CN110467159A - It is a kind of from driving, microcell, position ion insertion and patterning method - Google Patents

It is a kind of from driving, microcell, position ion insertion and patterning method Download PDF

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CN110467159A
CN110467159A CN201910641135.9A CN201910641135A CN110467159A CN 110467159 A CN110467159 A CN 110467159A CN 201910641135 A CN201910641135 A CN 201910641135A CN 110467159 A CN110467159 A CN 110467159A
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wire
intercalation
microcell
ion insertion
positioning
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CN110467159B (en
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谢伟广
赖浩杰
王思媛
陈楠
陈科球
刘彭义
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Jinan University
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/04—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion materials in the liquid state
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • ing And Chemical Polishing (AREA)

Abstract

The invention discloses a kind of from driving, microcell, position ion insertion and patterning method, method includes the following steps: choosing the wire with negative electricity chemical potential of high-purity, the tip with certain curvature radius is obtained using electrochemical etching, it prepares certain density metal salt solution and drips on two-dimensional material surface, wire after etching is fixed on the higher Three dimensions control platform of precision, wire is moved by control platform, make metallic wire tip and material surface contact by optical microscopy simultaneously, intercalation starts to carry out in contact site, the performance optimization of material is realized by the reaction, including widening response spectrum range and realizing local function, wire is controlled simultaneously to be moved on the surface of the material according to the pattern set, available positioning intercalation pattern, this is that existing intercalation technique is unable to reach.The present invention realizes that high-resolution patterning obtains remarkable result in regulation two-dimensional material property and at the nanoscale.

Description

It is a kind of from driving, microcell, position ion insertion and patterning method
Technical field
The present invention relates to Semiconductor Optoeletronic Materials technical fields, and in particular to a kind of to realize Ionic domain positioning from driving Intercalation, patterned method.
Background technique
Ion insertion is the technical method for regulating and controlling a kind of strength of two-dimensional material physicochemical properties.Currently, ion insertion Intercalation can be realized by introducing gas phase or melting ion in two-dimensional material growth course, this method can be prepared on a large scale Material, but it is difficult to control accurately intercalation, it can not especially realize in the material in-situ inserted.Another intercalation method is using zero Valence metal carries out intercalation after chemistry.Reversible, lossless intercalation may be implemented in this method, but the metastable state presoma of intercalation is unstable It is fixed, seriously limit intercalation type and scalability.Electrochemical intercalation method is a kind of method being widely used at present, it has can Inverse, easily controllable advantage.However, electrochemical method needs prepare microelectrode simultaneously by micro fabrication first on material It is aided with reference electrode, external bias setting and ionic conduction liquid/solid electrolyte, method is complicated, costly and time consuming.If Ion insertion is further applied to the production of complicated semiconductor heterostructure device and device integrates, positions intercalation and pattern Change will be essential technique, and above method cannot achieve this requirement.Complicated micro fabrication can be avoided, Intercalation 2D material is prepared in Partial controll intercalation and constructs the key challenge of complex devices.
Summary of the invention
The purpose of the present invention is to solve drawbacks described above in the prior art, provide a kind of from driving, microcell, position from Sub- intercalation and patterning method.
The purpose of the present invention can be reached by adopting the following technical scheme that:
It is a kind of from driving, microcell, position ion insertion and patterning method, the method the following steps are included:
Two-dimensional material is immersed into acid or metal salt solution, and is placed under optical microscopy and focuses observation surface；
The wire with negative electricity chemical potential for choosing high-purity has negative electricity chemical potential using electrochemical method etching Wire obtains the tip with certain curvature radius；
Wire is fixed on Three dimensions control platform, so that metallic wire tip is contacted two-dimensional material surface, utilizes Three dimensions control Platform keeps wire mobile with certain rate on two-dimensional material surface according to the figure of setting, and the positioning for being achieved in ion is inserted Layer pattern.
Further, the wire is the wire that standard electrode EMF is negative value, is selected from zinc silk, iron wire, tin silk One of or it is a variety of, but be not limited only to this, purity is higher than 99%.
Further, the process of the wire using electrochemical method etching with negative electricity chemical potential is as follows:
One end of wire and conducting wire is immersed in etching liquid, the other end respectively connects current source positive and negative anodes, and the inclined of 2-6V is arranged Pressure, etch period 10-60s.
Further, there is the radius of curvature of the wire of negative electricity chemical potential to be no more than 100 μ using electrochemical method etching M, the wire after etching are cleaned using acetone or alcohol is further.
Further, the metal salt solution includes at least one of salting liquid of Li, Na, K, Co, Cu and Sn, institute The metal salt solute purity stated is higher than 99%, and the metal salt solution concentration is 1mol/L-10-6mol/L。
Further, the two-dimensional material has characteristic of semiconductor, including MoO3、MoS2、WS2、MoSe2、WSe2、 At least one of Graphene, but it is not limited only to this.
Further, the three-dimensional platform precision is better than 2 μm.
Further, the rate that the wire moves on the surface of the material preferably 50 μm/s.
The present invention has the following advantages and effects with respect to the prior art:
(1) electrochemical intercalation and chemical graft process is mostly used to realize ion insertion to regulate and control two-dimensional material property at present, but It is for electrochemical intercalation method, it is desirable to provide the tedious steps such as external bias and device preparation encapsulation, and it is proposed by the present invention Ion insertion method passes through merely wire and contacts with two-dimensional material, and electric charge transfer occurs for the otherness of electrode potential to each other, Spontaneous reaction is realized under the premise of without carrying out preparation early period to device.
(2) furthermore current intercalation method all cannot achieve positioning intercalation, this to further to do two-dimensional material in situ special Journal of Sex Research has certain limitation, and positioning intercalation pattern may be implemented by the way that control wire is mobile in the present invention, these are existing What technology cannot achieve, local intercalation is positioned by ion, realizes topical functional, furthermore the molybdenum oxide of broad-band gap is by inserting Layer realizes the ultraviolet detection to near-infrared wide spectrum, can be applied to radionetric survey, Photometric Measurement, and infrared thermal imaging is infrared distant The application such as sense.
Detailed description of the invention
Fig. 1 (a) is the zinc silk schematic diagram before electrochemical etching；
Fig. 1 (b) is the zinc silk schematic diagram after electrochemical etching；
Fig. 2 (a) is optics picture of the zinc silk not in contact with molybdenum oxide；
Fig. 2 (b) is the optics picture of the rigid catalytic oxidation molybdenum of zinc silk；
Fig. 2 (c) is the zinc silk optics picture mobile in molybdenum oxide surface；
Fig. 3 (a) is the optics picture schematic diagram for positioning intercalation and realizing patterning (J)；
Fig. 3 (b) is the optics picture schematic diagram for positioning intercalation and realizing patterning (N)；
Fig. 3 (c) is the optics picture schematic diagram for positioning intercalation and realizing patterning (U)；
Fig. 4 is the high-resolution optical picture schematic diagram for positioning intercalation molybdenum oxide nanometer sheet and obtaining；
Fig. 5 is the XRD characterization contrast schematic diagram before and after cobalt ions intercalation molybdenum oxide nanometer sheet；
Fig. 6 (a) is the photoresponse figure of cobalt ions intercalation molybdenum oxide nanometer sheet；
Fig. 6 (b) is cobalt ions intercalation molybdenum oxide nanometer sheet magnetism microscope figure；
Fig. 7 (a) is cobalt ions intercalation MoS2The optical picture of front and back；
Fig. 7 (b) is cobalt ions intercalation WS2The optical picture of front and back；
Fig. 7 (c) is cobalt ions intercalation MoSe2The optical picture of front and back；
Fig. 7 (d) is cobalt ions intercalation WSe2The optical picture of front and back；
Fig. 7 (e) is the optical picture before and after cobalt ions intercalation Graphene；
Fig. 8 (a) is cobalt ions intercalation MoS2The Raman characterization comparison diagram of front and back；
Fig. 8 (b) is cobalt ions intercalation WS2The Raman characterization comparison diagram of front and back；
Fig. 8 (c) is cobalt ions intercalation MoSe2The Raman characterization comparison diagram of front and back；
Fig. 8 (d) is cobalt ions intercalation WSe2The Raman characterization comparison diagram of front and back；
Fig. 8 (e) is the Raman characterization comparison diagram before and after cobalt ions intercalation Graphene；
Fig. 9 (a) is cobalt ions intercalation MoS2The emission spectrum comparison diagram of front and back；
Fig. 9 (b) is cobalt ions intercalation WS2The emission spectrum comparison diagram of front and back；
Fig. 9 (c) is cobalt ions intercalation MoSe2The emission spectrum comparison diagram of front and back；
Fig. 9 (d) is cobalt ions intercalation WSe2The emission spectrum of front and back compares.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Embodiment one
Present embodiment discloses a kind of Co ion positioning intercalation molybdenum oxide nanometer sheets to realize patterned process, including following Step:
S1, preparation MoO3Nanometer sheet and monocrystalline:
It weighs 0.3g molybdenum oxide powder to be placed in tube furnace in crucible, lining is being placed at powder source or so 12cm Bottom.It keeps under atmospheric environment, tube furnace is warming up to 750-780 DEG C, preferably 780 DEG C, heating rate is 50 DEG C/min, is kept Temperature-resistant 60-120min, natural cooling cooling, molybdenum oxide monocrystalline deposition is on tube wall and substrate can find that width is 10-20 μ The molybdenum oxide nanometer sheet of m.
S2, electrochemical etching zinc silk:
The HCl solution that 10ml concentration is 37% is measured, adds 40ml deionized water to be diluted, selects diameter for 300 μm One end of zinc silk is connected to current source negative pole as shown in Fig. 1 (a) by zinc silk, and the other end is immersed in hydrochloric acid, selects the termination of conducting wire one The positive grade of current source, the other end are immersed in hydrochloric acid, and biasing 2-6V reacts 10s-60s, and preferably 5V reacts 30s, 300 μm of diameter Zinc silk is etched to 40 μm of tip, as shown in Fig. 1 (b).
S3, preparing metal salting liquid:
Metal salt solution can be at least one of the salting liquid that metal is Li, Na, K, Co, Cu and Sn, and metal salt is molten Liquid concentration is 10-1mol/L-10-3mol/L.In this embodiment, metal salt solution is cobalt sulfate solution, and cobalt sulfate solution is matched System: take 0.01g sulfuric acid cobalt dust that 60ml deionized water is added, ultrasonic vibration 10min, wherein the purity of sulfuric acid cobalt dust is higher than 99.9%.
S4, positioning intercalation is realized:
The zinc silk etched is fixed on Three dimensions control platform, there will be the substrate of molybdenum oxide nanometer sheet to be placed in optical microscopy It is lower and by cobalt sulfate solution drop in substrate surface, using three-dimensional platform slowly by zinc silk tip close to molybdenum oxide surface, but the two Intercalation starts to carry out when contacting in the solution, metachromasia occurs near contact site at this time, as zinc silk is aoxidizing Molybdenum surface is mobile, and color change interval also gradually extends, and shown in haptoreaction process such as Fig. 2 (a)-Fig. 2 (c), inserts finally by positioning Layer, which reacts, successfully forms the pattern of JNU in molybdenum oxide surface, as shown in Fig. 3 (a)-Fig. 3 (c), by changing zinc silk amount curvature Radius realizes more high-resolution pattern, as shown in Figure 4.
In cobalt sulfate solution, zinc silk is cathode, and molybdenum oxide is positive grade, since the potential difference of two-stage causes electronics to pass through It is transferred to molybdenum oxide from zinc silk by contact site, causes molybdenum oxide surface charged to attract the metal cation in solution to realize Intercalation, Fig. 4 are the XRD comparison before and after intercalation, according to Bragg diffraction, cause interlayer swollen since ion enters Van der Waals gap It is swollen, so that the peak position in the face (0k0) shifts toward low-angle.The molybdenum oxide after cobalt ions intercalation also shows visible-close simultaneously The response (such as Fig. 6 (a)) of infrared wide spectrum further, since magnetic ion doping so that non magnetic molybdenum oxide realizes office The enhancing (such as Fig. 6 (b)) of domain stray magnetic field.
Embodiment two
Present embodiment discloses a kind of Cu ion positioning intercalation molybdenum oxide nanometer sheets to realize patterned process, including following Step:
S1, preparation MoO3Nanometer sheet and monocrystalline；
S2, electrochemical etching zinc silk；
Step S1 and S2 specific implementation process, with embodiment one；
S3, prepare copper nitrate solution: take 0.01g nitric acid copper powders be added 60ml deionized water, ultrasonic vibration 5-10min, Solution is dripped in substrate surface.
S4, positioning intercalation is realized:
Step S4 specific implementation process, with embodiment one.
Embodiment three
Present embodiment discloses a kind of Co ions to position intercalation MoS2Nanometer sheet realizes patterned process, including following step It is rapid:
S1, preparation MoS2Nanometer sheet:
Take double source heat growth MoS2Nanometer sheet weighs 0.3g molybdenum oxide powder and is placed in tube furnace in crucible, 0.1g sulphur powder is being placed at powder source 15cm, and substrate is placed at the other end 12cm apart from powder source.Logical 100sccm argon Gas, 150 DEG C of sulphur powder source heating, oxidation molybdenum source heat up 760 DEG C, and heating rate is 50 DEG C/min, keep the temperature 1h, and natural cooling cools down, Substrate can find that width is 10-30 μm of MoS2Nanometer sheet.
S2, electrochemical etching zinc silk；
S3, preparing metal salting liquid；
S4, positioning intercalation is realized.
Step S1 and S2 specific implementation process, with embodiment one.
Fig. 7 (a)-Fig. 7 (e) indicates cobalt ions intercalation MoS2、WS2、MoSe2、WSe2, optics picture before and after Graphene, Size is 10 μm, is all changed a lot using the material color of zinc silk contact surface, this may be caused due to the increase of thickness Refractive index change.Meanwhile using the 532nm laser of 0.1% laser intensity to MoS2、WS2、MoSe2、WSe2、Graphene Raman characterization (Fig. 8 (a)-Fig. 8 (e)) and emission spectrum characterization test (Fig. 9 (a)-Fig. 9 (d)) are done before and after intercalation, before finding intercalation Corresponding Raman peaks and emission peak are basically unchanged afterwards, but intensity obviously weakens, this shows that the material after intercalation is shown relatively by force Electro sonic Coupling the phenomenon that.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (8)

1. a kind of from driving, microcell, positioning ion insertion and patterning method, which is characterized in that the method includes following Step:
Two-dimensional material is immersed into acid or metal salt solution, and is placed under optical microscopy and focuses observation surface；
The wire with negative electricity chemical potential for choosing high-purity has the metal of negative electricity chemical potential using electrochemical method etching Silk obtains the tip with certain curvature radius；
Wire is fixed on Three dimensions control platform, so that metallic wire tip is contacted two-dimensional material surface, utilizes Three dimensions control platform Keep wire mobile with certain rate on two-dimensional material surface according to the figure of setting, is achieved in the positioning intercalation figure of ion Case.
2. a kind of driving certainly according to claim 1, microcell, positioning ion insertion and patterning method, feature exist In, the wire is the wire that standard electrode EMF is negative value, it is selected from one of zinc silk, iron wire, tin silk or a variety of, Its purity is higher than 99%.
3. a kind of driving certainly according to claim 1, microcell, positioning ion insertion and patterning method, feature exist In the process of the wire using electrochemical method etching with negative electricity chemical potential is as follows:
One end of wire and conducting wire is immersed in etching liquid, the other end respectively connects current source positive and negative anodes, and the bias of 2-6V is arranged, and carves Lose time 10-60s.
4. a kind of driving certainly according to claim 1, microcell, positioning ion insertion and patterning method, feature exist In the radius of curvature using wire of the electrochemical method etching with negative electricity chemical potential is no more than 100 μm, the metal after etching Silk is cleaned using acetone or alcohol.
5. a kind of driving certainly according to claim 1, microcell, positioning ion insertion and patterning method, feature exist In the metal salt solution includes at least one of salting liquid of Li, Na, K, Co, Cu and Sn, the metal salt solute Purity is higher than 99%, and the metal salt solution concentration is 1mol/L-10-6mol/L。
6. a kind of driving certainly according to claim 1, microcell, positioning ion insertion and patterning method, feature exist In the two-dimensional material has characteristic of semiconductor, including MoO3、MoS2、WS2、MoSe2、WSe2, in Graphene at least one Kind.
7. a kind of driving certainly according to claim 1, microcell, positioning ion insertion and patterning method, feature exist In the three-dimensional platform precision is better than 2 μm.
8. a kind of driving certainly according to claim 1, microcell, positioning ion insertion and patterning method, feature exist In the rate that the wire moves on the surface of the material is 50 μm/s.
CN201910641135.9A 2019-07-16 2019-07-16 Self-driving, micro-area, positioning ion intercalation and patterning method Active CN110467159B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150275378A1 (en) * 2014-03-31 2015-10-01 Korea Institute Of Science And Technology Method for preparation of graphene using spontaneous process
US20170260637A1 (en) * 2016-03-09 2017-09-14 Aruna Zhamu Electrochemical production of graphene sheets directly from graphite mineral
CN109216648A (en) * 2018-08-21 2019-01-15 中国科学院金属研究所 Ion is embedded in the intercalation electrode and its preparation method and application that two-dimensional layer material is constructed in advance
CN109928427A (en) * 2019-03-21 2019-06-25 暨南大学 A kind of double ion intercalation molybdenum oxide nanometer sheet, hetero-junctions and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150275378A1 (en) * 2014-03-31 2015-10-01 Korea Institute Of Science And Technology Method for preparation of graphene using spontaneous process
US20170260637A1 (en) * 2016-03-09 2017-09-14 Aruna Zhamu Electrochemical production of graphene sheets directly from graphite mineral
CN109216648A (en) * 2018-08-21 2019-01-15 中国科学院金属研究所 Ion is embedded in the intercalation electrode and its preparation method and application that two-dimensional layer material is constructed in advance
CN109928427A (en) * 2019-03-21 2019-06-25 暨南大学 A kind of double ion intercalation molybdenum oxide nanometer sheet, hetero-junctions and preparation method thereof

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