CN108842135A - The preparation method of dendroid silver nano line array - Google Patents

The preparation method of dendroid silver nano line array Download PDF

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Publication number
CN108842135A
CN108842135A CN201810619095.3A CN201810619095A CN108842135A CN 108842135 A CN108842135 A CN 108842135A CN 201810619095 A CN201810619095 A CN 201810619095A CN 108842135 A CN108842135 A CN 108842135A
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line array
substrate
nano line
silver nano
film
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徐大鹏
康维刚
杨巍
陈建
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Xian Technological University
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Xian Technological University
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • 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
    • 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
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0694—Halides

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to a kind of preparation methods of dendroid silver nano line array, deposit silver ion KAg in glass basic surface using vacuum thermal evaporation method4I5Conductive film, in substrate one end, deposited metal Ag film is as anode, substrate other end deposited metal Al film as cathode, electrode spacing 5cm, then deposit silver ion KAg in substrate surface4I5Conductive film makes it cover full wafer substrate, and anode and cathode is connect with the anode and cathode of constant pressure source table respectively, the dendritic silver nano line array of Propagating Tree is used for after energization.This method is carried out in solid-state environment, and any template is not necessarily to, and being obtained with pattern only by applying direct current electric field is dendritic silver nano line array.Dendroid silver nano line array marshalling prepared by the present invention, direction is very regular, easily peels off from the substrate, and can be used as device and directly applies to photoelectric device, or is applied in the fields such as biological detection directly as surface enhanced Raman scattering substrate.

Description

The preparation method of dendroid silver nano line array
Technical field
The invention belongs to metal nano material preparation technical fields, and in particular to a kind of system of dendroid silver nano line array Preparation Method.
Background technique
Metal Nano structure shows special mechanics, optics, calorifics, the electricity that supplement is even higher than corresponding body material because of it The performances such as, magnetics, sterilizing and catalysis and the new hot spot for being increasingly becoming nanostructure research.In numerous metal materials, The activity of silver is low, chemical property is stable, electric conductivity and thermal conductivity are fine, while one-dimensional silver nanowires has high conductance The excellent properties such as rate, thermal conductivity and surface enhanced Raman scattering effect and widely studied.
Preparation method about silver nano line array has much at present, including template, pulling film forming method, mechanical means. It is wherein determined respectively by the aperture of template and thickness with the diameter and length of the silver nano line array of template preparation, mechanical means The depth of parallelism of nanowire alignment in the silver nano line array of preparation is not high；And the above method carries out in liquid environment, it is real It is more complicated to test process, is difficult to control；The length of nano wire is only capable of reaching micron dimension in array.
Patent No. 200510012005.7, it is entitled " preparation method of the silver monocrystal nano line array of cm-level length " Patent of invention in the preparation method of silver monocrystal nano line is illustrated.RbAg of the technology due to use4I5Silver ion is led Conductive film is under ambiance effect（Temperature, humidity, sunlight etc.）It is easier to decompose, directly affects the quality and shape of nano wire Looks；Simultaneously because the Silver Electrode spacing that the technology uses is set as 1 millimeter, lesser electrode spacing limits silver ion and exists RbAg4I5Effective transmission in thin film channel, so being unfavorable for preparing dendroid silver nano line array.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of dendroid silver nano line array, to overcome the prior art to exist The problem of.
The technical scheme adopted by the invention is as follows：
The preparation method of dendroid silver nano line array, it is characterised in that：
Include the following steps：
（1）Silver ion KAg is deposited in glass basic surface using vacuum thermal evaporation method4I5Conductive film；
（2）In substrate one end, deposited metal Ag film is as anode, substrate other end deposited metal Al film as cathode, electrode Spacing is 5cm；
（3）Silver ion KAg is deposited in substrate surface again4I5Conductive film makes it cover full wafer substrate；
（4）Anode and cathode is connect with the anode and cathode of constant pressure source table respectively, the dendritic silver nanoparticle of Propagating Tree is used for after energization Linear array, current strength are 3~5 μ A, time 24-44h.
Step（1）In, silver ion conductive film KAg4I5Material is the AgI and content >=99.0% by content >=99.5% KI presses 4:1 molar ratio configuration grinding 5h, which is uniformly mixed, to be made.
Step（2）In, the thickness of electrode of metal Ag film and Al metal membrane is 1 μm.
The present invention has the following advantages that：
1, the anodic-cathodic that the present invention uses is respectively aluminium film and silverskin, and spacing is 5cm.Because biggish electrode spacing helps In metal silver ion in KAg4I5Effective transmission in conductor thin film channel can be more preferable when this external application silverskin-aluminium film is as electrode Offer silver ion applying direct current electric field effect under continuously pass through KAg4I5Conductor thin film is to cathode transport, Jin Eryou Conducive to the preparation of dendroid silver nano line array.
2, raw materials used difference, silver ion conductive film of the present invention are KAg4I5Material.Because in identical ring Border atmosphere（Temperature, sunlight, humidity etc.）Under effect, KAg4I5Compare RbAg4I5Stablize, and cheap.
3, in prepared dendroid silver nano line array, the length of nano wire has reached 5cm, and wire diameter distribution Range is between dozens to a few hundred nanometers；Nanowire surface in array is dispersed with more silver nano-grain, nano particle In the presence of increasing the surface roughness of dendroid silver nano line array, therefore the dendroid silver nano line array has high surface Roughness.
Detailed description of the invention
Fig. 1 is the process flow chart of experimental provision of the invention；
Fig. 2 is the photomacrograph of dendroid silver nano line array prepared by embodiment 1；
Fig. 3 be impressed current intensity be 3 μ A when, a, b, c, d are the dendroid silver nano line array of different amplification respectively SEM figure；
Fig. 4 is the photomacrograph of dendroid silver nano line array prepared by embodiment 2；
Fig. 5 be impressed current intensity be 5 μ A when, a, b, c, d are the dendroid silver nano line array of different amplification respectively SEM figure；
Fig. 6 is the EDS spectrogram of dendroid silver nano line array.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
The present invention relates to a kind of preparation methods of dendroid silver nano line array, include the following steps：
（1）Silver ion KAg is deposited in glass basic surface using vacuum thermal evaporation method4I5Conductive film；
（2）In substrate one end, deposited metal Ag film is as anode, substrate other end deposited metal Al film as cathode, electrode Spacing is 5cm；
（3）Silver ion KAg is deposited in substrate surface again4I5Conductive film makes it cover full wafer substrate；
（4）Anode and cathode is connect with the anode and cathode of constant pressure source table respectively, the dendritic silver nanoparticle of Propagating Tree is used for after energization Linear array, current strength are 3~5 μ A, time 24-44h.
Step（1）In, silver ion conductive film KAg4I5Material is the AgI and content >=99.0% by content >=99.5% KI presses 4:1 molar ratio configuration grinding 5h, which is uniformly mixed, to be made.
Step（2）In, the thickness of electrode of metal Ag film and Al metal membrane is 1 μm.
Referring to Fig. 1, the preparation method of dendroid silver nano line array provided by the invention：Choosing specification is 10 × 5cm's Cleaning quartz glass is substrate（Fig. 1 (a)）, using vacuum thermal evaporation method glass basic surface deposition thickness about 500nm's Silver ion KAg4I5Conductive film（Fig. 1 (b)）；The metal Ag membrane electrode that difference deposition width is 4cm at substrate both ends（Fig. 1 (c)） The Al metal membrane electrode for being 1cm with width（Fig. 1 (d)）；Then in the silver ion of full wafer substrate surface deposition thickness 500nm or so KAg4I5Conductive film（Fig. 1 (e)）；Finally under applying direct current electric field effect, Ag membrane electrode surface and silver ion KAg4I5It is conductive The silver atoms that film is in contact lose electronics first and are transformed into silver ion, which is passed by conductive film to Al membrane electrode It is defeated, and electronics by the conducting wire of external circuit to movable cathode.Silver ion is reduced simultaneously after the edge of Al membrane electrode obtains electronics Accumulation and crystallization become dendroid silver nano line array（Fig. 1 (f)）.
Embodiment 1：
A kind of preparation method of dendroid silver nano line array, includes the following steps：
（1）Silver ion KAg is deposited in glass basic surface using vacuum thermal evaporation method4I5Conductive film, the silver ion Conductive film KAg4I5Material is the AgI by content >=99.5%（It analyzes pure）With the KI of content >=99.0%（It analyzes pure）By 4:1 Molar ratio configuration grinding 5h, which is uniformly mixed, to be made；
（2）In substrate one end, deposited metal Ag film is as anode, substrate other end deposited metal Al film as cathode, electrode Spacing is 5cm, and the thickness of electrode of the metal Ag film and Al metal membrane is 1 μm；
（3）Silver ion KAg is deposited in substrate surface again4I5Conductive film makes it cover full wafer substrate；
（4）Ag film anode and Al film cathode are connect with the anode and cathode of constant pressure source table respectively, for growing branch after energization Shape silver nano line array, wherein taking impressed current intensity is 3 μ A, the time is dendroid silver nano line array length obtained for 24 hours For 5cm, and organize sparse（Referring to fig. 2）.
Referring to Fig. 3, it can be seen that in array the diameter distribution of nano wire be 50-150nm, and nanowire surface have compared with More silver nano-grains generates, and the presence of nano particle increases the surface roughness of dendroid silver nano line array, therefore should Dendroid silver nano line array has the roughness on high surface.
Embodiment 2：
Difference from example 1 is that the（4）Step：By Ag film anode and Al film cathode respectively with constant pressure source table anode and Cathode connection, is used for the dendritic silver nano line array of Propagating Tree after energization, wherein take impressed current intensity for 5 μ A, time 40h, Dendroid silver nano line array length obtained is 5cm, and nanowire alignment is neat in array, and direction is very regular, and is organized close Collection（Referring to fig. 4）.
Referring to Fig. 5, it can be seen that the diameter distribution of nano wire is 90-250nm in array, and nanowire surface is equal Even is dispersed with silver nano-grain, and the presence of nano particle increases the surface roughness of dendroid silver nano line array, therefore The dendroid silver nano line array has the roughness on high surface.
Referring to Fig. 6, in conjunction with table 1, it can be seen that dendroid silver nano line array scanning electron microscope energy dispersion The analysis of spectrogram-EDS is as a result, should be statistics indicate that contain only Ag element in nano-wire array.
The contents of the present invention are not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention And to any equivalent transformation that technical solution of the present invention is taken, all are covered by the claims of the invention.

Claims (3)

1. the preparation method of dendroid silver nano line array, it is characterised in that：
Include the following steps：
（1）Silver ion KAg is deposited in glass basic surface using vacuum thermal evaporation method4I5Conductive film；
（2）In substrate one end, deposited metal Ag film is as anode, substrate other end deposited metal Al film as cathode, electrode Spacing is 5cm；
（3）Silver ion KAg is deposited in substrate surface again4I5Conductive film makes it cover full wafer substrate；
（4）Anode and cathode is connect with the anode and cathode of constant pressure source table respectively, the dendritic silver nanoparticle of Propagating Tree is used for after energization Linear array, current strength are 3~5 μ A, time 24-44h.
2. the preparation method of dendroid silver nano line array according to claim 1, it is characterised in that：
Step（1）In, silver ion conductive film KAg4I5Material be by content >=99.5% AgI and content >=99.0% KI by 4:1 molar ratio configuration grinding 5h, which is uniformly mixed, to be made.
3. the preparation method of dendroid silver nano line array according to claim 1, it is characterised in that：
Step（2）In, the thickness of electrode of metal Ag film and Al metal membrane is 1 μm.
CN201810619095.3A 2018-06-15 2018-06-15 The preparation method of dendroid silver nano line array Pending CN108842135A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5311890A (en) * 1976-07-20 1978-02-02 Sanyo Electric Co Ltd Electrochromic display device
CN1522952A (en) * 2003-02-21 2004-08-25 清华大学 Method and apparatus for preparing metal nanostructured material in all-solid-state environment
CN1709790A (en) * 2005-06-24 2005-12-21 清华大学 Method for preparing monocrystal silver nano line array with square cm order area
CN101468877A (en) * 2007-12-28 2009-07-01 西北工业大学 Infrared light transmission sandwich structure composite material based on silver dendritic structure

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5311890A (en) * 1976-07-20 1978-02-02 Sanyo Electric Co Ltd Electrochromic display device
CN1522952A (en) * 2003-02-21 2004-08-25 清华大学 Method and apparatus for preparing metal nanostructured material in all-solid-state environment
CN1709790A (en) * 2005-06-24 2005-12-21 清华大学 Method for preparing monocrystal silver nano line array with square cm order area
CN101468877A (en) * 2007-12-28 2009-07-01 西北工业大学 Infrared light transmission sandwich structure composite material based on silver dendritic structure

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
DAPENG XU.ET.AL: "Fabrication and surface enhanced Raman scattering effect of centimeter level AgCuAu composite nanowires", 《OPTICAL MATERIALS》 *
徐大鹏等: "纳米表面增强拉曼散射基底的研究进展", 《西安工业大学学报》 *
徐海涛: "KI-AgI三元化合物和有序介孔氧化硅SBA-15的制备及物性研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

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