CN106757249B - A kind of cathode surface nanosecond pulsed electric field prepares the solution and preparation method of nano thin-film - Google Patents

A kind of cathode surface nanosecond pulsed electric field prepares the solution and preparation method of nano thin-film Download PDF

Info

Publication number
CN106757249B
CN106757249B CN201611157739.9A CN201611157739A CN106757249B CN 106757249 B CN106757249 B CN 106757249B CN 201611157739 A CN201611157739 A CN 201611157739A CN 106757249 B CN106757249 B CN 106757249B
Authority
CN
China
Prior art keywords
film
nano thin
solution
electric field
parts
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.)
Expired - Fee Related
Application number
CN201611157739.9A
Other languages
Chinese (zh)
Other versions
CN106757249A (en
Inventor
蒋永锋
包晔峰
陈秉岩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou Campus of Hohai University
Original Assignee
Changzhou Campus of Hohai University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Changzhou Campus of Hohai University filed Critical Changzhou Campus of Hohai University
Priority to CN201611157739.9A priority Critical patent/CN106757249B/en
Publication of CN106757249A publication Critical patent/CN106757249A/en
Application granted granted Critical
Publication of CN106757249B publication Critical patent/CN106757249B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00Electrolytic coating other than with metals
    • C25D9/04Electrolytic coating other than with metals with inorganic materials
    • C25D9/08Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/18Electroplating using modulated, pulsed or reversing current
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00Electrolytic coating other than with metals
    • C25D9/04Electrolytic coating other than with metals with inorganic materials
    • C25D9/08Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • C25D9/10Electrolytic coating other than with metals with inorganic materials by cathodic processes on iron or steel

Abstract

The invention discloses the solution that a kind of cathode surface nanosecond pulsed electric field prepares nano thin-film, the parts by weight including following components and each component are as follows: 40~50 parts of acetate, 20~40 parts of organic acid, 10~15 parts of carbonate, surplus is water.The invention also discloses a kind of methods that cathode surface nanosecond pulsed electric field prepares nano thin-film, the following steps are included: metalwork is put into the solution of above-mentioned preparation, using metalwork as cathode, graphite is anode, apply nanosecond pulse voltage, i.e. in metalwork merging solution, metal surface can prepare uniform nano thin-film.Nano thin-film prepared by the present invention, because solution is room temperature, processing speed is fast, and the time is short, and uniformity greatly improves.

Description

A kind of cathode surface nanosecond pulsed electric field prepares the solution and preparation method of nano thin-film
Technical field
The present invention relates to solution and preparation method that a kind of cathode surface nanosecond pulsed electric field prepares nano thin-film, belong to table Surface treatment technical field.
Background technique
The nano thin-film of material surface has the performance of functional material.Common nano thin-film preparation method includes that colloidal sol is solidifying Glue method, pulse current method, cyclic voltammetry etc..The nano thin-film uniformity of sol-gal process preparation is influenced by number, and arteries and veins Rushing electric current and preparing nano thin-film is influenced by the uniformity of electric field, and cyclic voltammetry prepares film by electrode surface uniformity It influences.(Xue Jinbo, Shen Qianqian, Yang Huijuan, Shao Mingzhe, Hu Wenyue, Jia Husheng, Xu Bingshe, a kind of cuprous oxide are received so document The fast preparation method of rice film, CN201610051812.8 and Wang Yabin, Liu Zhong, Dong Yaping, Li Wu, one kind is in copper or copper The method that alloy surface prepares nano thin-film, CN201510310012.9) a kind of method for manufacturing thin film, but film are described respectively Uniformity is low, and function is easy to cause to reduce, and preparation efficiency is low.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of existing technologies, a kind of cathode surface nanosecond pulse is provided Electric field prepares the solution and preparation method of nano thin-film, and the present invention can improve the uniformity of nano thin-film and improve nanometer Film performance and efficiency, the processing method processing speed is fast, and the time is short, and surface uniformity is good.
In order to solve the above technical problems, the present invention, which provides a kind of cathode surface nanosecond pulsed electric field, prepares the molten of nano thin-film Liquid, characterized in that the parts by weight including following components and each component are as follows: 40~50 parts of acetate, 20~40 parts of organic acid, carbon 10~15 parts of hydrochlorate, surplus is water.
Further, the acetate is copper acetate or nickel acetate.Acetate not only provide the metal of nano thin-film from Son, and the thin film strength of reinforced nano and hardness, improve the mechanical property of film.
Further, the organic acid is lactic acid or acrylic acid.Organic acid is the matrix and skeleton to form nano thin-film, Simultaneously and matrix surface recombination reaction, raising adhesive force.
Further, the carbonate is sodium carbonate or potassium carbonate.Suitable electrochemistry is provided for nanosecond pulsed electric field The acid-base property of condition and solution.
Further, the water is distilled water or deionized water.
The present invention also provides a kind of methods that cathode surface nanosecond pulsed electric field prepares nano thin-film, characterized in that packet It includes following steps: metalwork being put into the solution of above-mentioned preparation, using metalwork as cathode, graphite is anode, applies nanosecond arteries and veins Voltage is rushed, uniform nano thin-film can be prepared in metal surface.Under suitable electrochemical conditions, the offer of nanosecond electric field has The energy field of selection and coupling so that organic acid and acetate in matrix surface electrochemical reaction and thermal response, coupling occurs Matrix potential field is attached to body surface, forms nano thin-film.
Further, the nanosecond pulse voltage pulsewidth is 10~500 ns, and impulse amplitude is 800~1500V.
Further, the nanosecond pulse voltage handles 1~3min.
Advantageous effects of the invention: nano thin-film prepared by the present invention, because solution is room temperature, processing speed is fast, Time is short, and uniformity greatly improves.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram for the cupric oxide nano film that the embodiment of the present invention 1 is prepared;
Fig. 2 is the scanning electron microscope diagram for the nickel oxide nano film that the embodiment of the present invention 2 is prepared;
Fig. 3 is the scanning electron microscope diagram for the cupric oxide nano film that the embodiment of the present invention 3 is prepared.
Specific embodiment
The invention will be further described below in conjunction with the accompanying drawings.Following embodiment is only used for clearly illustrating the present invention Technical solution, and not intended to limit the protection scope of the present invention.
Embodiment 1
2/3 distilled water is taken in a slot first, 4000g copper acetate and 3500g lactic acid is successively dissolved, waits reagent in slots All after dissolution, 1500g sodium carbonate is poured into tank liquor under fast stirring, until being mixed thoroughly, is finally added water to 10L obtains electrolyte, and copper is put into the solution of preparation, and using copper as cathode, graphite is anode, in 50 ns of pulsewidth, voltage amplitude 800 V of value handles 1 minute, that is, prepares cupric oxide nano film (see figure 1).Nano thin-film is uniform, and adhesive force is high, has and urges Change performance and corrosion resisting property.
Embodiment 2
The deionized water for taking 2/3 in a slot first, the 5000g nickel acetate and 3000g acrylic acid successively dissolved, waits slots All after dissolution, 1000g potassium carbonate is poured into tank liquor under fast stirring for middle reagent, until being mixed thoroughly, finally It adds water to 10L and obtains electrolyte, 13Cr stainless steel is put into the solution of preparation, using stainless steel as cathode, graphite is anode, 500 ns of pulsewidth, 1500 V of voltage magnitude handle 1 minute, that is, prepare nickel oxide nano film (see figure 2).Nano thin-film is equal Even, microscopic particles are tiny, and adhesive force is high, have catalytic performance and corrosion resisting property.
Embodiment 3
2/3 distilled water is taken in a slot first, 5000g copper acetate and 3500g lactic acid is successively dissolved, waits reagent in slots All after dissolution, 1000g sodium carbonate is poured into tank liquor under fast stirring, until being mixed thoroughly, is finally added water to 10L obtains electrolyte, and pure titanium is put into the solution of preparation, and using pure titanium as cathode, graphite is anode, in 20 ns of pulsewidth, voltage 1200 V of amplitude handles 3 minutes, that is, prepares cupric oxide nano film (see figure 3).Nano thin-film is uniform, and adhesive force is high, has Catalytic performance and corrosion resisting property.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations Also it should be regarded as protection scope of the present invention.

Claims (3)

1. a kind of method that cathode surface nanosecond pulsed electric field prepares nano thin-film, characterized in that the following steps are included: by metal Part is put into the solution of preparation, and the solution includes the parts by weight of following components and each component are as follows: 40~50 parts of acetate, is had 20~40 parts of machine acid, 10~15 parts of carbonate, surplus is water, and the acetate is copper acetate or nickel acetate, and described is organic Acid is lactic acid or acrylic acid, and the carbonate is sodium carbonate or potassium carbonate, and the water is distilled water or deionized water, with gold Category part is cathode, and graphite is anode, applies nanosecond pulse voltage, can prepare uniform nano thin-film in metal surface.
2. the method that a kind of cathode surface nanosecond pulsed electric field according to claim 1 prepares nano thin-film, characterized in that The nanosecond pulse voltage pulsewidth is 10~500 ns, and impulse amplitude is 800~1500V.
3. the method that a kind of cathode surface nanosecond pulsed electric field according to claim 1 prepares nano thin-film, characterized in that The nanosecond pulse voltage handles 1~3min.
CN201611157739.9A 2016-12-15 2016-12-15 A kind of cathode surface nanosecond pulsed electric field prepares the solution and preparation method of nano thin-film Expired - Fee Related CN106757249B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611157739.9A CN106757249B (en) 2016-12-15 2016-12-15 A kind of cathode surface nanosecond pulsed electric field prepares the solution and preparation method of nano thin-film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611157739.9A CN106757249B (en) 2016-12-15 2016-12-15 A kind of cathode surface nanosecond pulsed electric field prepares the solution and preparation method of nano thin-film

Publications (2)

Publication Number Publication Date
CN106757249A CN106757249A (en) 2017-05-31
CN106757249B true CN106757249B (en) 2019-01-15

Family

ID=58888394

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611157739.9A Expired - Fee Related CN106757249B (en) 2016-12-15 2016-12-15 A kind of cathode surface nanosecond pulsed electric field prepares the solution and preparation method of nano thin-film

Country Status (1)

Country Link
CN (1) CN106757249B (en)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1005619A (en) * 1962-06-29 1965-09-22 Ibm Improvements in and relating to the deposition of copper on non-conductive surfaces
JP2005163091A (en) * 2003-12-01 2005-06-23 Osaka City Composition for copper oxide electrolytic formation, and method of forming copper oxide film and copper oxide film using the same
WO2006136335A1 (en) * 2005-06-22 2006-12-28 Henkel Kommanditgesellschaft Auf Aktien PROCESS FOR PROVIDING A CORROSION-PROTECTIVE LAYER OF TiO2 ON AN ELECTRICALLY CONDUCTIVE SUBSTRATE AND METAL SUBSTRATE COATED WITH A LAYER OF TiO2
CN101717980A (en) * 2009-12-15 2010-06-02 天津大学 Method for preparing cuprous oxide/titanium dioxide core-shell structure array film through AC electro-deposition method
CN103225097A (en) * 2013-05-15 2013-07-31 南京航空航天大学 Preparation of Cu2O/TNTs (TiO2 nanotubes) heterojunction nano composite material and CO2 photoreduction method
CN103603018A (en) * 2013-10-23 2014-02-26 复旦大学 Pulse electroplating method and application thereof
CN103882494A (en) * 2014-03-12 2014-06-25 浙江大学 Preparation method of Cu2O/ZnO heterojunction material
CN104372394A (en) * 2014-07-03 2015-02-25 西安工业大学 Preparation method for oxide ceramic layer

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1893791A2 (en) * 2005-06-22 2008-03-05 Henkel Kommanditgesellschaft Auf Aktien ELECTRODEPOSITION MATERIAL, PROCESS FOR PROVIDING A CORROSION-PROTECTIVE LAYER OF TiO2 ON AN ELECTRICALLY CONDUCTIVE SUBSTRATE AND METAL SUBSTRATE COATED WITH A LAYER OF TiO2

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1005619A (en) * 1962-06-29 1965-09-22 Ibm Improvements in and relating to the deposition of copper on non-conductive surfaces
JP2005163091A (en) * 2003-12-01 2005-06-23 Osaka City Composition for copper oxide electrolytic formation, and method of forming copper oxide film and copper oxide film using the same
WO2006136335A1 (en) * 2005-06-22 2006-12-28 Henkel Kommanditgesellschaft Auf Aktien PROCESS FOR PROVIDING A CORROSION-PROTECTIVE LAYER OF TiO2 ON AN ELECTRICALLY CONDUCTIVE SUBSTRATE AND METAL SUBSTRATE COATED WITH A LAYER OF TiO2
CN101717980A (en) * 2009-12-15 2010-06-02 天津大学 Method for preparing cuprous oxide/titanium dioxide core-shell structure array film through AC electro-deposition method
CN103225097A (en) * 2013-05-15 2013-07-31 南京航空航天大学 Preparation of Cu2O/TNTs (TiO2 nanotubes) heterojunction nano composite material and CO2 photoreduction method
CN103603018A (en) * 2013-10-23 2014-02-26 复旦大学 Pulse electroplating method and application thereof
CN103882494A (en) * 2014-03-12 2014-06-25 浙江大学 Preparation method of Cu2O/ZnO heterojunction material
CN104372394A (en) * 2014-07-03 2015-02-25 西安工业大学 Preparation method for oxide ceramic layer

Also Published As

Publication number Publication date
CN106757249A (en) 2017-05-31

Similar Documents

Publication Publication Date Title
CN104846397B (en) One kind being used for electrochemical reduction CO2The electrode and its preparation method and application of formic acid processed
CN101276916B (en) Preparation technique for anti-corrosion fuel cell stainless dual-polar plate
CN104894595B (en) A kind of amorphous metal oxide hydrogen-precipitating electrode of high catalytic activity and preparation method thereof
CN106149026A (en) The preparation of a kind of Graphene/golden nanometer particle composite and characterizing method
CN103700813B (en) A kind of Ti base β-PbO 2the preparation method of dimensional stable anode
CN104451851A (en) Electrolytic corrosion agent capable of displaying nickel-based corrosion-resistant alloy metallographic structure and corrosion method thereof
CN103196733A (en) Etchant for displaying metallographic structure of nickel-based high temperature alloy and method
CN105603469A (en) CuO/Ni core-shell nanowire and preparation method thereof
CN103398892A (en) Method for displaying prior austenite crystal boundary of martensite heat-resistant steel
CN100503897C (en) Preparation of nano zinc powder by single groove ultrasonic electrolytic process
CN109628957A (en) A kind of preparation method of Zinc electrolysis titanium-based nano composite anode
CN104962977A (en) Preparation method of rod-shaped bimetallic-based composite anode material
CN106757249B (en) A kind of cathode surface nanosecond pulsed electric field prepares the solution and preparation method of nano thin-film
CN105200421B (en) A kind of method that laser fine fusion covering prepares hydrogen-precipitating electrode hydrogen storage layer
CN102899703A (en) Silicate electrolyte and application of silicate electrolyte in magnesium alloy micro-arc oxidation film preparation
CN101935864A (en) Anode stripping solution for magnesium and magnesium alloy nickel-plating layer and method for stripping coating
CN110255677A (en) Multicomponent is co-doped with modified ti-supported lead dioxide electric pole and preparation method thereof
CN106676619A (en) Method for preparing metal glass nano porous structure
CN108772054A (en) A kind of titanium dioxide-pucherite composite photocatalyst material and preparation method thereof
CN105206850B (en) A kind of Ti/W/Mo oxide in-situs strengthen the preparation method of platinum/palladium nanostructured composite catalyst
CN104966835A (en) Method for manufacturing AgVO<3> thin films on Ag substrates by means of electrolysis
CN106319579A (en) Method for preparing disinfection electrode material with copper sponge-based silver thin film loaded with nano particles
CN103526218B (en) A kind of titanium alloy anodic oxidation activation moves back the ageing method of the two-in-one solution of film
CN102251270B (en) Method for stripping metallic thin film plated on surface of material
CN108588789A (en) A kind of preparation method for the processing solution and boron titanium compound preparing boron titanium compound film layer

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
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20190115

Termination date: 20211215