CN108383148A - The preparation method of copper sulphide nano chip arrays - Google Patents
The preparation method of copper sulphide nano chip arrays Download PDFInfo
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- CN108383148A CN108383148A CN201810181257.XA CN201810181257A CN108383148A CN 108383148 A CN108383148 A CN 108383148A CN 201810181257 A CN201810181257 A CN 201810181257A CN 108383148 A CN108383148 A CN 108383148A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5007—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with salts or salty compositions, e.g. for salt glazing
- C04B41/5014—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with salts or salty compositions, e.g. for salt glazing containing sulfur in the anion, e.g. sulfides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/65—Coating or impregnation with inorganic materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of preparation methods of copper sulphide nano chip arrays.It includes solwution method, especially the specific steps are in the copper film of 20 500nm of substrate surface vapor deposition thickness, obtain the substrate that copper film is covered with to surface, later, the substrate that surface is first covered with to copper film is placed in the sodium sulfide solution of 0.001 0.1wt% and impregnates at least 4h, it is rinsed after being drawn off again, a length of 100 2000nm of piece is made, the purpose product that piece thickness is 10 50nm.It can grow copper sulphide nano chip arrays in a variety of substrates, and have that the raw material used is few, environmentally protective, energy- and time-economizing, feature at low cost, so make purpose product be extremely easy to widely commercial applications in solar cell, photocatalysis, sensor field.
Description
Technical field
The present invention relates to a kind of preparation method of nano-chip arrays, especially a kind of preparation side of copper sulphide nano chip arrays
Method.
Background technology
Nano-copper sulfide due to stable physicochemical property and excellent photoelectric properties, and solar cell, photocatalysis,
Extensive use in terms of sensing receives the extensive concern of people.Currently, the method for preparing nano-copper sulfide mainly has hydro-thermal
Method, pyrolysismethod, as Chinese invention patent application CN 106057478A announced on October 26th, 2016 one kind in nickel foam table
Face generates the preparation method and applications of coarse CuS nanosheet array.Preparation method described in the application for a patent for invention file
First to be pre-processed to nickel foam, after nickel foam Surface Creation copper simple substance layer, given birth in foam nickel surface using hydro-thermal method
At coarse CuS nanosheet array.Though this preparation method can obtain copper sulphide nano chip arrays, but also there is shortcoming,
First, product is that copper sulphide nano chip arrays invest foam nickel surface, limits the occasion of its application;Secondly, in preparation process
The raw material being related to is more, such as hydrochloric acid, copper chloride, ethyl alcohol, sulphur powder, and hydrochloric acid therein easily pollutes the environment;Again, it makes
Standby process is complex, not only consumes energy, also time-consuming.
Invention content
The technical problem to be solved in the present invention is to overcome shortcoming in the prior art, and providing one kind can be in a variety of substrate
Upper growth, and the raw material used is few, the preparation method of the copper sulphide nano chip arrays of energy- and time-economizing.
To solve the technical problem of the present invention, used technical solution is the preparation method of copper sulphide nano chip arrays
Including solwution method, especially:
Step 1, it in the copper film of substrate surface vapor deposition thickness 20-500nm, obtains to surface and is covered with the substrate of copper film;
Step 2, the substrate that surface is first covered with to copper film is placed in the sodium sulfide solution of 0.001-0.1wt% and impregnates at least
4h, then rinsed after being drawn off, a length of 100-2000nm of piece is made, the copper sulphide nano chip arrays that piece thickness is 10-50nm.
Preparation method as copper sulphide nano chip arrays is further improved:
Preferably, before copper film is deposited to the surface of substrate, ethyl alcohol and deionized water cleaning are first used for.
Preferably, substrate is silicon chip substrate or ceramic bases or substrate of glass.
Preferably, it is deposited as magnetron sputtering or electron beam evaporation or electro-deposition or chemical vapor deposition.
Preferably, surface is covered with to the substrate of copper film, and to be placed in time for being impregnated in sodium sulfide solution be 4-6h.
Preferably, it rinses as using deionized water or distilled water flushing 2-3 times.
Advantageous effect compared with the existing technology is:
First, being characterized using scanning electron microscope to purpose product obtained, and combine preparation method it is found that purpose product
To be covered with nano-chip arrays in substrate;Wherein, a length of 100-2000nm of the piece of the nanometer sheet in nano-chip arrays, piece thickness are 10-
50nm.Nanometer sheet is made of copper sulfide.This purpose product being assembled by Nano slices of copper sulphide array, both due to copper sulfide nano
The speciality of rice chip arrays, and change because the material of substrate can be with the special-purpose of purpose product, to greatly expand mesh
Product applicability.
Second, preparation method is simple, science, efficiently.The purpose production that can be grown in a variety of substrates has not only been made
Object --- copper sulphide nano chip arrays, also there is that the raw material used is few, environmentally protective, energy- and time-economizing, feature at low cost, in turn
Make purpose product be extremely easy to widely commercial applications in solar cell, photocatalysis, sensor field.
Description of the drawings
Fig. 1 is to use one of the result that scanning electron microscope (SEM) is characterized to purpose product made from preparation method.Its
In, figure a in Fig. 1, figure b and to scheme the concentration that c is sodium sulfide solution be respectively 0.001wt%, 0.01wt% and 0.1wt%
When, the SEM image of purpose product obtained.
Specific implementation mode
The preferred embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
It buys from market or is voluntarily made first:
Silicon chip substrate, ceramic bases and substrate of glass as substrate;
Sodium sulfide solution;
Ethyl alcohol;
Deionized water;
Distilled water.
Then:
Embodiment 1
Prepare the specific steps are:
Step 1, first substrate is cleaned using ethyl alcohol and deionized water.Then at the copper film of substrate surface vapor deposition thickness 20nm;Its
In, substrate is silicon chip substrate, is deposited as magnetron sputtering, obtains to surface and be covered with the substrate of copper film.
Step 2, the substrate that surface is first covered with to copper film is placed in the sodium sulfide solution of 0.001wt% and impregnates 6h.Again will
It is rinsed 2 times after taking out using deionized water (or distilled water), and the copper sulphide nano chip arrays as shown in a figures in Fig. 1 are made.
Embodiment 2
Prepare the specific steps are:
Step 1, first substrate is cleaned using ethyl alcohol and deionized water.Then at the copper film of substrate surface vapor deposition thickness 140nm;Its
In, substrate is silicon chip substrate, is deposited as magnetron sputtering, obtains to surface and be covered with the substrate of copper film.
Step 2, the substrate that surface is first covered with to copper film is placed in the sodium sulfide solution of 0.005wt% and impregnates 5.5h.Again
It is rinsed 2 times using deionized water (or distilled water) after being drawn off, copper sulphide nano shown in a figures being similar in Fig. 1 is made
Chip arrays.
Embodiment 3
Prepare the specific steps are:
Step 1, first substrate is cleaned using ethyl alcohol and deionized water.Then at the copper film of substrate surface vapor deposition thickness 260nm;Its
In, substrate is silicon chip substrate, is deposited as magnetron sputtering, obtains to surface and be covered with the substrate of copper film.
Step 2, the substrate that surface is first covered with to copper film is placed in the sodium sulfide solution of 0.01wt% and impregnates 5h.Again by it
It is rinsed 3 times using deionized water (or distilled water) after taking-up, the copper sulphide nano chip arrays as shown in the b figures in Fig. 1 is made.
Embodiment 4
Prepare the specific steps are:
Step 1, first substrate is cleaned using ethyl alcohol and deionized water.Then at the copper film of substrate surface vapor deposition thickness 380nm;Its
In, substrate is silicon chip substrate, is deposited as magnetron sputtering, obtains to surface and be covered with the substrate of copper film.
Step 2, the substrate that surface is first covered with to copper film is placed in the sodium sulfide solution of 0.015wt% and impregnates 4.5h.Again
It is rinsed 3 times using deionized water (or distilled water) after being drawn off, copper sulphide nano shown in the b figures being similar in Fig. 1 is made
Chip arrays.
Embodiment 5
Prepare the specific steps are:
Step 1, first substrate is cleaned using ethyl alcohol and deionized water.Then at the copper film of substrate surface vapor deposition thickness 500nm;Its
In, substrate is silicon chip substrate, is deposited as magnetron sputtering, obtains to surface and be covered with the substrate of copper film.
Step 2, the substrate that surface is first covered with to copper film is placed in the sodium sulfide solution of 0.1wt% and impregnates 4h.Again by it
It is rinsed 3 times using deionized water (or distilled water) after taking-up, the copper sulphide nano chip arrays as shown in the c figures in Fig. 1 is made.
It selects the silicon chip substrate or ceramic bases or substrate of glass as substrate respectively again, is deposited as magnetron sputtering or electronics
Beam evaporation or electro-deposition or chemical vapor deposition repeat above-described embodiment 1-5, have equally been made as or have been similar to shown in FIG. 1
Copper sulphide nano chip arrays.
Obviously, those skilled in the art can carry out the preparation method of the copper sulphide nano chip arrays of the present invention various
Modification and variation is without departing from the spirit and scope of the present invention.If in this way, belonging to this to these modifications and changes of the present invention
Within the scope of invention claim and its equivalent technologies, then the present invention is also intended to include these modifications and variations.
Claims (6)
1. a kind of preparation method of copper sulphide nano chip arrays, including solwution method, it is characterised in that key step is as follows:
Step 1, it in the copper film of substrate surface vapor deposition thickness 20-500nm, obtains to surface and is covered with the substrate of copper film;
Step 2, the substrate that surface is first covered with to copper film is placed in the sodium sulfide solution of 0.001-0.1wt% and impregnates at least 4h,
It is rinsed after being drawn off again, a length of 100-2000nm of piece is made, the copper sulphide nano chip arrays that piece thickness is 10-50nm.
2. the preparation method of copper sulphide nano chip arrays according to claim 1, it is characterized in that in the surface steaming to substrate
Before copper plating film, it is first used for ethyl alcohol and deionized water cleaning.
3. the preparation method of copper sulphide nano chip arrays according to claim 1, it is characterized in that substrate is silicon chip substrate, or
Ceramic bases or substrate of glass.
4. the preparation method of copper sulphide nano chip arrays according to claim 1, it is characterized in that vapor deposition is magnetron sputtering, or
Electron beam evaporation or electro-deposition or chemical vapor deposition.
5. the preparation method of copper sulphide nano chip arrays according to claim 1, it is characterized in that surface is covered with copper film
It is 4-6h that substrate, which is placed in time for being impregnated in sodium sulfide solution,.
6. the preparation method of copper sulphide nano chip arrays according to claim 1, it is characterized in that rinsing to use deionization
Water or distilled water flushing 2-3 times.
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CN201810181257.XA CN108383148A (en) | 2018-03-06 | 2018-03-06 | The preparation method of copper sulphide nano chip arrays |
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CN201810181257.XA CN108383148A (en) | 2018-03-06 | 2018-03-06 | The preparation method of copper sulphide nano chip arrays |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111974415A (en) * | 2020-08-31 | 2020-11-24 | 北京化工大学 | Copper sulfide/brass mesh electrode material with nanosheet array structure and preparation method and application thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106057478A (en) * | 2016-05-11 | 2016-10-26 | 郑州大学 | Preparation method of generating rough CuS nanosheet array on foamed nickel surface and application of rough CuS nanosheet array |
-
2018
- 2018-03-06 CN CN201810181257.XA patent/CN108383148A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106057478A (en) * | 2016-05-11 | 2016-10-26 | 郑州大学 | Preparation method of generating rough CuS nanosheet array on foamed nickel surface and application of rough CuS nanosheet array |
Non-Patent Citations (6)
Title |
---|
I. ZAAFARANY等: "Corrosion of copper electrode in sodium sulfide solution", 《JOURNAL OF SAUDI CHEMICAL SOCIETY》 * |
PIYUSH KAR等: "Anodic Cu2S and CuS nanorod and nanowall arrays: preparation, properties and application in CO2photoreduction", 《NANOSCALE》 * |
T. SAKAMOTO等: "Nanometer-scale switches using copper sulfide", 《APPLIED PHYSICS LETTERS》 * |
YAN LEI等: "A very facile, low temperature, one-step route toin situ fabricate copper sulfide nanosheet thin films", 《CRYSTENGCOMM》 * |
YUANQIANG WANG等: "CuxS counter electrodes in-situ prepared via the sulfidation of magnetron sputtering Cufilm for quantum dot sensitized solar cells", 《JOURNAL OF POWER SOURCES》 * |
洪晓丹等: "三种CuS对电极的制备及其对量子点敏化太阳能电池光电性能的影响", 《电化学》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111974415A (en) * | 2020-08-31 | 2020-11-24 | 北京化工大学 | Copper sulfide/brass mesh electrode material with nanosheet array structure and preparation method and application thereof |
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Application publication date: 20180810 |