CN108034968A - A kind of preparation method for the nano bowl noble coatings for suppressing Multipactor - Google Patents
A kind of preparation method for the nano bowl noble coatings for suppressing Multipactor Download PDFInfo
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- CN108034968A CN108034968A CN201711311539.9A CN201711311539A CN108034968A CN 108034968 A CN108034968 A CN 108034968A CN 201711311539 A CN201711311539 A CN 201711311539A CN 108034968 A CN108034968 A CN 108034968A
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- 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
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- 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
- C25D3/46—Electroplating: Baths therefor from solutions of silver
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- 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
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
- C25D5/44—Aluminium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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Abstract
A kind of preparation method for the nano bowl noble coatings for suppressing Multipactor, forms individual layer polystyrene microsphere template in silver-plated aluminum alloy surface, obtains the silver-plated aluminium alloy print with PS templates；It is then submerged in the coating bath containing precious metal salt solution, using the silver-plated aluminium alloy print with PS templates as cathode, graphite is anode, and side of the silver-plated aluminium alloy print with PS templates is opposite with graphite electrode, electric current is passed through between a cathode and an anode, make noble metal loading on silver-plated aluminium alloy print, rinse, dry after remove PS templates, formed suppress Multipactor nano bowl noble coatings.The present invention prepares noble metal nano bowl array structure using colloidal crystal template method, and preparation method is simple, and cost is low, and without special installation, repeatability is strong, can effectively reduce the secondary electron yield of silver coated aluminum alloy substrates.
Description
Technical field
The present invention relates to a kind of preparation method of nano bowl noble coatings, and in particular to a kind of suppression Multipactor
The preparation method of nano bowl noble coatings.
Background technology
Multipactor, is a kind of vacuum resonant discharge occurred in parts surface also known as " multipactor "
Phenomenon.In recent years, with the rapid development of space technology, substantial amounts of HIGH-POWERED MICROWAVES communication equipment is put into use, in equipment
It should not be underestimated by the harm that Multipactor produces in portion.Meanwhile with the increase of Space Facilities carrier number, Multipactor
The harm produced to Space Facilities also more highlights.Therefore, the Multipactor for suppressing Space Facilities is space technology research neck
One emphasis in domain.
When suppressing Multipactor, secondary electron yield can be reduced by constructing loose structure in material surface
(SEY), the basic principle of its suppression SEY is：Secondary electron is repeatedly stopped by the hole in loose structure, has fettered it from surface
The ability of escape.
At present, the method for preparing nano-porous structure mainly has etching method and template.Etching method can be divided into chemical quarter again
Erosion and physical etchings.Mainly by etching agent with pre-embossed corrosion material chemical reaction occurs for chemical etching so as to obtain porous knot
Structure, microcellular structure is prepared for such as leaf et al. by iron nitrate solution to initial silver-plated aluminium alloy progress chemical etching.It is although chemical
Etching method can be effectively reduced the SEY of parts surface, have cost it is low, without special equipment, simple operation and other advantages, but
It is that its etching is a uncontrollable process of non-directional, the size and pattern of loose structure can not be accurately controlled.Physical etchings
Mainly directly required pore space structure is etched in sample surfaces using high-power electron beam or ion beam.Using physical etchings
Reproducibility is good, and pattern is easily controllable, plays an important role in optical analysis and the preparation of bio-sensing, but this method into
This height, equipment requirement is harsh, etch period length.
The content of the invention
The object of the present invention is to provide a kind of preparation method for the nano bowl noble coatings for suppressing Multipactor.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of preparation method for the nano bowl noble coatings for suppressing Multipactor, comprises the following steps：
Step 1：The assembling of silver-plated aluminum alloy surface individual layer polystyrene microsphere
First, the sheet glass after cleaning is positioned over culture dish center, deionized water is injected into culture dish makes it just
Sheet glass is not crossed, the hanging drop that polystyrene emulsion, second alcohol and water are made into is added on sheet glass, suspension is diffused into water
Face, stops being added dropwise after complete film is formed on the water surface, and most backward surface plate injection deionized water, the film of formation is with liquid
The rise in face is picked up the film of formation from the water surface with silver-plated aluminium alloy print, i.e., in silver-plated aluminium alloy away from surface plate bottom
Surface forms individual layer polystyrene microsphere template, obtains the silver-plated aluminium alloy print with PS templates；
Step 2：Silver-plated aluminum alloy surface electrochemical deposition noble coatings
Silver-plated aluminium alloy print with PS templates prepared by step 1 is immersed in the coating bath containing precious metal salt solution
In, using the silver-plated aluminium alloy print with PS templates as cathode, graphite is anode, and silver-plated aluminium alloy print carries PS templates
Side is opposite with graphite electrode, is passed through electric current between a cathode and an anode, makes noble metal loading on silver-plated aluminium alloy print；
Step 3：The formation of silver-plated aluminum alloy surface nano bowl noble coatings
The silver-plated aluminium alloy print of depositing noble metal coating prepared by step 2 rinses, dry after using solvent impregnated or
Calcining removes PS templates, forms the nano bowl noble coatings for suppressing Multipactor.
Further improve of the invention is that polystyrene emulsion, the volume ratio of second alcohol and water are 1 in step 1:4:4~
1:15:15, and the volume ratio of second alcohol and water is 1:1.
Of the invention further improve be, in step 1 in polystyrene emulsion PS microballoons a diameter of 300nm~
1000nm；The size of silver-plated aluminium alloy print is 20 × 12 × 1mm3。
Further improve of the invention is that the distance between cathode and anode are 3~5cm in step 2.
Further improve of the invention is that precious metal salt solution is silver nitrate solution or chlorauric acid solution in step 2.
Of the invention further improve is, when precious metal salt solution be silver nitrate solution, deposition voltage is 0.2~
0.4V, sedimentation time are 10~30min.
Of the invention further improve is, when precious metal salt solution be chlorauric acid solution, sedimentation time is 0.7~
0.9V, sedimentation time are 10~60min.
Further improve of the invention is that silver nitrate solution is made by procedure below：By silver nitrate, complexing agent and
Potassium nitrate is added to the water, and uses ammonium hydroxide to adjust pH value as 8~10, obtains silver nitrate solution, wherein, the concentration of silver nitrate is
0.05~0.2mol/L, the concentration of complexing agent is 0.05~0.2mol/L, and the concentration of potassium nitrate is 0.025~0.1mol/L；Its
In, complexing agent is disodium ethylene diamine tetraacetate.
Further improve of the invention is that chlorauric acid solution is made by procedure below：By gold chloride, complexing agent, Asia
Sodium sulphate and disodium hydrogen phosphate are added to the water, and obtain chlorauric acid solution；Wherein, gold chloride concentration is 0.02~0.05mol/
L, complexing agent concentration are 0.01~0.03mol/L, and concentration of sodium sulfite is 0.5~1.5mol/L, and disodium hydrogen phosphate concentration is 0.1
~0.3mol/L；Wherein, complexing agent is disodium ethylene diamine tetraacetate.
Further improve of the invention is that solvent is dichloromethane, toluene or chloroform in step 3；The temperature of calcining is
200~400 DEG C, the time of calcining is 60min.
Compared with prior art, the invention has the advantages that：The present invention in silver-plated aluminum alloy surface by constructing
The PS colloidal crystals of arranged regular, and silver-plated aluminum alloy surface is electrochemically-deposited in as structure limitation template use using it and forms gold
Or the noble coatings such as silver, the method for then dissolving or calcining by solvent removes PS templates, so as to fulfill silver-plated aluminium alloy
The preparation of nano surface bowl noble coatings, reduces the SEY of silver-plated aluminium alloy.The nano bowl Au coatings prepared using the present invention can
The SEY of silver-plated aluminium alloy is set to be reduced to less than 1.67.The present invention prepares noble metal nano bowl array using colloidal crystal template method
Structure, preparation method is simple, and cost is low, and without special installation, repeatability is strong, can effectively reduce silver coated aluminum alloy substrates
Secondary electron yield.
Further, the Au nano bowls coating of preparation can effectively reduce the secondary of silver coated aluminum alloy substrates
Coefficient, the maximum 2.20 of relatively silver-plated aluminum alloy surface SEY, nano bowl array structure reduce by 24.09%.
Brief description of the drawings
Fig. 1 is the SEM photograph after silver-plated aluminum alloy surface self assembly PS templates.
Fig. 2 is the SEM photograph that silver-plated aluminum alloy surface constructs after nano bowl Ag coatings under 20000 times.
Fig. 3 is the SEM photograph that silver-plated aluminum alloy surface constructs after nano bowl Ag coatings under 5000 times.
Fig. 4 is the SEM photograph that silver-plated aluminum alloy surface constructs after nano bowl Au coatings under 20000 times.
Fig. 5 is the SEM photograph that silver-plated aluminum alloy surface constructs after nano bowl Au coatings under 5000 times.
Fig. 6 is the SEY characteristic curves that silver-plated aluminum alloy surface constructs nano bowl Au coating diverse locations.
Embodiment
With reference to embodiment and attached drawing, the present invention will be described in detail.
Polystyrene (PS) emulsion solid content is 10% in the present invention, and the producer of polystyrene (PS) lotion is：Shanghai brightness
Matter bio tech ltd.
The size of silver-plated aluminium alloy print is 20 × 12 × 1mm in the present invention3.The silver-plated aluminium alloy sample used in the present invention
Piece is existing.
Embodiment 1
Step 1：The assembling of silver-plated aluminum alloy surface individual layer polystyrene microsphere
First, the sheet glass of 2.5cm × 2.5cm is cleaned by ultrasonic in acetone, ethanol, deionized water successively, Ran Houfen
Yong not mass concentration 98%H2SO4：H2O2Volume ratio is 3:1 mixed liquor and H2O：NH3·H2O：H2O2Volume ratio is 3:1:1
Mixed liquor cleans, and is cleaned by ultrasonic afterwards with deionized water.
Then, it is placed onCulture dish center, into culture dish inject deionized water it was not had glass just
Piece, is slowly added to the hanging drop that polystyrene emulsion, second alcohol and water are made on sheet glass with liquid-transfering gun, suspension is diffused into
The water surface, stops being added dropwise after complete film is formed on the water surface.
Most backward surface plate is slowly injected into deionized water, the film of formation as the rise of liquid level is away from surface plate bottom,
The film of formation is picked up from the water surface with silver-plated aluminium alloy print, i.e., forms individual layer polystyrene microsphere in silver-plated aluminum alloy surface
Template, obtains the silver-plated aluminium alloy print with PS templates.The size of PS microballoons is 1000nm wherein in polystyrene emulsion, is gathered
Styrene emulsion, the volume ratio of second alcohol and water are 1:7:7.
Step 2：Silver-plated aluminum alloy surface electrochemical deposition Ag coatings
Silver-plated aluminium alloy print with PS templates prepared by step 1 is immersed in the coating bath containing silver plating liquid, with band
The silver-plated aluminium alloy print for having PS templates is cathode, and graphite is that the distance between anode, two electrodes is 4cm, and carries PS templates
Silver-plated aluminium alloy print on the side (side i.e. with PS templates) covered with PS monolayers it is opposite with graphite electrode.
Electric current is passed through between cathode and anode, makes noble metal loading on silver-plated aluminium alloy print.Wherein, deposition voltage 0.2V；It is heavy
The product time is 10min.Silver plating liquid is 20mL, and is made by procedure below：Silver nitrate, complexing agent and potassium nitrate are added to
In water, use ammonium hydroxide to adjust pH value as 10, obtain silver nitrate solution, also, the concentration of silver nitrate is 0.2mol/L, complexing agent
Concentration is 0.2mol/L, and the concentration of potassium nitrate is 0.1mol/L；Complexing agent is disodium ethylene diamine tetraacetate.
Step 3：The formation of silver-plated aluminum alloy surface nano bowl Ag coatings
Silver-plated aluminium alloy print deionized water and ethanol solution prepared by step 2 is rinsed, and is used after naturally dry
20mL dichloromethane removes PS templates, forms the nano bowl noble coatings for suppressing Multipactor.
Embodiment 2
Step 1：The assembling of silver-plated aluminum alloy surface individual layer polystyrene microsphere
First, the sheet glass of 2.5cm × 2.5cm is cleaned by ultrasonic in acetone, ethanol, deionized water successively, Ran Houfen
Yong not mass concentration 98%H2SO4：H2O2Volume ratio is 3:1 mixed liquor and H2O：NH3·H2O：H2O2Volume ratio is 3:1:1
Mixed liquor cleans, and is cleaned by ultrasonic afterwards with deionized water.
Then, it is placed onCulture dish center, into culture dish inject deionized water it was not had glass just
Piece, is slowly added to the hanging drop that polystyrene emulsion, second alcohol and water are made on sheet glass with liquid-transfering gun, suspension is diffused into
The water surface, stops being added dropwise after complete film is formed on the water surface.
Most backward surface plate is slowly injected into deionized water, the film of formation as the rise of liquid level is away from surface plate bottom,
The film of formation is picked up from the water surface with silver-plated aluminium alloy print, i.e., forms individual layer polystyrene microsphere in silver-plated aluminum alloy surface
Template, obtains the silver-plated aluminium alloy print with PS templates.The size of PS microballoons is 300nm wherein in polystyrene emulsion, is gathered
Styrene emulsion, the volume ratio of second alcohol and water are 1:15:15.
Step 2：Silver-plated aluminum alloy surface electrochemical deposition Ag coatings
By step 1 prepare the silver-plated aluminium alloy print with PS templates be immersed in the coating bath containing silver plating liquid, with containing
The silver-plated aluminium alloy print with PS templates of PS is cathode, and graphite is that the distance between anode, two electrodes is 4cm, and silver-plated
Side covered with PS monolayers on aluminium alloy is opposite with graphite electrode.Electric current is passed through between a cathode and an anode, makes your gold
Category is deposited on silver-plated aluminium alloy print.Wherein deposition voltage is 0.2V；Sedimentation time is 30min.Silver plating liquid is 20mL, and logical
Procedure below is crossed to be made：Silver nitrate, complexing agent and potassium nitrate are added to the water, uses ammonium hydroxide to adjust pH value as 8, obtains nitre
Sour silver solution, and the concentration of silver nitrate is 0.1mol/L, and the concentration of complexing agent is 0.1mol/L, and the concentration of potassium nitrate is
0.05mol/L；Complexing agent is disodium ethylene diamine tetraacetate.
Step 3：The formation of silver-plated aluminum alloy surface nano bowl Ag coatings
Silver-plated aluminium alloy print deionized water and ethanol solution prepared by step 2 is rinsed, and is used after naturally dry
400 DEG C of calcining 1h remove PS templates, form the nano bowl noble coatings for suppressing Multipactor.
Embodiment 3
Step 1：The assembling of silver-plated aluminum alloy surface individual layer polystyrene microsphere
First, the sheet glass of 2.5cm × 2.5cm is cleaned by ultrasonic in acetone, ethanol, deionized water successively, Ran Houfen
Yong not mass concentration 98%H2SO4：H2O2Volume ratio is 3:1 mixed liquor and H2O：NH3·H2O：H2O2Volume ratio is 3:1:1
Mixed liquor cleans, and is cleaned by ultrasonic afterwards with deionized water.
Then, it is placed onCulture dish center, into culture dish inject deionized water it was not had glass just
Piece, is slowly added to the hanging drop that polystyrene emulsion, second alcohol and water are made on sheet glass with liquid-transfering gun, suspension is diffused into
The water surface, stops being added dropwise after complete film is formed on the water surface.
Most backward surface plate is slowly injected into deionized water, the film of formation as the rise of liquid level is away from surface plate bottom,
The film of formation is picked up from the water surface with silver-plated aluminium alloy print, i.e., forms individual layer polystyrene microsphere in silver-plated aluminum alloy surface
Template, obtains the silver-plated aluminium alloy print with PS templates.The size of PS microballoons is 500nm wherein in polystyrene emulsion, is gathered
Styrene emulsion, the volume ratio of second alcohol and water are 1:15:15.
Step 2：Silver-plated aluminum alloy surface electrochemical deposition Ag coatings
By step 1 prepare the silver-plated aluminium alloy print with PS templates be immersed in the coating bath containing silver plating liquid, with containing
The silver-plated aluminium alloy print with PS templates of PS is cathode, and graphite is that the distance between anode, two electrodes is 4cm, and silver-plated
Side covered with PS monolayers on aluminium alloy is opposite with graphite electrode.Electric current is passed through between a cathode and an anode, makes your gold
Category is deposited on silver-plated aluminium alloy print.Wherein deposition voltage is 0.4V；Sedimentation time is 10min.Silver plating liquid is 20mL, and logical
Procedure below is crossed to be made：Silver nitrate, complexing agent and potassium nitrate are added to the water, uses ammonium hydroxide to adjust pH value as 8, obtains nitre
Sour silver solution, also, the concentration of silver nitrate is 0.05mol/L, the concentration of complexing agent is 0.05mol/L, and the concentration of potassium nitrate is
0.025mol/L；Complexing agent is disodium ethylene diamine tetraacetate.
Step 3：The formation of silver-plated aluminum alloy surface nano bowl Ag coatings
Silver-plated aluminium alloy print deionized water and ethanol solution prepared by step 2 is rinsed, and is used after naturally dry
200 DEG C of calcining 1h remove PS templates, form the nano bowl noble coatings for suppressing Multipactor.
Embodiment 4
Step 1：The assembling of silver-plated aluminum alloy surface individual layer polystyrene microsphere
First, the sheet glass of 2.5cm × 2.5cm is cleaned by ultrasonic in acetone, ethanol, deionized water successively, Ran Houfen
Yong not mass concentration 98%H2SO4：H2O2Volume ratio is 3:1 mixed liquor and H2O：NH3·H2O：H2O2Volume ratio is 3:1:1
Mixed liquor cleans, and is cleaned by ultrasonic afterwards with deionized water.
Then, it is placed onCulture dish center, into culture dish inject deionized water it was not had glass just
Piece, is slowly added to the hanging drop that polystyrene emulsion, second alcohol and water are made on sheet glass with liquid-transfering gun, suspension is diffused into
The water surface, stops being added dropwise after complete film is formed on the water surface.
Most backward surface plate is slowly injected into deionized water, the film of formation as the rise of liquid level is away from surface plate bottom,
The film of formation is picked up from the water surface with silver-plated aluminium alloy print, i.e., forms individual layer polystyrene microsphere in silver-plated aluminum alloy surface
Template, obtains the silver-plated aluminium alloy print with PS templates.The size of PS microballoons is 800nm wherein in polystyrene emulsion, is gathered
Styrene emulsion, the volume ratio of second alcohol and water are 1:10:10.
Step 2：Silver-plated aluminum alloy surface electrochemical deposition Au coatings
By step 1 prepare the silver-plated aluminium alloy print with PS templates be immersed in the coating bath containing gold plating liquid, with containing
The silver-plated aluminium alloy print with PS templates of PS is cathode, and graphite is that the distance between anode, two electrodes is 5cm, and silver-plated
Side covered with PS monolayers on aluminium alloy is opposite with graphite electrode.Electric current is passed through between a cathode and an anode, makes your gold
Category is deposited on silver-plated aluminium alloy print.Wherein deposition voltage is 0.9V；Sedimentation time is 10min.Gold plating liquid is 20mL, and logical
Procedure below is crossed to be made：Gold chloride, complexing agent, sodium sulfite and disodium hydrogen phosphate are added to the water, it is molten to obtain gold chloride
Liquid；And gold chloride concentration is 0.02mol/L, complexing agent concentration 0.01mol/L, concentration of sodium sulfite 0.5mol/L, phosphorus
Sour disodium hydrogen concentration is 0.1mol/L；Complexing agent is disodium ethylene diamine tetraacetate.
Step 3：The formation of the silver-plated expensive Au of aluminum alloy surface nano bowl
Silver-plated aluminium alloy print deionized water and ethanol solution prepared by step 2 is rinsed, and is used after naturally dry
20mL toluene removal PS templates, form the nano bowl noble coatings for suppressing Multipactor.
Embodiment 5
Step 1：The assembling of silver-plated aluminum alloy surface individual layer polystyrene microsphere
First, the sheet glass of 2.5cm × 2.5cm is cleaned by ultrasonic in acetone, ethanol, deionized water successively, Ran Houfen
Yong not mass concentration 98%H2SO4：H2O2Volume ratio is 3:1 mixed liquor and H2O：NH3·H2O：H2O2Volume ratio is 3:1:1
Mixed liquor cleans, and is cleaned by ultrasonic afterwards with deionized water.
Then, it is placed onCulture dish center, into culture dish inject deionized water it was not had glass just
Piece, is slowly added to the hanging drop that polystyrene emulsion, second alcohol and water are made on sheet glass with liquid-transfering gun, suspension is diffused into
The water surface, stops being added dropwise after complete film is formed on the water surface.
Most backward surface plate is slowly injected into deionized water, the film of formation as the rise of liquid level is away from surface plate bottom,
The film of formation is picked up from the water surface with silver-plated aluminium alloy print, i.e., forms individual layer polystyrene microsphere in silver-plated aluminum alloy surface
Template, obtains the silver-plated aluminium alloy print with PS templates.The size of PS microballoons is 1000nm wherein in polystyrene emulsion, is gathered
Styrene emulsion, the volume ratio of second alcohol and water are 1:10:10.
Step 2：Silver-plated aluminum alloy surface electrochemical deposition Au coatings
By step 1 prepare the silver-plated aluminium alloy print with PS templates be immersed in the coating bath containing gold plating liquid, with containing
The silver-plated aluminium alloy print with PS templates of PS is cathode, and graphite is that the distance between anode, two electrodes is 4cm, and silver-plated
Side covered with PS monolayers on aluminium alloy is opposite with graphite electrode.Electric current is passed through between a cathode and an anode, makes your gold
Category is deposited on silver-plated aluminium alloy print.Wherein deposition voltage is 0.7V；Sedimentation time is 60min.Gold plating liquid is 20mL, and logical
Procedure below is crossed to be made：Gold chloride, complexing agent, sodium sulfite and disodium hydrogen phosphate are added to the water, it is molten to obtain gold chloride
Liquid；And gold chloride concentration is 0.05mol/L, complexing agent concentration 0.03mol/L, concentration of sodium sulfite 1.5mol/L, phosphorus
Sour disodium hydrogen concentration is 0.3mol/L；Complexing agent is disodium ethylene diamine tetraacetate.
Step 3：The formation of silver-plated aluminum alloy surface nano bowl Au coatings
Silver-plated aluminium alloy print deionized water and ethanol solution prepared by step 2 is rinsed, and is used after naturally dry
200 DEG C of calcining 1h remove PS templates, form the nano bowl noble coatings for suppressing Multipactor.
Embodiment 6
Step 1：The assembling of silver-plated aluminum alloy surface individual layer polystyrene microsphere
First, the sheet glass of 2.5cm × 2.5cm is cleaned by ultrasonic in acetone, ethanol, deionized water successively, Ran Houfen
Yong not mass concentration 98%H2SO4：H2O2Volume ratio is 3:1 mixed liquor and H2O：NH3·H2O：H2O2Volume ratio is 3:1:1
Mixed liquor cleans, and is cleaned by ultrasonic afterwards with deionized water.
Then, it is placed onCulture dish center, into culture dish inject deionized water it was not had glass just
Piece, is slowly added to the hanging drop that polystyrene emulsion, second alcohol and water are made on sheet glass with liquid-transfering gun, suspension is diffused into
The water surface, stops being added dropwise after complete film is formed on the water surface.
Most backward surface plate is slowly injected into deionized water, the film of formation as the rise of liquid level is away from surface plate bottom,
The film of formation is picked up from the water surface with silver-plated aluminium alloy print, i.e., forms individual layer polystyrene microsphere in silver-plated aluminum alloy surface
Template, obtains the silver-plated aluminium alloy print with PS templates.The size of PS microballoons is 1000nm wherein in polystyrene emulsion, is gathered
Styrene emulsion, the volume ratio of second alcohol and water are 1：4：4.
Step 2：Silver-plated aluminum alloy surface electrochemical deposition Au coatings
By step 1 prepare the silver-plated aluminium alloy print with PS templates be immersed in the coating bath containing gold plating liquid, with containing
The silver-plated aluminium alloy print with PS templates of PS is cathode, and graphite is that the distance between anode, two electrodes is 3cm, and silver-plated
Side covered with PS monolayers on aluminium alloy is opposite with graphite electrode.Electric current is passed through between a cathode and an anode, makes your gold
Category is deposited on silver-plated aluminium alloy print.Wherein deposition voltage is 0.9V；Sedimentation time is 10min.Gold plating liquid is 20mL, and logical
Procedure below is crossed to be made：Gold chloride, complexing agent, sodium sulfite and disodium hydrogen phosphate are added to the water, it is molten to obtain gold chloride
Liquid；And gold chloride concentration is 0.03mol/L, complexing agent concentration 0.02mol/L, concentration of sodium sulfite 0.75mol/L, phosphorus
Sour disodium hydrogen concentration is 0.2mol/L；Complexing agent is disodium ethylene diamine tetraacetate.
Step 3：The formation of the silver-plated expensive Au of aluminum alloy surface nano bowl
Silver-plated aluminium alloy print deionized water and ethanol solution prepared by step 2 is rinsed, and is used after naturally dry
400 DEG C of calcining 1h remove PS templates, form the nano bowl noble coatings for suppressing Multipactor.
The present invention is successfully prepared nano bowl noble coatings in silver-plated aluminum alloy surface.It will be seen from figure 1 that by gas
The method of liquid self assembly can obtain the compact arranged PS microballoons of compound with regular structure in silver-plated aluminum alloy surface；From Fig. 2, Fig. 3, Fig. 4
With Fig. 5 as can be seen that nano bowl array structure coating can be obtained by template electrochemical deposition Ag and Au of PS microballoons；From Fig. 6
As can be seen that the nano bowl Au coatings SEY that silver-plated aluminum alloy surface is constructed is less than 1.67, secondary can be suppressed.
Claims (10)
1. a kind of preparation method for the nano bowl noble coatings for suppressing Multipactor, it is characterised in that comprise the following steps：
Step 1：The assembling of silver-plated aluminum alloy surface individual layer polystyrene microsphere
First, the sheet glass after cleaning is positioned over culture dish center, deionized water is injected into culture dish makes it not have just
Sheet glass, the hanging drop that polystyrene emulsion, second alcohol and water are made into is added on sheet glass, suspension is diffused into the water surface, treats
Stop being added dropwise after forming complete film on the water surface, most backward surface plate injection deionized water, the film of formation is with liquid level
Rise is picked up the film of formation from the water surface with silver-plated aluminium alloy print, i.e., in silver-plated aluminum alloy surface away from surface plate bottom
Individual layer PS templates are formed, obtain the silver-plated aluminium alloy print with PS templates；
Step 2：Silver-plated aluminum alloy surface electrochemical deposition noble coatings
Silver-plated aluminium alloy print with PS templates prepared by step 1 is immersed in the coating bath containing precious metal salt solution, with
Silver-plated aluminium alloy print with PS templates is cathode, and graphite is anode, and silver-plated aluminium alloy print carries the side of PS templates
It is opposite with graphite electrode, electric current is passed through between a cathode and an anode, makes noble metal loading on silver-plated aluminium alloy print；
Step 3：The formation of silver-plated aluminum alloy surface nano bowl noble coatings
The silver-plated aluminium alloy print flushing of depositing noble metal coating prepared by step 2, use solvent impregnated or calcining after drying
PS templates are removed, form the nano bowl noble coatings for suppressing Multipactor.
2. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 1, it is special
Sign is that polystyrene emulsion, the volume ratio of second alcohol and water are 1 in step 1:4:4~1:15:15, and the body of second alcohol and water
Product is than being 1:1.
3. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 1, it is special
Sign is, in step 1 in polystyrene emulsion PS microballoons a diameter of 300nm~1000nm；The size of silver-plated aluminium alloy print
For 20 × 12 × 1mm3。
4. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 1, it is special
Sign is that the distance between cathode and anode are 3~5cm in step 2.
5. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 1, it is special
Sign is that precious metal salt solution is silver nitrate solution or chlorauric acid solution in step 2.
6. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 5, it is special
Sign is, when precious metal salt solution is silver nitrate solution, deposition voltage is 0.2~0.4V, and sedimentation time is 10~30min.
7. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 5, it is special
Sign is, when precious metal salt solution is chlorauric acid solution, sedimentation time is 0.7~0.9V, and sedimentation time is 10~60min.
8. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 5, it is special
Sign is that silver nitrate solution is made by procedure below：Silver nitrate, complexing agent and potassium nitrate are added to the water, using ammonia
It is 8~10 that water, which adjusts pH value, obtains silver nitrate solution, wherein, the concentration of silver nitrate is 0.05~0.2mol/L, complexing agent it is dense
Spend for 0.05~0.2mol/L, the concentration of potassium nitrate is 0.025~0.1mol/L；Wherein, complexing agent is ethylenediamine tetra-acetic acid two
Sodium.
9. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 5, it is special
Sign is that chlorauric acid solution is made by procedure below：Gold chloride, complexing agent, sodium sulfite and disodium hydrogen phosphate are added
Into water, chlorauric acid solution is obtained；Wherein, gold chloride concentration is 0.02~0.05mol/L, complexing agent concentration for 0.01~
0.03mol/L, concentration of sodium sulfite are 0.5~1.5mol/L, and disodium hydrogen phosphate concentration is 0.1~0.3mol/L；Wherein, it is complexed
Agent is disodium ethylene diamine tetraacetate.
10. a kind of preparation method of nano bowl noble coatings for suppressing Multipactor according to claim 1, it is special
Sign is that solvent is dichloromethane, toluene or chloroform in step 3；The temperature of calcining is 200~400 DEG C, and the time of calcining is
60min。
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