CN110467159B - Self-driving, micro-area, positioning ion intercalation and patterning method - Google Patents

Self-driving, micro-area, positioning ion intercalation and patterning method Download PDF

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CN110467159B
CN110467159B CN201910641135.9A CN201910641135A CN110467159B CN 110467159 B CN110467159 B CN 110467159B CN 201910641135 A CN201910641135 A CN 201910641135A CN 110467159 B CN110467159 B CN 110467159B
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CN110467159A (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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    • 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
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Abstract

The invention discloses a self-driving, micro-area, positioning ion intercalation and patterning method, which comprises the following steps: the method comprises the steps of selecting a high-purity metal wire with negative electrochemical potential, obtaining a tip with a certain curvature radius by electrochemical etching, preparing a metal salt solution with a certain concentration, dripping the metal salt solution on the surface of a two-dimensional material, fixing the etched metal wire on a three-dimensional control platform with higher precision, moving the metal wire through the control platform, enabling the tip of the metal wire to be in contact with the surface of the material by means of an optical microscope, and starting intercalation reaction at a contact part. The invention obtains remarkable effect in regulating and controlling the property of the two-dimensional material and realizing high-resolution patterning under the nanoscale.

Description

Self-driving, micro-area, positioning ion intercalation and patterning method
Technical Field
The invention relates to the technical field of semiconductor photoelectron materials, in particular to a method for realizing ion micro-area positioning intercalation and patterning by self-driving.
Background
Ion intercalation is a powerful technical method for regulating and controlling the physicochemical properties of two-dimensional materials. At present, the intercalation can be realized by introducing gas phase or molten ions in the growth process of a two-dimensional material, and the method can prepare the material in large scale, but the intercalation is difficult to accurately control, and particularly the in-situ intercalation can not be realized in the material. Another intercalation method is chemical post-intercalation with zero-valent metal. The method can realize reversible and lossless intercalation, but the metastable precursor for intercalation is unstable, and the intercalation variety and expansibility are severely limited. The electrochemical intercalation method is widely applied at present and has the advantages of reversibility and easy control. However, the electrochemical method requires first preparing microelectrodes on a material by microfabrication process while assisting with reference electrodes, external bias arrangement, and ionic conducting liquid/solid electrolyte, and is complicated, expensive, and time-consuming. If the ion intercalation is further applied to the manufacture of complex semiconductor heterostructure devices and the integration of the devices, the positioning intercalation and the patterning are indispensable processes, and the above methods can not realize the requirement. The key challenges of preparing the intercalation 2D material and constructing a complex device in local control intercalation can be avoided by using a complex micromachining process.
Disclosure of Invention
The present invention is directed to overcoming the above-mentioned deficiencies in the prior art and providing a self-driven, micro-domain, localized ion intercalation and patterning process.
The purpose of the invention can be achieved by adopting the following technical scheme:
a self-driven, micro-domain, localized ion intercalation and patterning process, said process comprising the steps of:
immersing a two-dimensional material into an acidic or metal salt solution, and placing the two-dimensional material under an optical microscope to focus and observe the surface;
selecting a high-purity metal wire with negative electrochemical potential, and etching the metal wire with negative electrochemical potential by adopting an electrochemical method to obtain a tip with a certain curvature radius;
fixing the metal wire on a three-dimensional control platform, enabling the tip of the metal wire to contact the surface of the two-dimensional material, and enabling the metal wire to move on the surface of the two-dimensional material at a certain speed according to the set pattern by utilizing the three-dimensional control platform, thereby realizing the positioning intercalation pattern of ions.
Further, the metal wire is a metal wire with a negative standard electrode potential, and is selected from one or more of zinc wire, iron wire and tin wire, but not limited thereto, and the purity of the metal wire is higher than 99%.
Further, the process of electrochemically etching the metal wire with negative electrochemical potential is as follows:
one end of the metal wire and one end of the lead are soaked in the etching solution, the other end of the metal wire and the lead are respectively connected with the anode and the cathode of a current source, 2-6V bias voltage is set, and the etching time is 10-60 s.
Furthermore, the curvature radius of the metal wire with negative electrochemical potential is etched by adopting an electrochemical method and is not more than 100 mu m, and the etched metal wire is further cleaned by adopting acetone or ethanol.
Further, the metal salt solution comprises at least one of salt solutions of Li, Na, K, Co, Cu and Sn, the purity of the metal salt solution is higher than 99%, and the concentration of the metal salt solution is 1mol/L-10-6mol/L。
Further, the two-dimensional material has semiconductor properties, including MoO3、MoS2、WS2、MoSe2、WSe2And Graphene, but not limited thereto.
Furthermore, the precision of the three-dimensional platform is better than 2 mu m.
Further, the moving speed of the metal wire on the surface of the material is preferably 50 μm/s.
Compared with the prior art, the invention has the following advantages and effects:
(1) at present, the two-dimensional material properties are adjusted and controlled by mainly adopting an electrochemical intercalation method and a chemical intercalation method, but for the electrochemical intercalation method, complicated steps such as external bias, device preparation and encapsulation and the like need to be provided, but the ion intercalation method provided by the invention is only in contact with the two-dimensional material through a metal wire, the charge transfer is generated by the difference of electrode potentials among the two-dimensional material, and the spontaneous reaction is realized on the premise of not preparing the device in the early stage.
(2) In addition, the current intercalation method can not realize positioning intercalation, which has certain limitation on further in-situ two-dimensional material characteristic research, the invention can realize positioning intercalation patterns by controlling the movement of metal wires, which can not be realized by the prior art, local functionality is realized by ion positioning local intercalation, and in addition, the molybdenum oxide with wide band gap realizes the detection of ultraviolet to near infrared wide spectrum through intercalation, and can be applied to ray measurement, photometric measurement, infrared thermal imaging, infrared remote sensing and the like.
Drawings
FIG. 1(a) is a schematic representation of a zinc wire prior to electrochemical etching;
FIG. 1(b) is a schematic representation of a zinc wire after electrochemical etching;
FIG. 2(a) is an optical photograph of a zinc wire not in contact with molybdenum oxide;
FIG. 2(b) is an optical picture of zinc wire just in contact with molybdenum oxide;
FIG. 2(c) is an optical picture of zinc wire moving on the surface of molybdenum oxide;
FIG. 3(a) is a schematic optical picture of localized intercalation implementing patterning (J);
FIG. 3(b) is a schematic optical picture of positioning intercalation to realize patterning (N);
FIG. 3(c) is a schematic optical picture of positioning intercalation implementing patterning (U);
FIG. 4 is a schematic view of a high resolution optical picture obtained by positioning intercalated molybdenum oxide nanoplates;
FIG. 5 is a comparative schematic diagram of XRD characterization before and after intercalation of cobalt ions into molybdenum oxide nanosheets;
fig. 6(a) is a photoresponse plot of cobalt ion intercalated molybdenum oxide nanoplates;
fig. 6(b) is a magnetic micrograph of cobalt ion intercalated molybdenum oxide nanosheets;
FIG. 7(a) is a cobalt ion intercalated MoS2Front and back optical diagrams;
FIG. 7(b) shows cobalt ion intercalation WS2Front and back optical images;
FIG. 7(c) is intercalation of cobalt ions into MoSe2Front and back optical diagrams;
FIG. 7(d) is a WSe with intercalation of cobalt ions2Front and back optical diagrams;
FIG. 7(e) is an optical diagram before and after intercalation of cobalt ions into Graphene;
FIG. 8(a) is a cobalt ion intercalated MoS2Before and after Raman characterization contrast diagram;
FIG. 8(b) shows cobalt ion intercalation WS2Before and after Raman characterization contrast diagram;
FIG. 8(c) is intercalation of cobalt ions into MoSe2Before and after Raman characterization contrast diagram;
FIG. 8(d) is a WSe with intercalation of cobalt ions2Before and after Raman characterization contrast diagram;
FIG. 8(e) is a comparison of Raman characterization before and after intercalation of cobalt ions into Graphene;
FIG. 9(a) is a cobalt ion intercalated MoS2Comparing the emission spectra before and after;
FIG. 9(b) shows cobalt ion intercalation WS2Comparing the emission spectra before and after;
FIG. 9(c) is intercalation of cobalt ions into MoSe2Comparing the emission spectra before and after;
FIG. 9(d) is a WSe with intercalation of cobalt ions2And comparing the emission spectra before and after.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The embodiment discloses a process for realizing patterning of Co ion positioning intercalation molybdenum oxide nanosheets, which comprises the following steps:
s1 preparation of MoO3Nanosheet and single crystal:
0.3g of molybdenum oxide powder was weighed into a crucible and placed in a tube furnace, and the substrate was placed 12cm from the powder source. And (3) keeping the atmospheric environment, heating the tube furnace to 750-780 ℃, preferably 780 ℃, at the heating rate of 50 ℃/min, keeping the temperature unchanged for 60-120min, naturally cooling and cooling, wherein molybdenum oxide single crystals are deposited on the tube wall, and the substrate can find molybdenum oxide nano-sheets with the width of 10-20 mu m.
S2, electrochemically etching the zinc wire:
measuring 10ml of HCl solution with the concentration of 37%, adding 40ml of deionized water for dilution, selecting a zinc wire with the diameter of 300 microns, connecting one end of the zinc wire to the negative electrode of a current source, soaking the other end of the zinc wire in hydrochloric acid, selecting one end of a lead wire to be connected with a positive level of the current source, soaking the other end of the lead wire in the hydrochloric acid, applying a bias voltage of 2-6V for reaction for 10-60s, preferably 5V for reaction for 30s, and etching the zinc wire with the diameter of 300 microns into a tip of 40 microns as shown in FIG. 1 (b).
S3, preparing a metal salt solution:
the metal salt solution may be at least one of Li, Na, K, Co, Cu and Sn, and has a concentration of 10-1mol/L-10-3mol/L. In this example, the metal salt solution is a cobalt sulfate solution, and the preparation of the cobalt sulfate solution is as follows: 0.01g of cobalt sulfate powder is added into 60ml of deionized water, and ultrasonic oscillation is carried out for 10min, wherein the purity of the cobalt sulfate powder is higher than 99.9%.
S4, positioning intercalation:
fixing the etched zinc wire on a three-dimensional control platform, placing a substrate with molybdenum oxide nano-sheets under an optical microscope, dripping cobalt sulfate solution on the surface of the substrate, slowly enabling the tip of the zinc wire to be close to the surface of the molybdenum oxide by using the three-dimensional platform, starting intercalation reaction when the zinc wire and the molybdenum oxide are contacted in the solution, generating color change reaction near the contact part, gradually extending a color change area along with the movement of the zinc wire on the surface of the molybdenum oxide, wherein the contact reaction process is as shown in fig. 2(a) -2 (c), and finally successfully forming JNU patterns on the surface of the molybdenum oxide through positioning the intercalation reaction, as shown in fig. 3(a) -3 (c), realizing higher resolution patterns by changing the curvature radius of the zinc wire limit, as shown in fig. 4.
In a cobalt sulfate solution, a zinc wire is a negative electrode, molybdenum oxide is a positive electrode, electrons are transferred from the zinc wire to the molybdenum oxide through a contact part due to potential difference of two stages, so that the surface of the molybdenum oxide is charged to attract metal cations in the solution to realize intercalation, fig. 4 shows XRD contrast before and after intercalation, and according to Bragg diffraction, the peak position of a (0k0) plane is shifted to a small angle due to the fact that ions enter a Van der Waals gap to cause interlayer expansion. Meanwhile, the molybdenum oxide after cobalt ion intercalation also shows a wide spectrum response of visible-near infrared (as shown in figure 6(a)), and in addition, due to the doping of magnetic ions, the non-magnetic molybdenum oxide realizes the enhancement of local stray magnetic field (as shown in figure 6 (b)).
Example two
The embodiment discloses a process for realizing patterning of a Cu ion positioning intercalation molybdenum oxide nanosheet, which comprises the following steps:
s1 preparation of MoO3Nanosheets and single crystals;
s2, electrochemically etching the zinc wire;
the steps S1 and S2 are implemented in the same manner as in the first embodiment;
s3, preparing a copper nitrate solution: 0.01g of copper nitrate powder is added into 60ml of deionized water, and the solution is dripped on the surface of the substrate after ultrasonic oscillation for 5-10 min.
S4, positioning intercalation:
step S4 is implemented in the same manner as in the first embodiment.
EXAMPLE III
The embodiment discloses a Co ion positioning intercalation MoS2The process for patterning the nanosheet comprises the following steps:
s1 preparation of MoS2Nanosheet:
MoS growth by adopting double-source heating2And (3) weighing 0.3g of molybdenum oxide powder, putting the molybdenum oxide powder into a crucible, putting the crucible into a tube furnace, putting 0.1g of sulfur powder at a position 15cm away from a powder source, and putting a substrate at a position 12cm away from the other end of the powder source. Introducing 100sccm argon, heating the sulfur powder source to 150 ℃, heating the molybdenum oxide source to 760 ℃, heating at a rate of 50 ℃/min, keeping the temperature for 1h, naturally cooling and cooling to find MoS with the width of 10-30 mu m on the substrate2Nanosheets.
S2, electrochemically etching the zinc wire;
s3, preparing a metal salt solution;
and S4, realizing positioning intercalation.
The steps S1 and S2 are implemented in the same manner as in the first embodiment.
FIGS. 7(a) to 7(e) show cobalt ion intercalationLayer MoS2、WS2、MoSe2、WSe2The optical pictures before and after Graphene, with dimensions of 10 μm, all have a certain change in the color of the material on the contact surface with the zinc wire, which may result in a change in the refractive index due to an increase in the thickness. Meanwhile, 532nm laser with 0.1% laser intensity is adopted for MoS2、WS2、MoSe2、WSe2Raman characterization (figure 8(a) -figure 8(e)) and emission spectrum characterization test (figure 9(a) -figure 9(d)) are carried out before and after Graphene intercalation, and the corresponding Raman peak and emission peak are basically unchanged before and after intercalation, but the intensity is obviously weakened, which indicates that the material after intercalation shows a stronger electro-acoustic coupling phenomenon.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (6)

1. A self-driven, micro-domain, localized ion intercalation and patterning process, comprising the steps of:
immersing a two-dimensional material into an acidic or metal salt solution, and placing the two-dimensional material under an optical microscope to focus and observe the surface;
selecting a high-purity metal wire with negative electrochemical potential, and etching the metal wire with negative electrochemical potential by adopting an electrochemical method to obtain a tip with a certain curvature radius; wherein, the curvature radius of the metal wire with negative electrochemical potential etched by an electrochemical method is not more than 100 μm, and the etched metal wire is cleaned by acetone or ethanol;
fixing a metal wire on a three-dimensional control platform, enabling the tip of the metal wire to contact the surface of a two-dimensional material, and enabling the metal wire to move on the surface of the two-dimensional material at a certain speed according to a set pattern by using the three-dimensional control platform, thereby realizing the positioning intercalation pattern of ions; the two-dimensional material has semiconductor properties and comprises MoO3、MoS2、WS2、MoSe2、WSe2And Graphene.
2. The self-driven, micro-domain, localized ion intercalation and patterning process of claim 1, wherein the metal wire is a wire with a negative standard electrode potential selected from one or more of zinc wire, iron wire, and tin wire with a purity of greater than 99%.
3. The self-driven, micro-area, localized ion intercalation and patterning method of claim 1, wherein the electrochemically etching of the wire with negative electrochemical potential is performed as follows:
one end of the metal wire and one end of the lead are soaked in the etching solution, the other end of the metal wire and the lead are respectively connected with the anode and the cathode of a current source, 2-6V bias voltage is set, and the etching time is 10-60 s.
4. The self-driven, micro-domain, localized ion intercalation and patterning process of claim 1, wherein the metal salt solution comprises at least one of Li, Na, K, Co, Cu and Sn, the metal salt solution has a purity of greater than 99%, and the metal salt solution has a concentration of 1mol/L to 10 mol/L-6mol/L。
5. The method of claim 1, wherein the three-dimensional control platform has a precision better than 2 μm.
6. The method of claim 1, wherein the wire is moving at a rate of 50 μm/s over the surface of the material.
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Citations (2)

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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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KR101563585B1 (en) * 2014-03-31 2015-10-28 한국과학기술연구원 Method for preparation of graphene using spontaneous process
US11247906B2 (en) * 2016-03-09 2022-02-15 Global Graphene Group, Inc. Electrochemical production of graphene sheets directly from graphite mineral

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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