in horizontal pipe furnace heating zone downstream area, apart from heating zone 5-20cm.
(2) 20mg SnS is weighed2Powder (purity is not less than 99%) is put into ceramic boat, is then put in horizontal tube The heating zone of formula stove.
(3) sulphur powder (excess) for weighing 1g is placed in another ceramic boat, is then put in the heating zone of horizontal pipe furnace Upstream region, apart from heated center 18cm.
(4) vacuumized with mechanical pump, pressure in stove is down to below 0.1Pa.
(5) being filled with high purity argon makes pressure in horizontal pipe furnace return to atmospheric pressure, and argon gas flow velocity is maintained at 80sccm.
(6) horizontal pipe furnace is heated to 700 DEG C, heating rate is maintained at 20 DEG C/min, the heat time is 20 points Clock.
(7) after heating terminates, treat that horizontal pipe furnace Temperature fall, to room temperature, takes out mica sheet substrate.
As shown in Fig. 2 can see that well-proportioned one layer of yellow film in mica substrate.Table is carried out using light microscope Levy, acquired results are as shown in Figure 3.Occur the hexagon of random distribution or rescinded angle hexagonal nanosheet in mica substrate, its is straight Footpath is in several microns between hundreds of microns.AFM, which is characterized, shows that these nanometer sheet thickness are about 100nm, as a result as schemed Shown in 4.X-ray diffraction, which characterizes these nanometer sheets, has 2T type hexagonal structures, and its bottom crystal face is (0001) face, as shown in Figure 5. The Raman of nanometer sheet, which is characterized, shows its Raman spectrum in 313.9cm-1And 202.2cm-1There are two peaks, artificial gold is corresponded to respectively A1gAnd EgRaman peaks.Therefore Raman, which is characterized, proves that these nanometer sheets are stannic disulfide really, as shown in Figure 6.Transmission electron microscopy Mirror characterization result is as shown in Figure 7:Wherein Fig. 7 a are the TEM bright field images of a hexagon nanometer sheet;Fig. 7 b are this nanometer sheets It is 0.32nm between the lattice fringe measured in low power HRTEM pictures, figure, just with { 10-10 } interplanar distance phase of stannic disulfide It is the corresponding SAED pictures in this region Deng, illustration, a set of six sub-symmetries diffraction spot proves that this nanometer sheet is monocrystalline;Fig. 7 c are pair 7b high power HRTEM images are answered, its lattice arrangement is consistent with the arrangement of the sulphur or tin atom of stannic disulfide, all arranged in six sides Row;Fig. 7 d are EDX data, and it, which shows, several elements of sulphur, tin, copper, chromium, carbon in nanometer sheet, and wherein copper, chromium, carbon comes from carbon branch Film and electronic microscope sample rod are held, illustration shows that the atomic ratio of sulphur and tin is about 2:1, it was demonstrated that this nanometer sheet is stannic disulfide.
Embodiment 2
1. the preparation of mica sheet substrate:
1) specification of the cutting mica sheet into 2cm × 3.5cm.
2) layer on mica sheet is removed with the tapering tweezers in top, it is standby using intermediate layer as substrate.
2. prepare SnS2Nanometer sheet:
(1) mica sheet substrate is put in horizontal pipe furnace heating zone downstream area, apart from heating zone 5-20cm.
(2) 20mg SnS is weighed2Powder (purity is not less than 99%) is put into ceramic boat, is then put in horizontal tube The heating zone heart of formula stove.
(3) sulphur powder (excess) for weighing 0.5g is placed in another ceramic boat, is then put in the heating of horizontal pipe furnace Center upstream region, apart from heated center 15cm.
(4) vacuumized with mechanical pump, pressure in stove is down to below 0.1Pa.
(5) being filled with high-purity argon gas makes pressure in horizontal pipe furnace return to atmospheric pressure, and argon gas flow velocity is maintained at 120sccm.
(6) horizontal pipe furnace is heated to 650 DEG C, heating rate is maintained at 20 DEG C/min, the heat time is 20 minutes.
(7) after heating terminates, treat that horizontal pipe furnace Temperature fall, to room temperature, takes out mica sheet substrate.
Embodiment 3
1. the preparation of mica sheet substrate:
1) specification of the cutting mica sheet into 2cm × 3.5cm.
2) layer on mica sheet is removed with the tapering tweezers in top, it is standby using intermediate layer as substrate.
2. prepare SnS2Nanometer sheet:
(1) mica sheet substrate is put in horizontal pipe furnace heating zone downstream area, apart from heated center 5-20cm.
(2) 30mg SnS is weighed2Powder (purity is not less than 99%) is put into another ceramic boat, is then put in water The heating zone of flat tube furnace.
(3) sulphur powder (excess) for weighing 1.6g is placed in another ceramic boat, is then put in the heating of horizontal pipe furnace Area's upstream region, apart from heating zone 22cm.
(4) vacuumized with mechanical pump, pressure in stove is down to below 0.1Pa.
(5) being filled with high pure nitrogen makes pressure in horizontal pipe furnace return to atmospheric pressure, and nitrogen flow rate is maintained at 40sccm.
(6) horizontal pipe furnace is heated to 750 DEG C, heating rate is maintained at 20 DEG C/min, the heat time is 20 minutes.
(7) after heating terminates, treat that the horizontal pipe furnace Temperature fall, to room temperature, takes out mica sheet substrate.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.

Claims (4)

1. a kind of preparation method of stannic disulfide single crystal nanoplate, it is characterised in that comprise the following steps:
1) substrate is positioned over horizontal pipe furnace heating zone downstream area;
2) SnS is weighed2Powder, is placed in high-temperature resistant container, then places it in the horizontal pipe furnace heating zone;
3) sulphur powder is weighed, is placed in another high-temperature resistant container, then places it in horizontal pipe furnace heating zone upstream Region;
4) the horizontal tube furnace pressure is reduced;
5) inert gas is filled with into the horizontal pipe furnace, stove internal pressure is returned to normal pressure, while keeping the lazy of certain flow rate Property gas;
6) the horizontal tube furnace temperature is risen to 650-750 DEG C;
7) by horizontal pipe furnace heating zone Temperature fall to room temperature;
The substrate is mica sheet, silica, quartz plate or sapphire sheet;
The substrate is positioned over apart from heating zone 5-20cm position;
Container equipped with sulphur powder is positioned over apart from heated center 15-30cm position;
Pressure in the heater is reduced to below 0.1Pa;
Step 6) horizontal pipe furnace heating rate be 10-25 DEG C/min, the heating response time be 5-30 minutes.
2. the preparation method of stannic disulfide single crystal nanoplate according to claim 1, it is characterised in that:The sulphur powder with SnS2Mol ratio be more than 300.
3. the preparation method of stannic disulfide single crystal nanoplate according to claim 1, it is characterised in that:SnS2Powder it is pure Degree more than 99%.
4. the preparation method of stannic disulfide single crystal nanoplate according to claim 1, it is characterised in that:The inert gas For argon gas, nitrogen, helium or neon.
CN201510178074.9A 2015-04-15 2015-04-15 A kind of preparation method of stannic disulfide single crystal nanoplate Active CN104746144B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510178074.9A CN104746144B (en) 2015-04-15 2015-04-15 A kind of preparation method of stannic disulfide single crystal nanoplate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510178074.9A CN104746144B (en) 2015-04-15 2015-04-15 A kind of preparation method of stannic disulfide single crystal nanoplate

Publications (2)

Publication Number Publication Date
CN104746144A CN104746144A (en) 2015-07-01
CN104746144B true CN104746144B (en) 2017-10-17

Family

ID=53586373

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510178074.9A Active CN104746144B (en) 2015-04-15 2015-04-15 A kind of preparation method of stannic disulfide single crystal nanoplate

Country Status (1)

Country Link
CN (1) CN104746144B (en)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105463580B (en) * 2016-01-07 2018-05-08 中国科学院理化技术研究所 A kind of preparation method of cadmium selenide or cadmium sulfide two dimension single crystal nanoplate
CN105420815B (en) * 2016-01-07 2018-01-30 中国科学院理化技术研究所 A kind of method of controllable preparation orthorhombic phase stannous sulfide two dimension single crystal nanoplate
CN109956495B (en) * 2017-12-25 2020-12-22 中国科学院物理研究所 Vertical staggered petal-shaped tin disulfide nanosheet and preparation method thereof
CN108103580A (en) * 2017-12-27 2018-06-01 广东工业大学 A kind of preparation method of two sulphur stannic selenide single-crystal semiconductor material
CN108531981A (en) * 2018-03-09 2018-09-14 广东工业大学 A method of preparing two-dimentional indium trisulfide monocrystalline in mica substrate
CN109650354B (en) * 2019-01-22 2022-09-20 中国科学院苏州纳米技术与纳米仿生研究所 Preparation method and application of two-dimensional lead telluride nanosheet and nanomaterial
CN110028098B (en) * 2019-05-31 2020-04-07 南京倍格电子科技有限公司 High-concentration SnS prepared by liquid-phase stripping method2Nano-sheet
CN113484302B (en) * 2021-07-01 2022-12-13 中国科学院上海硅酸盐研究所 SnS with capillary effect 2 Microsphere SERS substrate and preparation method and application thereof
CN114477270B (en) * 2022-02-21 2023-10-27 福建师范大学 Method for growing ultrathin stannous sulfide nanosheets by sulfur passivation

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103614777A (en) * 2013-10-15 2014-03-05 中国科学院理化技术研究所 Preparation method of large-area single-layer or multi-layer molybdenum diselenide single chip
CN104178815A (en) * 2014-08-18 2014-12-03 中国科学院理化技术研究所 Method for epitaxial growth of large-area monocrystal ZnS film on monocrystal ZnO substrate

Also Published As

Publication number Publication date
CN104746144A (en) 2015-07-01

Similar Documents

Publication Publication Date Title
CN104746144B (en) A kind of preparation method of stannic disulfide single crystal nanoplate
Yue et al. Two-dimensional high-quality monolayered triangular WS2 flakes for field-effect transistors
Tao et al. The effect of seed layer on morphology of ZnO nanorod arrays grown by hydrothermal method
Wen et al. Epitaxial 2D PbS nanoplates arrays with highly efficient infrared response
Zhao et al. Controlled synthesis of single-crystal SnSe nanoplates
Nie et al. Ultrafast growth of large-area monolayer MoS2 film via gold foil assistant CVD for a highly sensitive photodetector
CN105420815B (en) A kind of method of controllable preparation orthorhombic phase stannous sulfide two dimension single crystal nanoplate
Hu et al. Controlled growth and photoconductive properties of hexagonal SnS 2 nanoflakes with mesa-shaped atomic steps
CN104538288B (en) A kind of device and method of direct growth atomic scale two-dimensional semiconductor hetero-junctions
Wang et al. Chemical vapor deposition growth of two-dimensional monolayer gallium sulfide crystals using hydrogen reduction of Ga2S3
CN110416065B (en) Preparation method of molybdenum disulfide/tungsten diselenide vertical heterojunction
CN103614777A (en) Preparation method of large-area single-layer or multi-layer molybdenum diselenide single chip
Wang et al. Control growth of catalyst-free high-quality ZnO nanowire arrays on transparent quartz glass substrate by chemical vapor deposition
Zhu et al. van der Waals epitaxy and photoresponse of two-dimensional CdSe plates
CN104389016A (en) Method for quickly preparing large-size single-crystal graphene
CN107445204A (en) A kind of method for preparing transient metal chalcogenide compound nano flake and vanadium disulfide, two selenizing vanadium nano flakes
CN106159000A (en) A kind of prepare the method for uniform monolayers molybdenum sulfide under centimeter scale
CN108069416B (en) Ultra-clean graphene and preparation method thereof
Xia et al. van der Waals epitaxial two-dimensional CdS x Se (1− x) semiconductor alloys with tunable-composition and application to flexible optoelectronics
CN107539976A (en) A kind of method that carbon dioxide prepares ultra-clean graphene
Chen et al. Growth of 12-inch uniform monolayer graphene film on molten glass and its application in PbI 2-based photodetector
Shekari et al. High-quality GaN nanowires grown on Si and porous silicon by thermal evaporation
Guo et al. Controllable synthesis of MoS2 nanostructures from monolayer flakes, few-layer pyramids to multilayer blocks by catalyst-assisted thermal evaporation
Xu et al. 2D perovskite single crystals for photodetectors: from macro‐to microscale
Ekthammathat et al. Growth of hexagonal prism ZnO nanorods on Zn substrates by hydrothermal method and their photoluminescence

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant