CN106835078A - A kind of structure of trap Ag/TiO2The preparation method of/Au coatings - Google Patents

A kind of structure of trap Ag/TiO2The preparation method of/Au coatings Download PDF

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CN106835078A
CN106835078A CN201710042284.4A CN201710042284A CN106835078A CN 106835078 A CN106835078 A CN 106835078A CN 201710042284 A CN201710042284 A CN 201710042284A CN 106835078 A CN106835078 A CN 106835078A
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trap
silver
coatings
tio
tbt
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CN106835078B (en
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马建中
吴朵朵
鲍艳
崔万照
胡天存
杨晶
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Shaanxi University of Science and Technology
Xian Institute of Space Radio Technology
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Xian Institute of Space Radio Technology
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    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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    • C23C18/1241—Metallic substrates
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    • 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
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1254—Sol or sol-gel processing
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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Abstract

The invention discloses a kind of structure of trap Ag/TiO2The preparation method of/Au coatings, silver-plated aluminum alloy surface is processed using two step wet-chemical chamber methods, silver-plated aluminum alloy surface is formed structure of trap；Then TiO is prepared using class electroless plating method on structure of trap surface2Film transition layer, to reach TiO2Profile-followed deposition of the film on structure of trap surface；Finally using electroless plating method in TiO2Surface deposits Au films with the shape, so as to form a kind of structure of trap Ag/TiO in silver-plated aluminum alloy surface2/ Au coatings, improve the secondary electron rejection characteristic and its environmental stability of silver-plated aluminum alloy surface.

Description

A kind of structure of trap Ag/TiO2The preparation method of/Au coatings
Technical field
The present invention relates to a kind of structure of trap Ag/TiO2The preparation method of/Au coatings, more particularly in silver-plated aluminium alloy table Structure of trap Ag/TiO is constructed in face2/ Au coatings, improve the secondary electron rejection characteristic and its ambient stable of silver-plated aluminum alloy surface Property.
Background technology
The base material that silver-plated aluminium alloy is commonly used as microwave component in current Satellite Payloads system, with device can be reduced The advantage of part loss, but in actual use, silver-plated part is susceptible to two under great-power electromagnetic ripple transmission conditions Secondary electron multiplication is to produce Multipactor, causes HIGH-POWERED MICROWAVES component failure.Suppress the method master of Multipactor at present Parts surface is included in construct coating and construct structure of trap etc. in parts surface.
Research shows that being prepared in silver-plated aluminum alloy surface has the coating material of low secondary electron yield (SEY), such as Titanium nitride (TiN), graphitized carbon etc., can effectively suppress Multipactor, but such coating material self-conductive is poor, makes microwave Part is big in high frequency condition lower surface impedance.
Document " Controllable fabrication of one-dimensional ZnO nanoarrays and their application in constructing silver trap structures.RSC Advances.2014,4, 33198-33205. " one kind is disclosed with ZnO arrays as template, is prepared in silver-plated aluminum alloy surface by electrochemical deposition method Structure of trap silver, it is possible to decrease SEY to less than 1.6, but the method technical process is relatively complicated.
Document " Investigation into anomalous total secondary electron yield for micro-porous Ag surface under oblique incidence conditions.Journal of Applied Physics.2013,114:1-9. " discloses the method for constructing structure of trap silver a kind of easy to operate and low cost, it is possible to decrease The SEY of silver-plated aluminium alloy to less than 1.2, but the method there are certain requirements to the grain boundary structure of initial silver-plated aluminium alloy.Additionally, falling into The environmental stability of well structure silver is typically poor.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of structure of trap Ag/TiO2The preparation of/Au coatings Method, the method is simple, and grain boundary structure to initial silver-plated aluminium alloy is not required, while can both reduce silver coated aluminum conjunction The SEY of gold, can improve its environmental stability again.
To realize above-mentioned target, the technical solution adopted by the present invention is：
A kind of structure of trap Ag/TiO2The preparation method of/Au coatings, comprises the following steps：
(1) using Fe (NO3)3The aqueous solution is performed etching to silver-plated aluminium alloy, and etching temperature is 45-55 DEG C, and etch period is 35-45s, dries after cleaning；
Repeat step (1), structure of trap is formed in silver-plated aluminum alloy surface；
(2) the silver-plated aluminium alloy that surface forms structure of trap be impregnated in into 10-30min in TBT solution, is then transferred to 10-20min is reacted in ionized water, is finally calcined；
(3) the silver-plated aluminium alloy after step (2) is calcined is placed in gold plating liquid and reacts 0.5-2h at 25-35 DEG C, cleans After dry, obtain structure of trap Ag/TiO2/ Au coatings.
The present invention is further improved, the Fe (NO3)3The mass fraction of the aqueous solution is 20%-40%.
Further improvement of the invention is that the TBT solution is by obtained in procedure below：By TBT, glacial acetic acid and Ethanol is well mixed, and obtains TBT solution, wherein, the mass fraction of TBT is 3%-7%, the quality point of glacial acetic acid in TBT solution Number is 4%-6%.
Further improvement of the invention is that the temperature of the calcining is 100-400 DEG C, and the time is 1h.
Further improvement of the invention is that the gold plating liquid is prepared by procedure below：By HAuCl4, glucose, nothing Aqueous sodium carbonate is added to the water, and is well mixed, and obtains the gold plating liquid that pH value is 10.5-11.5；Wherein, HAuCl4Concentration be 2- 6mmol/L, the concentration of glucose is 4-12mmol/L.
Further improvement of the invention is that the dry temperature in step (1), step (2) and step (3) is 50-70 DEG C, the time is 30min.
Compared with the prior art, the invention has the advantages that：
1. the present invention prepares structure of trap silver, to initial by repeating etch step using two step wet-chemical chamber methods The grain boundary structure of silver-plated aluminium alloy do not require, and two step wet-chemical chambers prepare structure of trap silver technology stability it is good.Adopt TiO is prepared with class electroless plating method2Film transition layer, it is easy to operate, it is possible to achieve TiO2The profile-followed deposition of film, does not destroy original Structure of trap.Using chemically plating for Au films as environmental stability coating, technical process is easy.
2. the present invention constructs structure of trap reduction SEY by silver-plated aluminum alloy surface, and profile-followed deposition Au coatings improve ring Border stability, introduces TiO between the two2Transition zone prevents the formation of electrum, it is to avoid electrical property declines.
3. the structure of trap Ag/TiO for being prepared using the present invention2/Au coatings can make the SEY of silver-plated aluminium alloy be reduced to 1.2 with Under, the secondary electron rejection characteristic of silver-plated aluminum alloy surface is improved, and environmental stability is good.
Further, Fe (NO in the present invention3)3The mass fraction of the aqueous solution is 20%-40%, if concentration is too low, it is impossible to Structure of trap is formed, if excessive concentration, overetch can be caused.
Further, the glacial acetic acid in TBT solution plays a part of complexing agent, and ethanol plays scattered work as solvent With.
Further, the temperature of calcining uses 100-400 DEG C, because different calcining heats can form different crystal forms Titanium dioxide, and calcining heat is too high, silver-plated aluminium alloy can deform, in order to obtain anatase crystal and not shadow in the present invention The shape of the silver-plated aluminium alloy of sound, so using 100-400 DEG C.
Brief description of the drawings
Fig. 1 is the SEM photograph of silver-plated aluminium alloy after two step wet-chemical chambers, wherein, figure (a) multiplication factor is 10k, figure B () multiplication factor is 20k.
Fig. 2 is class chemically plating for TiO2SEM photograph after film, wherein, figure (a) multiplication factor is 10k, and figure (b) is put Big multiple is 30k.
Fig. 3 be chemically plating for the SEM photograph after Au films, wherein, figure (a) multiplication factor be 5k, scheme (b) multiplication factor It is 30k.
Fig. 4 is that the SEY characteristics of the 4 silver-plated aluminum alloy samples prepared by the step wet-chemical chamber technique of identical two are bent Line.
Fig. 5 is structure of trap Ag/TiO2After/Au coatings are placed 6 months, the SEY after its surface takes 3 point tests at random Characteristic curve.
Specific embodiment
With reference to specific embodiment and accompanying drawing, the present invention will be described in detail.
Embodiment 1
(1) it is 20mm long, 12mm wide, 1mm high to size to use 50mL detergent, deionized water, acetone and ethanol successively Silver-plated aluminium alloy be cleaned by ultrasonic, each 15min.
(2) use 12g mass fractions for 20% Fe (NO3)3Silver-plated aluminium alloy after the aqueous solution is cleaned to step (1) enters Row etching, etching temperature is 45 DEG C, and etch period is 35s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 50 DEG C of baking ovens.
(3) use 12g mass fractions for 20% Fe (NO3)3The aqueous solution enters to the dried silver-plated aluminium alloy of step (2) Row etching, etching temperature is 45 DEG C, and etch period is 35s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 50 DEG C of baking ovens, and structure of trap is formed in silver-plated aluminum alloy surface.
(4) the dried silver-plated aluminium alloy of step (3) be impregnated in into 10min in 10g TBT solution, is then transferred to 50mL 10min is reacted in deionized water, finally in Muffle furnace in calcining 1h at 100 DEG C.Wherein, TBT solution passes through procedure below system ：TBT, glacial acetic acid and ethanol are well mixed, TBT solution is obtained, wherein, the mass fraction of TBT is 3%, ice in TBT solution The mass fraction of acetic acid is 4%.
(5) the silver-plated aluminium alloy after step (4) is calcined is placed in 25mL gold plating liquids and reacts 0.5h at 25 DEG C, then adopts Silver-plated aluminium alloy is cleaned with deionized water and is cleaned by ultrasonic 15min, finally dry 30min in 50 DEG C of baking ovens, obtain trap knot Structure Ag/TiO2/ Au coatings.Wherein, gold plating liquid is prepared by procedure below：By HAuCl4, glucose, natrium carbonicum calcinatum be added to In water, it is well mixed, obtains the gold plating liquid that pH value is 10.5；Wherein, HAuCl4Concentration be 2mmol/L, the concentration of glucose It is 4mmol/L.
Embodiment 2
(1) successively using 50mL detergent, deionized water, acetone and ethanol to the 20mm long, 12mm wide, 1mm high of size Silver-plated aluminium alloy be cleaned by ultrasonic, each 15min.
(2) use 12g mass fractions for 40% Fe (NO3)3Silver-plated aluminium alloy after the aqueous solution is cleaned to step (1) enters Row etching, etching temperature is 55 DEG C, and etch period is 45s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 70 DEG C of baking ovens.
(3) use 12g mass fractions for 40% Fe (NO3)3The aqueous solution enters to the dried silver-plated aluminium alloy of step (2) Row etching, etching temperature is 55 DEG C, and etch period is 45s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 70 DEG C of baking ovens, and structure of trap is formed in silver-plated aluminum alloy surface.
(4) the dried silver-plated aluminium alloy of step (3) be impregnated in into 30min in 10g TBT solution, is then transferred to 50mL 20min is reacted in deionized water, finally in Muffle furnace in calcining 1h at 400 DEG C.Wherein, TBT solution passes through procedure below system ：TBT, glacial acetic acid and ethanol are well mixed, TBT solution is obtained, wherein, the mass fraction of TBT is 7%, ice in TBT solution The mass fraction of acetic acid is 6%.
(5) the silver-plated aluminium alloy after step (4) is calcined is placed in 25mL gold plating liquids and reacts 2h at 35 DEG C, then uses Deionized water is cleaned silver-plated aluminium alloy and is cleaned by ultrasonic 15min, finally dries 30min in 70 DEG C of baking ovens, obtains structure of trap Ag/TiO2/ Au coatings.Wherein, gold plating liquid is prepared by procedure below：By HAuCl4, glucose, natrium carbonicum calcinatum be added to water In, it is well mixed, obtain the gold plating liquid that pH value is 11.5；Wherein, HAuCl4Concentration be 6mmol/L, the concentration of glucose is 12mmol/L。
Embodiment 3
(1) it is 20mm long, 12mm wide, 1mm high to size to use 50mL detergent, deionized water, acetone and ethanol successively Silver-plated aluminium alloy be cleaned by ultrasonic, each 15min.
(2) use 12g mass fractions for 30% Fe (NO3)3Silver-plated aluminium alloy after the aqueous solution is cleaned to step (1) enters Row etching, etching temperature is 50 DEG C, and etch period is 40s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 60 DEG C of baking ovens.
(3) use 12g mass fractions for 20% Fe (NO3)3Silver-plated aluminium alloy after the aqueous solution is cleaned to step (2) enters Row etching, etching temperature is 50 DEG C, and etch period is 40s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 60 DEG C of baking ovens, and structure of trap is formed in silver-plated aluminum alloy surface.
(4) the dried silver-plated aluminium alloy of step (3) be impregnated in into 20min in 10g TBT, be then transferred to 50mL go from 10min is reacted in sub- water, finally in Muffle furnace in calcining 1h at 200 DEG C.Wherein, TBT solution is obtained by procedure below：Will TBT, glacial acetic acid and ethanol are well mixed, and obtain TBT solution, wherein, the mass fraction of TBT is 5%, glacial acetic acid in TBT solution Mass fraction be 4%.
(5) the silver-plated aluminium alloy after step (4) is calcined is placed in 25mL gold plating liquids and reacts 1h at 30 DEG C, then uses Deionized water is cleaned silver-plated aluminium alloy and is cleaned by ultrasonic 15min, finally dries 30min in 60 DEG C of baking ovens, obtains structure of trap Ag/TiO2/ Au coatings.Wherein, gold plating liquid is prepared by procedure below：By HAuCl4, glucose, natrium carbonicum calcinatum be added to water In, it is well mixed, obtain the gold plating liquid that pH value is 10.8；Wherein, HAuCl4Concentration be 4mmol/L, the concentration of glucose is 8mmol/L。
Embodiment 4
(1) it is 20mm long, 12mm wide, 1mm high to size to use 50mL detergent, deionized water, acetone and ethanol successively Silver-plated aluminium alloy be cleaned by ultrasonic, each 15min.
(2) use 12g mass fractions for 40% Fe (NO3)3Silver-plated aluminium alloy after the aqueous solution is cleaned to step (1) enters Row etching, etching temperature is 50 DEG C, and etch period is 40s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 60 DEG C of baking ovens.
(3) use 12g mass fractions for 20% Fe (NO3)3The aqueous solution enters to the dried silver-plated aluminium alloy of step (2) Row etching, etching temperature is 50 DEG C, and etch period is 40s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 60 DEG C of baking ovens, and structure of trap is formed in silver-plated aluminum alloy surface.
(4) the dried silver-plated aluminium alloy of step (3) be impregnated in into 20min in 10g TBT solution, is then transferred to 50mL 10min is reacted in deionized water, finally in Muffle furnace in calcining 1h at 400 DEG C.Wherein, TBT solution passes through procedure below system ：TBT, glacial acetic acid and ethanol are well mixed, TBT solution is obtained, wherein, the mass fraction of TBT is 3%, ice in TBT solution The mass fraction of acetic acid is 4%.
(5) the silver-plated aluminium alloy after step (4) is calcined is placed in 25mL gold plating liquids and reacts 1h at 30 DEG C, then uses Deionized water is cleaned silver-plated aluminium alloy and is cleaned by ultrasonic 15min, finally dries 30min in 60 DEG C of baking ovens, obtains structure of trap Ag/TiO2/ Au coatings.Wherein, gold plating liquid is prepared by procedure below：By HAuCl4, glucose, natrium carbonicum calcinatum be added to water In, it is well mixed, obtain the gold plating liquid that pH value is 11.5；Wherein, HAuCl4Concentration be 4mmol/L, the concentration of glucose is 8mmol/L。
Embodiment 5
(1) it is 20mm long, 12mm wide, 1mm high to size to use 50mL detergent, deionized water, acetone and ethanol successively Silver-plated aluminium alloy be cleaned by ultrasonic, each 15min.
(2) use 12g mass fractions for 30% Fe (NO3)3Silver-plated aluminium alloy after the aqueous solution is cleaned to step (1) enters Row etching, etching temperature is 50 DEG C, and etch period is 38s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 70 DEG C of baking ovens.
(3) use 12g mass fractions for 30% Fe (NO3)3The aqueous solution enters to the dried silver-plated aluminium alloy of step (2) Row etching, etching temperature is 55 DEG C, and etch period is 38s, then cleans silver-plated aluminium alloy using deionized water and is cleaned by ultrasonic 3min, finally dries 30min in 60 DEG C of baking ovens, and structure of trap is formed in silver-plated aluminum alloy surface.
(4) the dried silver-plated aluminium alloy of step (3) be impregnated in into 20min in 10g TBT solution, is then transferred to 50mL 10min is reacted in deionized water, finally in Muffle furnace in calcining 1h at 300 DEG C.Wherein, TBT solution passes through procedure below system ：TBT, glacial acetic acid and ethanol are well mixed, TBT solution is obtained, wherein, the mass fraction of TBT is 5%, ice in TBT solution The mass fraction of acetic acid is 4%.
(5) the silver-plated aluminium alloy after step (4) treatment is placed in 25mL gold plating liquids and reacts 1h at 35 DEG C, then used Deionized water is cleaned silver-plated aluminium alloy and is cleaned by ultrasonic 15min, finally dries 30min in 70 DEG C of baking ovens, obtains structure of trap Ag/TiO2/ Au coatings.Wherein, gold plating liquid is prepared by procedure below：By HAuCl4, glucose, natrium carbonicum calcinatum be added to water In, it is well mixed, obtain the gold plating liquid that pH value is 11.5；Wherein, HAuCl4Concentration be 6mmol/L, the concentration of glucose is 12mmol/L。
Structure of trap Ag/TiO is successfully prepared using the method for the present invention2/ Au coatings.It will be seen from figure 1 that by two There is significant structure of trap in the silver-plated aluminum alloy surface for walking wet-chemical chamber, figure it is seen that TiO2Film is by tiny TiO2Particle is constituted, and the film realizes profile-followed deposition in structure of trap silver surface.From figure 3, it can be seen that Au coating is by chi Very little uniform Au particles are constituted, and structure of trap surface is deposited on the shape.Fig. 4 is prepared by the step wet-chemical chamber technique of identical two 4 SEY characteristic curves of silver-plated aluminum alloy sample, 4 silver-plated aluminum alloy samples are respectively designated as S-1, S-2, S-3 and S-4,4 The SEY of individual silver-plated aluminum alloy sample shows the technique that two step wet-chemical chamber methods prepare structure of trap silver coating below 1.3 Stability is preferable.Fig. 5 is structure of trap Ag/TiO2After/Au coatings are placed 6 months, take what 3 points were tested at random on its surface SEY, 3 points are respectively designated as point 1, point 2 and 3,3 SEY of point of point below 1.2, show trap knot Structure Ag/TiO2The covering of/Au coatings is uniform, and environmental stability is good.

Claims (6)

1. a kind of structure of trap Ag/TiO2The preparation method of/Au coatings, it is characterised in that comprise the following steps：
(1) using Fe (NO3)3The aqueous solution is performed etching to silver-plated aluminium alloy, and etching temperature is 45-55 DEG C, and etch period is 35- 45s, dries after cleaning；
Repeat step (1), structure of trap is formed in silver-plated aluminum alloy surface；
(2) the silver-plated aluminium alloy that surface forms structure of trap be impregnated in into 10-30min in TBT solution, is then transferred to deionization 10-20min is reacted in water, is finally calcined；
(3) the silver-plated aluminium alloy after step (2) is calcined is placed in gold plating liquid and 0.5-2h is reacted at 25-35 DEG C, is done after cleaning It is dry, obtain structure of trap Ag/TiO2/ Au coatings.
2. a kind of structure of trap Ag/TiO according to claim 12The preparation method of/Au coatings, it is characterised in that described Fe(NO3)3The mass fraction of the aqueous solution is 20%-40%.
3. a kind of structure of trap Ag/TiO according to claim 12The preparation method of/Au coatings, it is characterised in that described TBT solution is by obtained in procedure below：TBT, glacial acetic acid and ethanol are well mixed, TBT solution is obtained, wherein, TBT is molten The mass fraction of TBT is 3%-7% in liquid, and the mass fraction of glacial acetic acid is 4%-6%.
4. a kind of structure of trap Ag/TiO according to claim 12The preparation method of/Au coatings, it is characterised in that described The temperature of calcining is 100-400 DEG C, and the time is 1h.
5. a kind of structure of trap Ag/TiO according to claim 12The preparation method of/Au coatings, it is characterised in that described Gold plating liquid is prepared by procedure below：By HAuCl4, glucose, natrium carbonicum calcinatum be added to the water, be well mixed, obtain pH value It is the gold plating liquid of 10.5-11.5；Wherein, HAuCl4Concentration be 2-6mmol/L, the concentration of glucose is 4-12mmol/L.
6. a kind of structure of trap Ag/TiO according to claim 12The preparation method of/Au coatings, it is characterised in that step (1), the dry temperature in step (2) and step (3) is 50-70 DEG C, and the time is 30min.
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