CN108060436B - A method of nano-wire array is prepared using low-melting-point metal as bridging agent - Google Patents
A method of nano-wire array is prepared using low-melting-point metal as bridging agent Download PDFInfo
- Publication number
- CN108060436B CN108060436B CN201711285677.4A CN201711285677A CN108060436B CN 108060436 B CN108060436 B CN 108060436B CN 201711285677 A CN201711285677 A CN 201711285677A CN 108060436 B CN108060436 B CN 108060436B
- Authority
- CN
- China
- Prior art keywords
- pct
- substrate
- low
- melting
- sample
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/006—Nanostructures, e.g. using aluminium anodic oxidation templates [AAO]
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/20—Separation of the formed objects from the electrodes with no destruction of said electrodes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Cell Electrode Carriers And Collectors (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of methods that nano-wire array is prepared using low-melting-point metal as bridging agent, comprising the following steps: cleans to PCT and Cu substrate；Appropriate low-melting alloy powder is placed on Cu substrate, then it is heated in high-temperature cabinet, when temperature reaches, kept for a period of time to guarantee that low-melting-point metal all melts, it is then shut off and directly opens high-temperature cabinet, PCT is placed on the low-melting-point metal of fusing, guarantee molten metal as far as possible is uniformly contacted with PCT, then in another Cu plate of PCT upper press cover, high-temperature cabinet is then reopened；It is then shut off high-temperature cabinet, is taken out after sample is cooling, the Cu plate of top gland is removed, obtain the sample of PCT and Cu substrate phase adhesion；Electrolyte is added in electrolytic cell and carries out chemical deposition process；Sample is taken out, is heated in a water bath, so that the low-melting-point metal of substrate is melted and is fallen off together with the Cu substrate of bottom, realizes being kept completely separate for template and substrate.
Description
Technical field
This patent be related to nano-wire array preparation field more particularly to it is a kind of using low-melting-point metal as bridging agent prepare
The method of nano-wire array.
Background technique
Electrochemical deposition-template is to select have the porous as cathode of nano aperture, utilizes the substance in electrolyte
Enter material directionally in nano pore in the electrochemical reducting reaction of cathode, the hole wall of template will limit synthesized material
Shape and size, to obtain nano material.
The step of being typically prepared nano-wire array are as follows: first pass through etching and obtain the template with nano-pore；Then in template
One side sputtering layer of metal film be used as cathode, anode is using inert electrode；Electrochemical deposition process is carried out, pattern hole is deposited
It is full and it is long portal outer, when nano wire is covered to the upper surface of template, stopping electrochemical deposition process, (this process passes through observation
Current density in reaction process is judged: when material deposits in hole, electric current is almost unchanged；When growing cap, make face
Product becomes larger, so that electric current becomes larger；When material is when template upper surface increases, electric current increase is slack-off, when material covers with whole surface
When, electric current tends to definite value.)；Template is finally dissolved, to obtain nano-wire array.The nanometer material obtained by the above process
The phenomenon that material, the conductive metallic material as cathode is often difficult to remove, usually there will be adhesion electrode metal at one end, obtains
Nano-wire array it is not pure enough.
Summary of the invention
In order to overcome the deficiencies of the prior art, the present invention provides one kind prepares nano wire using low-melting-point metal as bridging agent
The method of array, the preparation method are on the basis of Conventional electrochemical deposition-template, to the connection type of electrode and template
On be adjusted, using low-melting-point metal as bridging agent, can simply realize electrode and the adhesion of template with separate, thus
More simple it can must obtain purer nano-wire array.
A method of nano-wire array is prepared using low-melting-point metal as bridging agent, which is characterized in that including following step
It is rapid:
(1) PCT and Cu substrate is cleaned, removes surface irregularities, is subsequently placed in high temperature drying case and is dried；
(2) the appropriate low-melting alloy powder lower than 80 DEG C is placed on the Cu substrate of step (1) acquisition, then in high temperature
It is heated in case, when temperature reaches, holding a period of time to guarantee that low-melting-point metal all melts, is then shut off and direct
High-temperature cabinet is opened, PCT is placed on the low-melting-point metal of fusing, guarantee molten metal as far as possible is uniformly contacted with PCT, then
In another Cu plate of PCT upper press cover, then reopen high-temperature cabinet, temperature be set as again before numerical value, keep a timing
Between；It is then shut off high-temperature cabinet, is taken out after sample is cooling, the Cu plate of top gland is removed, obtain the phase adhesion of PCT and Cu substrate
Sample；
(3) electrolyte is added in electrolytic cell；Using Pt electrode as positive and negative anodes, positive and negative anodes are fixed, are in the two
The sample that step (2) obtain is connected by face position with cathode, then by electrolytic cell as shaking in ultrasonic washing instrument
It swings, the air in PCT hole is discharged, and solution is allowed sufficiently to soak PCT, electrolytic cell is transferred to thermostatted water after ultrasonic treatment
It bathes in magnetic stirring apparatus, carries out chemical deposition process；
(4) when nano wire covers with whole surface, stop electrochemical deposition process, take out sample, heat, make in a water bath
The low-melting-point metal of substrate is melted and is fallen off together with the Cu substrate of bottom, realizes being kept completely separate for template and substrate；
(5) sample that step (4) obtain is placed in methylene chloride, in ultrasonic washing instrument, dissolves PCT template, then
It is cleaned three times with deionized water, it is ensured that PCT is removed, and can be obtained nano material.
Compared with the conventional method compared with, the beneficial effects of the present invention are:
Use low-melting-point metal connection template and substrate as electrode, make electrochemical deposition process, convenient for template and
The separation of electrode, by the temperature-fall period that suitably heats up, separation process may make template and low melting point gold using heating water bath
It is more thorough to belong to separation, relatively pure nano material can be obtained.
Detailed description of the invention:
Fig. 1 is placement position figure of the sample before heating；
Fig. 2 be obtain use low-melting-point metal as the sample schematic diagram of bridging agent；
Fig. 3 is electrochemical deposition schematic diagram；
Fig. 4 is that low-melting-point metal and substrate remove schematic diagram.
Figure label explanation: I Cu plate；Ⅱ PCT；III low-melting-point metal；IV metal Co ion；1 metal Co nano wire；2
Template；3 low-melting-point metals；4Cu substrate；5 beakers；6 water-baths.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment:
Ethanol solution and dilute H are used in ultrasonic cleaning instrument2SO4Solution respectively carries out polycarbonate template PCT and Cu substrate
Clean 10min, then clean 3min in ultrasonic washing instrument using deionized water, be placed in high temperature drying case after completing into
Row drying, temperature are set as 100 DEG C, drying time 5min；By CoSO4·7H2O、H3BO4400mL is configured to deionized water
The electrolyte of pH=3；Appropriate low-melting alloy, that is, martial virtue alloy (70 DEG C of fusing point) is placed on the Cu plate after cleaning, is then put
It on zirconium plate, is heated in high-temperature cabinet, temperature is set as 75 DEG C, and when temperature reaches, holding 5 minutes to guarantee low melting point
Metal all melts, and is then shut off and directly opens high-temperature cabinet, PCT is placed on the low-melting-point metal of fusing with tweezers, so
High-temperature cabinet is then reopened, temperature is set as 75 again in another copper sheet of PCT upper press cover afterwards to apply pressure appropriate
DEG C, the retention time is 5 minutes.It is then shut off high-temperature cabinet, is taken out after sample is cooling.Electrolytic cell is added in prepared electrolyte
In；Using Pt electrode as positive and negative anodes, positive and negative anodes are fixed, make the two in face position, the sample for then obtaining previous step
Product are connected with cathode.By electrolytic cell as vibrating 5min in supersonic wave cleaning machine.Electrolytic cell is transferred to constant temperature after ultrasonic treatment
In water-bath magnetic stirring apparatus, water-bath maintains 26 DEG C (room temperatures), and voltage is set as 1.0V；To Co nanowire growth to top layer, stop
Only electrochemical deposition process takes out sample, heats in a water bath, and bath temperature is set as 75 DEG C, and sample inclination is placed, to melt
Low-melting-point metal after change is fallen, it is made to fall off together with the Cu substrate of bottom, realizes being kept completely separate for template and substrate；By upper one
The sample that step obtains is placed in methylene chloride, and 30min is vibrated in ultrasonic washing instrument, dissolves PCT template, then use deionized water
Cleaning is three times.It can be obtained pure Co nano wire.
Claims (1)
1. a kind of method for preparing nano-wire array using low-melting alloy as bridging agent, which comprises the following steps:
(1) polycarbonate template PCT and Cu substrate is cleaned, removes surface irregularities, and be dried；
(2) low-melting alloy powder of the appropriate fusing point lower than 80 DEG C is placed on the Cu substrate of step (1) acquisition, then in high temperature
It is heated in case, when temperature reaches, holding a period of time to guarantee that low-melting alloy all melts, is then shut off and direct
High-temperature cabinet is opened, PCT is placed on the low-melting alloy of fusing, guarantee molten metal as far as possible is uniformly contacted with PCT, then
In another Cu plate of PCT upper press cover, then reopen high-temperature cabinet, temperature be set as again before numerical value, keep a timing
Between；It is then shut off high-temperature cabinet, is taken out after sample is cooling, the Cu plate of top gland is removed, obtain the phase adhesion of PCT and Cu substrate
Sample；
(3) electrolyte is added in electrolytic cell；Using Pt electrode as positive and negative anodes, positive and negative anodes are fixed, make the two in face
The sample that step (2) obtain is connected with cathode, then electrolytic cell is placed in ultrasonic washing instrument and is vibrated, is made by position
Air discharge in PCT hole, and solution is allowed sufficiently to soak PCT, electrolytic cell is transferred to water bath with thermostatic control magnetic after ultrasonic treatment
In power blender, electrochemical deposition process is carried out；
(4) when nano wire covers with whole surface, stop electrochemical deposition process, take out sample, heat in a water bath, make substrate
Low-melting alloy melt and fall off together with the Cu substrate of bottom, realize being kept completely separate for template and substrate；
(5) sample that step (4) obtain is placed in methylene chloride, in ultrasonic washing instrument, dissolves PCT template, then spend
Ionized water cleans three times, it is ensured that PCT is removed, and can be obtained nano material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711285677.4A CN108060436B (en) | 2017-12-07 | 2017-12-07 | A method of nano-wire array is prepared using low-melting-point metal as bridging agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711285677.4A CN108060436B (en) | 2017-12-07 | 2017-12-07 | A method of nano-wire array is prepared using low-melting-point metal as bridging agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108060436A CN108060436A (en) | 2018-05-22 |
| CN108060436B true CN108060436B (en) | 2019-08-23 |
Family
ID=62135369
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711285677.4A Active CN108060436B (en) | 2017-12-07 | 2017-12-07 | A method of nano-wire array is prepared using low-melting-point metal as bridging agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108060436B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109192918A (en) * | 2018-07-27 | 2019-01-11 | 苏州市模度智能科技有限公司 | A kind of the single battery temperature device for fusing and its blowout method of power battery module |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332272A (en) * | 2001-07-09 | 2002-01-23 | 杭州五源材料发展有限公司 | Manufacture of nanometer material reinforced electroformed crystalline metal product |
| CN103303861A (en) * | 2013-05-14 | 2013-09-18 | 中国科学院上海硅酸盐研究所 | Three-dimensional ordered precious metal nanotube array electrode and preparation method thereof |
| CN107099822A (en) * | 2017-05-12 | 2017-08-29 | 信阳师范学院 | Bipolar metal nanometer line and preparation method thereof |
| CN107265439A (en) * | 2017-05-11 | 2017-10-20 | 江西理工大学 | A kind of method of the lossless separation of carbon nano-tube macroscopic film |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102012021222B4 (en) * | 2012-10-27 | 2015-02-05 | Forschungszentrum Jülich GmbH | Process for producing a nanoporous layer on a substrate |
-
2017
- 2017-12-07 CN CN201711285677.4A patent/CN108060436B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332272A (en) * | 2001-07-09 | 2002-01-23 | 杭州五源材料发展有限公司 | Manufacture of nanometer material reinforced electroformed crystalline metal product |
| CN103303861A (en) * | 2013-05-14 | 2013-09-18 | 中国科学院上海硅酸盐研究所 | Three-dimensional ordered precious metal nanotube array electrode and preparation method thereof |
| CN107265439A (en) * | 2017-05-11 | 2017-10-20 | 江西理工大学 | A kind of method of the lossless separation of carbon nano-tube macroscopic film |
| CN107099822A (en) * | 2017-05-12 | 2017-08-29 | 信阳师范学院 | Bipolar metal nanometer line and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Ce＇line Rousse •Patrick Fricoteaux.Electrodeposition of thin films and nanowires Ni–Fe alloys,study of their magnetic susceptibility.《J Mater Sci》.2011,第46卷 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108060436A (en) | 2018-05-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108070883B (en) | A method of pure nanometer cobalt array is prepared based on anodic oxidation aluminium formwork method | |
| KR100767053B1 (en) | Preparation method of metal uranium and apparatus thereused | |
| CN110061191A (en) | A kind of 3-dimensional metal cathode of lithium and the preparation method and application thereof | |
| JP7357936B2 (en) | Graphene manufacturing method and graphene manufacturing device | |
| KR101093663B1 (en) | Method for manufacturing CZTS film by one step electrodeposition | |
| CN108060436B (en) | A method of nano-wire array is prepared using low-melting-point metal as bridging agent | |
| CN103966667B (en) | A kind of preparation method of three-dimensional ordered macroporous germanium/carbon composite | |
| CN105603469A (en) | CuO/Ni core-shell nanowire and preparation method thereof | |
| CN106711419A (en) | Core-shell NiO/C porous composite lithium ion battery negative electrode material | |
| Belov et al. | Pulsed electrodeposition of metals into porous anodic alumina | |
| CN108199003A (en) | A kind of big/mesoporous antimony cathode of three-dimensional, preparation method and applications | |
| CN104785871B (en) | A kind of preparation method of probe and preparation facilitiess | |
| CN101298682A (en) | Method for preparing platinum nano-perforated electrode by evaporation deposition | |
| CN104787720B (en) | A kind of preparation method of nano-wire array based on Graphene | |
| CN106207147A (en) | A kind of two-dimensional nano-film lithium ion battery negative material and preparation method thereof | |
| CN107130219B (en) | A kind of preparation method of ultra-thin through-hole anodic aluminum oxide film | |
| CN106602001B (en) | A kind of preparation method and application of the porous negative electrode material of lithium ion battery | |
| KR101548704B1 (en) | Silicon nanowire array, anode of lithium ion battery and fabricating method for the same | |
| CN105755528A (en) | Method for controlling corrosion depth of porous silicon | |
| CN113466271B (en) | Method for accurately determining type, morphology and elemental composition of intermetallic compounds in steel | |
| CN109301200A (en) | AZO modified 3 D copper/lithium an- ode material preparation method | |
| CN108866582A (en) | A kind of technique of electrodeposition process preparation roughening nickel foil | |
| CN108588810A (en) | A kind of preparation process of porous tantalum piece | |
| CN108950500A (en) | A kind of preparation method of the nano-pore structure gold electrode based on magnetron sputtering | |
| CN108069389B (en) | Preparation method of magnetic control directional fast moving micro-nano robot |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |