CN103320799A - Method for restraining secondary electron yield on silver coating surface of microwave component - Google Patents
Method for restraining secondary electron yield on silver coating surface of microwave component Download PDFInfo
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- CN103320799A CN103320799A CN2013102641496A CN201310264149A CN103320799A CN 103320799 A CN103320799 A CN 103320799A CN 2013102641496 A CN2013102641496 A CN 2013102641496A CN 201310264149 A CN201310264149 A CN 201310264149A CN 103320799 A CN103320799 A CN 103320799A
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- microwave component
- secondary electron
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- electron yield
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Abstract
The invention relates to a method for restraining secondary electron yield on a silver coating surface of a microwave component, particularly relates to the method for restraining the secondary electron yield on the silver coating surface of the microwave component by an electrochemical corrosion method, and belongs to the technical field of micro-discharge. Firstly, anodic oxidation treatment is carried out on the inner surface of the microwave component by using an acid solution; a porous structure is formed at the inner surface of the microwave component; then the caliber of a large hole is increased by using a chemical solution corrosion method; and finally metal with good electrical conductivity such as gold or silver and the like is spluttered and deposited at the inner surface of the microwave component, so that the inner surface of the microwave component has a low secondary electron yield and good conductivity.
Description
Technical field
The present invention relates to a kind of method that suppresses microwave component silvered film surface secondary electron yield, particularly a kind ofly suppress the method for the secondary electron yield of aluminium alloy silver-plated surface by electrochemical etching method, belong to the micro discharges technical field.
Background technology
The micro discharges effect is under vacuum condition, electronics under the acceleration of radio-frequency field, the secondary electron emission that between two metallic surfaces, excites and the effect of multiplication.The micro discharges effect takes place in the internal electric field of spacecraft such as multiplexer, wave filter HIGH-POWERED MICROWAVES parts strong zone easily, causes the HIGH-POWERED MICROWAVES component failure, even whole useful load was thoroughly lost efficacy.Therefore, the spacecraft microwave component must carry out the inhibition design of micro discharges effect, guarantees that spacecraft is at safety, the reliability service of rail.
Patent " Carbon nitride coating applicable to prevent the multipactor effect " proposes to suppress in material surface plating one deck carbon nitride films the surface treatment method of micro discharges, but the poor electric conductivity of carbon nitride films makes that the Insertion Loss of microwave component is bigger.
Patent " Titanium nitride thin films for minimizing multipactoring " proposes to suppress at material surface plating one deck titanium nitride membrane the surface treatment method of micro discharges, but the aerial poor stability of titanium nitride membrane, secondary electron yield sharply increases after after a while.
Summary of the invention
The objective of the invention is in order to propose a kind of method that suppresses microwave component silvered film surface secondary electron yield, this method can make micro discharges threshold value height, little, the good stability of loss on aluminium alloy silvered film surface.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method that suppresses microwave component silvered film surface secondary electron yield of the present invention, the microwave component internal surface is carried out anodic oxidation treatment with acid solution earlier, form vesicular structure at the microwave component internal surface, utilize the chemical solution corroding method to increase the bore in hole then, last metal in good conductivity such as microwave component internal surface sputtering sedimentation gold or silver, make the microwave component internal surface both have low secondary electron yield, have excellent conducting performance again.
Concrete step is:
1) be that the method for galvanic corrosion is in microwave component surface punching with electrolyzer;
Corrosion current: 200～400mA/cm
2, etching time is 10～30s;
Electrolyte prescription: HCl+K
2Cr
2O
7+ H
2SO
4(HCl0.5M～1.5M, K
2Cr
2O
70.1M～0.5M, H
2SO
40.2M～0.6M), anode material is microwave component, the material of described microwave component is aluminium alloy; Cathode material is graphite;
2) microwave component that has the hole that step 1) is obtained carries out further reaming; It is the method for galvanic corrosion that electrolyzer is adopted in reaming;
Corrosion current: 10～50mA/cm
2, etching time 3～8min;
The HCl of electrolyte prescription: 0.01～0.05M; Anode material is microwave component, and cathode material is graphite;
3) in step 2) the internal surface magnetron sputtering copper layer in the hole of the microwave component that obtains is as transition layer; At the surface magnetic control sputtering silver layer of transition layer, at last microwave component is carried out vacuum heat treatment then, obtain the low microwave component of silvered film surface secondary electron yield.
Behind the magnetron sputtering silver layer silver layer surface of microwave component is carried out vacuum nitrogen in the described step 3) and clean, vacuum tightness is higher than 3 * 10
-4Pa;
Splash-proofing sputtering process parameter in the described step 3) during sputter copper layer is: Ar air-flow 20sccm, sputtering pressure 1.4Pa, sputtering current 0.5A, voltage 280V, sputtering time 10mins, sputter temperature: room temperature;
Splash-proofing sputtering process parameter in the described step 3) during sputter silver layer is: Ar air-flow 30sccm, sputtering pressure 1.4Pa, sputtering current 0.2A, voltage 260V, sputtering time 10mins, sputter temperature: room temperature;
The condition of vacuum heat treatment is in the described step 3): vacuum tightness is higher than 2.5 * 10
-4Pa, temperature is 200 ℃, the time is 20mins; Vacuum heat treatment can further increase the bonding force between top layer metal and the alloy matrix aluminum.
Description of drawings
Fig. 1 is the structural representation of electrolyzer of the present invention;
Fig. 2 is the surface microscopic topographic figure of microwave component when not carrying out splash-proofing sputtering metal;
Fig. 3 is the surface microscopic topographic figure that carries out microwave component behind the sputter silver layer;
The surperficial secondary electron yield graphic representation of the microwave component that Fig. 4 obtains for Comparative Examples and method of the present invention.
Embodiment
So-called its conversion unit of electrolyzer is used in galvanic corrosion, makes electric current pass through electrolyte solution (or ionogen of fusion), and causes the process of redox reaction at yin, yang the two poles of the earth.The electrode that links to each other with the positive pole of power supply is called anode.Material loses electronics at anode, and oxidizing reaction takes place.The electrode that links to each other with the negative pole of power supply becomes negative electrode.Material obtains electronics at negative electrode, and reduction reaction takes place.
The two electrodes method is taked in galvanic corrosion, and as electrolytic solution, as anode, inert material is as cathodic counter electrode (as Graphite Electrodes, Ti electrode) with aluminum alloy materials with specific corrosive fluid.After the energising, aluminum alloy surface loses electronics, causes atom to come off from aluminum alloy surface, forms corrosion hole.When a large amount of electronics come off from the position of concentrating, just might form micron-sized big corrosion hole.
Relative certain metal in the galvanic corrosion, specific ion has two kinds of results after its surface adsorption, and first kind is to be adsorbed on its surface, and second kind and metal ion diffuse to solution together.These two kinds of different states are exactly the effect of protection and corrosion for the effect of corrosion.By adding the effect that the different etching reagent of measuring and protective material just can reach pitting corrosion.Easier being corroded in position that corrosion is come out,, the hole reaches the hole of the high aspect ratio of final requirement thereby enlarging.
Who preponderates in the corrosion protection process; determined by erosion rate; it is the principal elements that influence corrosion process that the free energy of activation of etching reagent and protectant concentration, etching reagent and protective material precipitation thinner free energy change, free etching reagent molecule and free protective material molecule and metal reaction becomes these three kinds of factors, and temperature also is a significant effects factor in addition.
Mainly be to adopt the combination of different protective materials and etching reagent to realize the directional etching on duralumin surface in corrosion; increase the on average inhibition ability of secondary electron of its surface by increasing hole density and depth-to-width ratio, and guarantee that the size in aperture is lower than the pore size of the microwave transmission scope that influences.
The invention will be further described below in conjunction with drawings and Examples.
Embodiment
1) with electrolyzer as shown in Figure 1, in the punching of microwave component surface;
Corrosion current: 200～400mA/cm
2, etching time is 10～30s;
Electrolyte prescription: HCl+K
2Cr
2O
7+ H
2SO
4(HCl0.5M～1.5M, K
2Cr
2O
70.1M～0.5M, H
2SO
40.2M～0.6M), anode material is microwave component, the material of described microwave component is aluminium alloy; Cathode material is graphite;
2) microwave component that has the hole that step 1) is obtained carries out further reaming, and the microscopic appearance of the microwave component that obtains as shown in Figure 2; It is the method for galvanic corrosion that electrolyzer is adopted in reaming;
Corrosion current: 10～50mA/cm
2, etching time 3～8min;
The HCl of electrolyte prescription: 0.01～0.05M; Anode material is microwave component, and cathode material is graphite;
3) in step 2) the internal surface magnetron sputtering copper layer in the hole of the microwave component that obtains is as transition layer; At the surface magnetic control sputtering silver layer of transition layer, at last microwave component is carried out vacuum heat treatment then, obtain the low microwave component of silvered film surface secondary electron yield, the microscopic appearance of the microwave component that obtains as shown in Figure 3;
Behind the sputter silver layer silver layer surface of microwave component is carried out vacuum nitrogen in the described step 3) and clean, vacuum tightness is higher than 3 * 10
-4Pa;
Splash-proofing sputtering process parameter in the described step 3) during sputter copper layer is: Ar air-flow 20sccm, sputtering pressure 1.4Pa, sputtering current 0.5A, voltage 280V, sputtering time 10mins, sputter temperature: room temperature;
Splash-proofing sputtering process parameter in the described step 3) during sputter silver layer is: Ar air-flow 30sccm, sputtering pressure 1.4Pa, sputtering current 0.2A, voltage 260V, sputtering time 10mins, sputter temperature: room temperature;
The condition of vacuum heat treatment is in the described step 3): vacuum tightness is higher than 2.5 * 10
-4Pa, temperature is 200 ℃, the time is 20mins; Vacuum heat treatment can further increase the bonding force between top layer metal and the alloy matrix aluminum.
Comparative Examples
1) surface cleaning of aluminium alloy microwave component
The aluminium alloy microwave component was soaked in 50～90 ℃ metal cleaner more than 30 minutes, and remaining scavenging solution on the cleaning aluminum alloy microwave component in hot water tank cleans with alkali electroless reagent again;
2) silver-plated at aluminium alloy microwave component surface electrochemistry
The aluminium alloy microwave component as anode, is put into electroplate liquid, and the chemical ingredients of electroplate liquid is: silver potassium cyanide: 66.5g/L, and Repone K: 150g/L, salt of wormwood: 15g/L, temperature of electroplating solution: 20 ℃, electroplating time: 30s, current density: 1.0A/cm
2
3) carry out chemical passivation at silver-plated surface
The microwave component of having electroplated is put into passivating solution, passivating solution composition: potassium bichromate: 15g/L, nitric acid: 15ml/L, passivating solution temperature: room temperature, passivation time: 30s.
The microwave component that the microwave component that Comparative Examples is obtained and embodiment obtain carries out the secondary electron yield test, the result as shown in Figure 4, as shown in Figure 4, the secondary electron yield of the microwave component that obtains of embodiment has reduced by 24%, the first energy intersection point and has improved 1 times.
Claims (5)
1. method that suppresses microwave component silvered film surface secondary electron yield, it is characterized in that: concrete step is as follows:
1) be that the method for galvanic corrosion is in microwave component surface punching with electrolyzer;
Corrosion current: 200～400mA/cm
2, etching time is 10～30s;
Electrolyte prescription: HCl+K
2Cr
2O
7+ H
2SO
4(HCl0.5M～1.5M, K
2Cr
2O
70.1M～0.5M, H
2SO
40.2M～0.6M), anode material is microwave component, the material of described microwave component is aluminium alloy; Cathode material is graphite;
2) microwave component that has the hole that step 1) is obtained carries out further reaming; It is the method for galvanic corrosion that electrolyzer is adopted in reaming;
Corrosion current: 10～50mA/cm
2, etching time 3～8min;
The HCl of electrolyte prescription: 0.01～0.05M; Anode material is microwave component, and cathode material is graphite;
3) in step 2) the internal surface magnetron sputtering copper layer in the hole of the microwave component that obtains is as transition layer; At the surface magnetic control sputtering silver layer of transition layer, at last microwave component is carried out vacuum heat treatment then, obtain the low microwave component of silvered film surface secondary electron yield.
2. a kind of method that suppresses microwave component silvered film surface secondary electron yield according to claim 1 is characterized in that: behind the magnetron sputtering silver layer silver layer surface of microwave component is carried out vacuum nitrogen in the step 3) and clean, vacuum tightness is higher than 3 * 10
-4Pa.
3. a kind of method that suppresses microwave component silvered film surface secondary electron yield according to claim 1, it is characterized in that: the splash-proofing sputtering process parameter in the step 3) during sputter copper layer is: Ar air-flow 20sccm, sputtering pressure 1.4Pa, sputtering current 0.5A, voltage 280V, sputtering time 10mins, sputter temperature: room temperature.
4. a kind of method that suppresses microwave component silvered film surface secondary electron yield according to claim 1, it is characterized in that: the splash-proofing sputtering process parameter in the step 3) during sputter silver layer is: Ar air-flow 30sccm, sputtering pressure 1.4Pa, sputtering current 0.2A, voltage 260V, sputtering time 10mins, sputter temperature: room temperature.
5. a kind of method that suppresses microwave component silvered film surface secondary electron yield according to claim 1, it is characterized in that: the condition of vacuum heat treatment is in the step 3): vacuum tightness is higher than 2.5 * 10
-4Pa, temperature is 200 ℃, the time is 20mins.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107453726A (en) * | 2017-08-08 | 2017-12-08 | 随州泰华电子科技有限公司 | A kind of technique for lifting tuning fork crystal oscillation ion(ic) etching speed |
| CN111270249A (en) * | 2020-03-24 | 2020-06-12 | 西安交通大学 | Aluminum-based material and surface treatment method for reducing secondary electron emission coefficient |
| CN113594014A (en) * | 2020-04-30 | 2021-11-02 | 中微半导体设备(上海)股份有限公司 | Component, plasma reaction device and component processing method |
| CN115261776B (en) * | 2022-07-22 | 2024-04-09 | 西安空间无线电技术研究所 | Method for inhibiting secondary electron emission of microwave component material based on plasma fluorination |
| CN113594014B (en) * | 2020-04-30 | 2024-04-12 | 中微半导体设备(上海)股份有限公司 | Component, plasma reaction device, and component processing method |
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|---|---|---|---|---|
| US7090554B1 (en) * | 1998-12-11 | 2006-08-15 | Candescent Technologies Corporation | Fabrication of flat-panel display having spacer with rough face for inhibiting secondary electron escape |
| CN102515085A (en) * | 2011-11-14 | 2012-06-27 | 西安交通大学 | Method for restraining secondary emission of surface nano-structure of microwave component |
| CN102732931A (en) * | 2012-06-27 | 2012-10-17 | 西安交通大学 | Method for inhibiting secondary electron emission of microwave component surface by adopting nanostructure plating layer |
| CN102925893A (en) * | 2012-10-31 | 2013-02-13 | 西安空间无线电技术研究所 | Microetch process for restraining micro-discharge effect of microwave part |
-
2013
- 2013-06-27 CN CN201310264149.6A patent/CN103320799B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7090554B1 (en) * | 1998-12-11 | 2006-08-15 | Candescent Technologies Corporation | Fabrication of flat-panel display having spacer with rough face for inhibiting secondary electron escape |
| CN102515085A (en) * | 2011-11-14 | 2012-06-27 | 西安交通大学 | Method for restraining secondary emission of surface nano-structure of microwave component |
| CN102732931A (en) * | 2012-06-27 | 2012-10-17 | 西安交通大学 | Method for inhibiting secondary electron emission of microwave component surface by adopting nanostructure plating layer |
| CN102925893A (en) * | 2012-10-31 | 2013-02-13 | 西安空间无线电技术研究所 | Microetch process for restraining micro-discharge effect of microwave part |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107453726A (en) * | 2017-08-08 | 2017-12-08 | 随州泰华电子科技有限公司 | A kind of technique for lifting tuning fork crystal oscillation ion(ic) etching speed |
| CN111270249A (en) * | 2020-03-24 | 2020-06-12 | 西安交通大学 | Aluminum-based material and surface treatment method for reducing secondary electron emission coefficient |
| CN111270249B (en) * | 2020-03-24 | 2021-09-03 | 西安交通大学 | Aluminum-based material and surface treatment method for reducing secondary electron emission coefficient |
| CN113594014A (en) * | 2020-04-30 | 2021-11-02 | 中微半导体设备(上海)股份有限公司 | Component, plasma reaction device and component processing method |
| CN113594014B (en) * | 2020-04-30 | 2024-04-12 | 中微半导体设备(上海)股份有限公司 | Component, plasma reaction device, and component processing method |
| CN115261776B (en) * | 2022-07-22 | 2024-04-09 | 西安空间无线电技术研究所 | Method for inhibiting secondary electron emission of microwave component material based on plasma fluorination |
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| CN103320799B (en) | 2014-11-19 |
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