CN111748805A - Preparation method of nickel metal nano pattern - Google Patents
Preparation method of nickel metal nano pattern Download PDFInfo
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- CN111748805A CN111748805A CN202010626328.XA CN202010626328A CN111748805A CN 111748805 A CN111748805 A CN 111748805A CN 202010626328 A CN202010626328 A CN 202010626328A CN 111748805 A CN111748805 A CN 111748805A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1603—Process or apparatus coating on selected surface areas
- C23C18/1607—Process or apparatus coating on selected surface areas by direct patterning
- C23C18/1608—Process or apparatus coating on selected surface areas by direct patterning from pretreatment step, i.e. selective pre-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1834—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
Abstract
The invention discloses a preparation method of a patterned Ni nano-film, which takes gold as a substrate material, self-assembles 1, -10 decanedithiol on the surface of the gold substrate material, and prepares a Ni nano-film pattern on the gold substrate material by a solution method; the preparation method is simple, low in cost and good in repeatability, can be carried out at room temperature, the pattern of the prepared Ni nano film can be adjusted within the size range from nanometer to micrometer, can be square or round with different sizes, is complete in shape, and has the advantages of easiness in characterization, good stability and the like.
Description
Technical Field
The invention belongs to the technical field of nano-pattern preparation, and relates to a preparation method of a patterned nickel nano-film.
Background
Metallized organic thin films, i.e., the addition of a metal film to an organic molecular film, have been successfully used in polymer light emitting diodes and memory storage electronic devices. In pioneering work after the nineties of the last century, self-assembled monolayers of gold substrate surfaces became a model system for the study of metal/organic interface properties. The organic molecule has the characteristics of convenient synthesis, low cost, easy processing and capability of forming a molecular film with atomic level regularity by self-assembly, and has wide application prospect in the direction of a metallized organic film. The metalized organic film is used on the premise that: a patterned metal thin film must be formed on the organic molecular film. Patterning refers to the generation of a regular surface structure on the order of nanometers or micrometers in at least one dimension. With the development of modern scientific technology, micro-machining or patterning of micro-and nano-scale surfaces has attracted much attention. Today, people can perform micron and nanometer scale characterization on the structure and properties of a solid surface by advanced instruments such as a scanning electron microscope and an atomic force microscope, and can control the microstructure and properties on the solid surface by various physical, chemical and even biological surface patterning technologies. The use of patterning technology in the microelectronics industry, chemical and biological material micro-analysis, biochips, micro-volume reactors, combinatorial synthesis, and micro-electro-mechanical systems is rapidly growing. Researchers have used physical evaporation of metal films to form organic molecular layers on top of organic molecules, but the entire metal/organic molecule/metal structure is destroyed because metal atoms tend to penetrate the molecular film during evaporation. The metal film can be formed on the organic molecular layer by adopting a chemical vapor deposition method and an atomic layer deposition method, but the methods have many and complicated experimental steps, easily cause metal atoms to penetrate through the molecular layer to cause short circuit of a metal/organic molecule/metal structure, and increase the experimental cost because the experimental process needs to be operated in a vacuum environment. Researchers have used photosensitive resin in photoresist as a carbon source to compound with hollow nickel oxide nanospheres synthesized by a hydrothermal method to prepare patterned nickel microelectrodes (a preparation process of carbon/nickel oxide/nickel patterned microelectrodes, China patent application No. CN201610209074.5), and related reports on preparation of patterned polyethylene tetrathiol nickel films (a preparation method of patterned polyethylene tetrathiol nickel films and devices, China patent application No. CN201610937199.X), but no report has been reported so far on preparation of patterned nickel elementary substance nano films on self-assembled organic monomolecular layers.
Since the self-assembled organic monomolecular film can be connected with different materials at the head and the tail, at present, people grow one end of the organic monomolecular film and the surface of gold, and connect the other end of the organic monomolecular film with another material, such as nano particles, nano wires or nano metal films. In this case, if the self-assembled organic molecular film is patterned, nanoparticles, nanowires, or other nano-structured substances attached to the other end of the organic molecular film are also patterned accordingly. The preparation of the patterned metal nano film has important scientific significance and application value in the aspects of supermolecular science, material science, microelectronics, cell biology and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a patterned metallic nickel simple substance nano film, which has the advantages of simple preparation method, short preparation period, good reproducibility, operable room temperature environment and the like, and the prepared patterned nickel nano film is easy to characterize and good in stability.
In order to achieve the purpose, the invention adopts the following technical scheme: the method comprises the steps of taking gold as a substrate material, self-assembling 1, 10-decanedithiol on the surface of the gold substrate material by adopting a micro-contact printing method, and preparing a patterned nickel nano-film on the gold substrate material by adopting a solution method through a solution with nickel ions.
The preparation method comprises the following steps:
step 1: self-assembling a patterned 1, 10-decanedithiol organic monomolecular layer on the surface of the gold substrate material by adopting a micro-contact printing method;
step 2: nickel sulfate hexahydrate with the concentration of 0.1-0.2 mol/L and sodium dihydrogen hypophosphite solution with the concentration of 0.5-1 mol/L are mixed according to the weight ratio of 1: 2 to obtain a mixed solution;
and step 3: placing a sample self-assembled with a 1, -10 decanedithiol organic monomolecular layer into the mixed solution, carrying out water bath at 30-50 ℃ for 30-60 minutes, and taking out the sample after the water bath is finished;
and 4, step 4: and ultrasonically cleaning the taken sample by using deionized water, and then drying the sample by using a nitrogen gun to obtain the patterned nickel nano film.
And 4, the ultrasonic cleaning time is 1-5 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes a metal material self-assembled with a 1-10 decanedithiol monomolecular layer as a substrate material, and prepares a patterned nickel nano-film on the surface of the 1-10 decanedithiol monomolecular layer by a solution method. Has the characteristics of simple preparation method, low cost, good repeatability and capability of being carried out at room temperature.
The pattern size of the nickel nano-film prepared by the method can be adjusted within the size range from nanometer to micrometer, the pattern can be square or round with different sizes, the pattern shape is complete, and the method has the advantages of easy characterization, good stability and the like, and can be used in the fields of catalysts, molecular electronics, nano-reactors and the like.
Drawings
FIG. 1 is a micro-topography of a square patterned Ni nano-film prepared in example 1 of the present invention.
FIG. 2 is a micro-topography of a circular patterned Ni nano-film prepared in example 2 of the present invention.
Fig. 3 is a graph showing EDS detection results of the circular patterned Ni nano-film prepared in example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
Example 1:
step 1: self-assembling a 1, 10-decanedithiol organic monomolecular layer with a square pattern on the surface of the gold substrate material by adopting a micro-contact printing method;
step 2: nickel sulfate hexahydrate (NiSO) with the concentration of 0.1mol/L4·6H2O) and 1 mol-Sodium dihydrogen hypophosphite (NaH) of L2PO2) The solution is prepared according to the following steps of 1: 2 to obtain a mixed solution;
and step 3: putting a sample self-assembled with a 1, -10 decanedithiol organic monomolecular layer into the mixed solution, carrying out water bath at 50 ℃ for 60 minutes, and taking out the sample after the water bath is finished;
and 4, step 4: and ultrasonically cleaning the taken sample by deionized water for 5min, and blow-drying the sample by a nitrogen gun to obtain the patterned nickel nano film.
Referring to fig. 1, the Ni nano-film pattern has a square size of 50 μm × 50 μm and a complete shape.
Example 2
Step 1: self-assembling a 1, 10-decyl dithiol organic monomolecular layer with a circular pattern on the surface of the gold substrate material by adopting a micro-contact printing method;
step 2: nickel sulfate hexahydrate (NiSO) with the concentration of 0.2mol/L4·6H2O) and 0.5mol/L sodium dihydrogen hypophosphite (NaH)2PO2) The solution is prepared according to the following steps of 1: 2 to obtain a mixed solution;
and step 3: putting a sample self-assembled with a 1, -10 decanedithiol organic monomolecular layer into the mixed solution, carrying out water bath at 30 ℃ for 60 minutes, and taking out the sample after the water bath is finished;
and 4, step 4: and ultrasonically cleaning the taken sample by deionized water for 3min, and blow-drying the sample by a nitrogen gun to obtain the patterned nickel nano film.
Referring to fig. 2, the Ni nano-film pattern has a circular shape with a size of 20 μm × 20 μm and a complete shape.
Referring to fig. 3, the prepared metal nano-film is shown as a Ni nano-film.
Example 3
Step 1: self-assembling a patterned 1, 10-decanedithiol organic monomolecular layer on the surface of the gold substrate material by adopting a micro-contact printing method;
step 2: nickel sulfate hexahydrate (NiSO) with the concentration of 0.15mol/L4·6H2O) and 0.75mol/L sodium dihydrogen hypophosphite (NaH)2PO2) The solution is prepared according to the following steps of 1: 2 to obtain a mixed solution；
And step 3: putting a sample self-assembled with the 1-10 decanedithiol organic monomolecular layer into the mixed solution, carrying out water bath at 40 ℃ for 50 minutes, and taking out the sample after the water bath is finished;
and 4, step 4: and ultrasonically cleaning the taken sample by deionized water for 1min, and blow-drying the sample by a nitrogen gun to obtain the patterned nickel nano film.
Example 4
Step 1: self-assembling a patterned 1, 10-decanedithiol organic monomolecular layer on the surface of the gold substrate material by adopting a micro-contact printing method;
step 2: nickel sulfate hexahydrate (NiSO) with the concentration of 0.18mol/L4·6H2O) and 0.8mol/L sodium dihydrogen hypophosphite (NaH)2PO2) The solution is prepared according to the following steps of 1: 2 to obtain a mixed solution;
and step 3: putting a sample self-assembled with a 1, -10 decanedithiol organic monomolecular layer into the mixed solution, carrying out water bath at 50 ℃ for 30 minutes, and taking out the sample after the water bath is finished;
and 4, step 4: and ultrasonically cleaning the taken sample by deionized water for 3min, and blow-drying the sample by a nitrogen gun to obtain the patterned nickel nano film.
The metal substrate of the present invention and the procedure of self-assembling a patterned 1, 10-decanediol organic monolayer on the surface of a gold substrate material by microcontact printing are described in YanniJie, Jermey R Niskala, Aaron C Johnton-Peck, Peter J Krommenhok, Joseph B.Tracy, Huiqing Fan and Wei You, LaternallyPattern printed Magnetic nanoparticles of Material chemistry.22(5), 1962-.
In conclusion, the method is simple and convenient to operate. And preparing the patterned Ni nano film by adopting a micro-contact printing combined solution method. The method does not need to adopt a template, has low cost, simple and easily controlled preparation process, low energy consumption and good repeatability of the product.
Claims (3)
1. A method for preparing nickel metal nanometer patterns is characterized in that: the method comprises the steps of taking gold as a substrate material, self-assembling 1, 10-decanedithiol on the surface of the gold substrate material by adopting a micro-contact printing method, and preparing a patterned nickel nano-film on the gold substrate material by adopting a solution method through a solution with nickel ions.
2. The method for preparing nickel metal nanopattern according to claim 1, comprising the steps of:
step 1: self-assembling a patterned 1, 10-decanedithiol organic monomolecular layer on the surface of the gold substrate material by adopting a micro-contact printing method;
step 2: nickel sulfate hexahydrate with the concentration of 0.1-0.2 mol/L and sodium dihydrogen hypophosphite solution with the concentration of 0.5-1 mol/L are mixed according to the weight ratio of 1: 2 to obtain a mixed solution;
and step 3: placing a sample self-assembled with a 1, -10 decanedithiol organic monomolecular layer into the mixed solution, carrying out water bath at 30-50 ℃ for 30-60 minutes, and taking out the sample after the water bath is finished;
and 4, step 4: and ultrasonically cleaning the taken sample by using deionized water, and then drying the sample by using a nitrogen gun to obtain the patterned nickel nano film.
3. The method of preparing nickel metal nanopattern as set forth in claim 2, wherein: and 4, the ultrasonic cleaning time is 1-5 min.
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| CN202010626328.XA CN111748805A (en) | 2020-07-02 | 2020-07-02 | Preparation method of nickel metal nano pattern |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105110288A (en) * | 2015-08-27 | 2015-12-02 | 陕西科技大学 | Method for preparing patterned Ag nano-particles |
| CN109261984A (en) * | 2018-11-23 | 2019-01-25 | 陕西科技大学 | A kind of preparation method of Ni nano-hollow ball |
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- 2020-07-02 CN CN202010626328.XA patent/CN111748805A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105110288A (en) * | 2015-08-27 | 2015-12-02 | 陕西科技大学 | Method for preparing patterned Ag nano-particles |
| CN109261984A (en) * | 2018-11-23 | 2019-01-25 | 陕西科技大学 | A kind of preparation method of Ni nano-hollow ball |
Non-Patent Citations (2)
| Title |
|---|
| YANNI JIE等: ""Growth of nickel nanoparticles on an organic self-assembled monolayer template by means of electroless plating"", 《COLLOIDS AND SURFACES A: PHYSICOCHEMICAL AND ENGINEERING ASPECTS》 * |
| YANNI JIE等: ""Laterally patterned magnetic nanoparticles"", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
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