CN102407219A - Preparation method of super-hydrophobic surface of amorphous metal - Google Patents
Preparation method of super-hydrophobic surface of amorphous metal Download PDFInfo
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- CN102407219A CN102407219A CN201110277020XA CN201110277020A CN102407219A CN 102407219 A CN102407219 A CN 102407219A CN 201110277020X A CN201110277020X A CN 201110277020XA CN 201110277020 A CN201110277020 A CN 201110277020A CN 102407219 A CN102407219 A CN 102407219A
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Abstract
The invention provides a preparation method of a super-hydrophobic surface of an amorphous metal. The preparation method comprises the following steps of: processing the surface of the amorphous metal, processing the surface of a silicon wafer, pressing the amorphous metal and the silicon wafer in a universal material tester, carrying out low-temperature plasma surface treatment on the amorphous metal and so on. According to the preparation method of the super-hydrophobic surface of the amorphous metal provided by the invention, the prepared super-hydrophobic surface of the amorphous metal has higher stability. The super-hydrophobic ability and corrosion characteristics of the surface of the amorphous metal can keep stable within multiple months; furthermore, the prepared surface of the amorphous metal has the characteristics of being water-proof, acid-proof and alkali-proof. The prepared super-hydrophobic surface can be used for soil and rust protection of the surface of the metal, also can be used in pipeline transportation of corrosive liquids and further can be used in non-destructive convey of minim liquids.
Description
Technical field
The invention belongs to the metallic substrate surface process field, be specifically related to a kind of preparation method of amorphous metal super hydrophobic surface.
Background technology
Metal and alloy remain most important structural material so far owing to have favorable conductive, thermal conductivity and mechanical strength performance preferably.Yet common metal and alloy are very easy to be corroded in humidity or corrosive environment, thereby influence the service life of material, cause it normally not play a role, and also bring a lot of unsafe factors to the user.
Corrosion is very huge to the direct losses that metal and alloy material bring.Someone adds up, and about 100,000,000 tons of the annual metal that corrosion is scrapped in the whole world account for 20%～40% of annual production, and along with industrialized process, etching problem is on the rise.The consumption that causes by metal erosion account for that whole industrial products produce 2～3%, China since Corrosion of Metallic Materials every year with a toll of 5,000 hundred million yuans.The massive losses that corrosion brings not only is embodied on the economic loss, and it also can bring the aspects such as development of serious casualties, environmental pollution, the wasting of resources, obstruction new technology.Mention a kind of composite material and manufacturing approach thereof that comprises the infiltrating carbon-based material that improves the surface among the patent CN1760400, have problems such as metal base is restricted, operating procedure is complicated, commercial Application is not extensive.Meanwhile, both at home and abroad to the infiltrating research of amorphous metal, and at amorphous metal surface construction patterning regular array, thereby the research that realizes amorphous metal surface super hydrophobic and automatically cleaning purposes is less relatively.
Summary of the invention
To the problem that exists in the prior art, the present invention provides a kind of preparation method of amorphous metal super hydrophobic surface, realizes anticorrosive metal and self-cleaning effect.The surface coverage skim of the amorphous metal of treated mistake is gathered the film of perfluoroalkyl siloxanes, and the thickness of this film is 30～40nm.That this method has is simple to operate, expend time in less, advantages such as cost is low, good reproducibility.
The present invention proposes a kind of preparation method of amorphous metal super hydrophobic surface, specifically comprises several steps:
(1) processing on amorphous metal surface.With a side surface of amorphous metal successively with the smooth even curface that obtains of No. 400, No. 800, No. 1200 sand papering; For preventing the oxidation and the crystallization on amorphous metal surface; In bruting process, splash into absolute ethyl alcohol and (analyze alcohol; The mass fraction of ethanol >=99.7%), plays lubrication simultaneously.After there is golden colour lustre on the amorphous metal surface, stop polishing, the amorphous metal after the polishing is put into absolute ethyl alcohol, ultrasonic concussion is cleaned more than 2 minutes and is taken out, and dries up subsequent use.
(2) processing of silicon chip surface.The silicon chip template that experiment impression uses is monocrystalline silicon, and thickness 0.3mm～1mm, the specification of silicon chip are that specifications such as 30um * 20um, 30um * 15um, 30um * 10um, 20um * 20um, 20um * 10um (are preferably 20um * 10um); Wherein 20um represents the length of side of uniform array on the silicon chip; 10um represents the spacing between the uniform array on the silicon chip, and the silicon chip template is put into absolute ethyl alcohol, and ultrasonic concussion is cleaned more than 2 minutes; Remove surperficial oil stain, dry up subsequent use.
(3) with the ganoid one side of amorphous metal upwards, one of the regular array of silicon chip faces down and places on the smooth surface of amorphous metal.
(4) resistance-heated furnace is put into universal testing machine, stop heating when resistance-heated furnace is begun to be warming up to 70～130 ℃, the reative cell that the amorphous metal in the step (3) and silicon chip are put into resistance-heated furnace; Keep silicon chip to place on the smooth surface of amorphous metal; Regulate the universal testing machine parameter, selecting control model is displacement control, and speed is 0.01～0.5mm/min; Maintenance stage control model is a Load Control; Keeping the beginning standard is compression stress, and the compression stress retention value is that 10～100Mpa impresses, and it is to stop heating behind 10～100Mpa that stress to be compressed reaches the compression stress retention value.Impression finishes the back for guaranteeing the impression effect, and pressurize was taken out after 1～2 minute.
(5) the amorphous metal surface behind the impression has micron-sized ordered array, for guaranteeing to reach super-hydrophobic experiment effect, amorphous metal is put into the absolute ethyl alcohol sonic oscillation more than 2 minutes, removes the oil stain on amorphous metal surface.
(6) reative cell of will the amorphous metal after above-mentioned steps is handled putting into low temperature plasma surface treatment appearance; It is 9～20pa that a parameter back of the body end vacuum is set; Parameter one tunnel air inflow 10～1000 standard ml/min are set one time; 10～100 a seconds parameter stability time, 100～300 watts of parameter high frequency powers, 10～1000 seconds discharge time of parameter; Two times parameter back of the body end vacuum 8～20pa; Two times parameter one tunnel air inflow 0 standard ml/min; Two times 10～100 seconds parameter stability times; 100～300 watts of two times parameter high frequency powers, two times 10～1000 seconds discharge times of parameter, light extinguishes to sound a buzzer and represent the processing procedure end in the reative cell of daughter surface treatment appearance such as low temperature by the time.
(7) take out through plasma treated amorphous metal, put into the mixed solution that gathers perfluoroalkyl siloxanes-ethanol and soak more than 24 hours.Wherein, gathering the mass fraction that gathers the perfluoroalkyl siloxanes in the mixed solution of perfluoroalkyl siloxanes-ethanol is 1%～5%.
(8) will pass through the amorphous metal that step (7) handled washes more than 4～5 times with absolute ethyl alcohol repeatedly; Put into 80 ℃～110 ℃ dry 1～4 hour of baking oven; Obtain the film of surface coverage one strata perfluoroalkyl siloxanes; This film thickness is 30～40nm, promptly obtains amorphous metal super hydrophobic surface of the present invention, realizes the preparation of amorphous metal super hydrophobic surface.
The advantage that the present invention has is:
1, the preparation method of a kind of amorphous metal super hydrophobic surface of the present invention's proposition, the super-hydrophobic amorphous metal surface of preparation has advantages of higher stability.Super-hydrophobic, the anti-corrosion property on amorphous metal surface still can keep stable in the several months.
2, the preparation method of a kind of amorphous metal super hydrophobic surface of the present invention's proposition; The amorphous metal surface of preparation has the characteristic that does not get wet, is not stained with acid and is not stained with alkali; Can be used for the antifouling and antirust of metal surface; Can also also can be used for the conveying of harmless micro liquid as the pipeline transportation of corrosive liquids.
3, the preparation method of a kind of amorphous metal super hydrophobic surface of the present invention's proposition, the amorphous metal super hydrophobic surface of preparation can be used on the needle point of microsyringe, can eliminate the adhesion of liquid sample to needle point, can be widely used in places such as hospital, laboratory.
4, the preparation method of a kind of amorphous metal super hydrophobic surface of proposing of the present invention is used for the housing of water means of transport, can effectively reduce the resistance of water, improves headway and reduces energy resource consumption.
5, the preparation method of a kind of amorphous metal super hydrophobic surface of the present invention's proposition, method of operating is simple, and the consumption amount of reagent is few; Productive rate is high; Cost consumption is low, has environmental protection and environment amenable characteristics, and good reproducibility; Can be applicable to many industries such as industry, agricultural, scientific research, hospital, especially be widely used in having self-cleaning function surfacing field.
Description of drawings
Fig. 1: the present invention proposes a kind of preparation method's of amorphous metal super hydrophobic surface flow chart;
Fig. 2: experiment is with the stereoscan photograph of silicon chip among the present invention;
Fig. 3: the metallograph of 400 times silicon chip is amplified in experiment among the present invention with silicon chip;
Fig. 4: the electromicroscopic photograph of impression back cerium Base Metal amorphous among the present invention;
Fig. 5: the stereoscan photograph of impression back cerium Base Metal amorphous section among the present invention;
Fig. 6: the metallograph of 400 times cerium Base Metal amorphous is amplified in the impression back among the present invention;
Fig. 7: the contact angle sketch map of common cerium Base Metal amorphous;
Fig. 8: the contact angle sketch map of using the cerium Base Metal amorphous after the present invention handles.
The specific embodiment
The preparation method who comes to explain particularly a kind of amorphous metal super hydrophobic surface of the present invention below in conjunction with accompanying drawing and embodiment.
The present invention proposes a kind of preparation method of amorphous metal super hydrophobic surface, and is as shown in Figure 1, specifically comprises several steps:
(1) processing on amorphous metal surface.With a side surface of amorphous metal successively with the smooth even curface that obtains of No. 400, No. 800, No. 1200 sand papering; For preventing the oxidation and the crystallization on amorphous metal surface; In bruting process, splash into absolute ethyl alcohol and (analyze alcohol; The mass fraction of ethanol >=99.7%), plays lubrication simultaneously.After there is golden colour lustre on the amorphous metal surface, stop polishing, the amorphous metal after the polishing is put into absolute ethyl alcohol, ultrasonic concussion is cleaned more than 2 minutes and is taken out, and dries up subsequent use.
(2) processing of silicon chip surface.The silicon chip template that the experiment impression uses is monocrystalline silicon, and thickness 0.3mm～1mm is preferably 0.5mm; The specification of silicon chip is specifications such as 30um * 20um, 30um * 15um, 30um * 10um, 20um * 20um, 20um * 10um, is preferably 20um * 10um, and wherein 20um represents the length of side of uniform array on the silicon chip; 10um represents the spacing between the uniform array on the silicon chip; As shown in Figures 2 and 3, the silicon chip template is put into absolute ethyl alcohol, ultrasonic concussion is cleaned more than 2 minutes; Remove surperficial oil stain, dry up subsequent use.
(3) with the ganoid one side of amorphous metal upwards, one of the regular array of silicon chip faces down and places on the smooth surface of amorphous metal.
(4) resistance-heated furnace is put into universal testing machine, resistance-heated furnace is begun to be warming up to 70～130 ℃, stop heating when being preferably 120 ℃; With the reative cell that the amorphous metal in the step (3) and silicon chip are put into resistance-heated furnace, keep silicon chip to place on the smooth surface of amorphous metal, regulate the universal testing machine parameter; Selecting control model is displacement control, and speed is 0.01～0.5mm/min, is preferably 0.186mm/min; Maintenance stage control model is a Load Control; Keeping the beginning standard is compression stress, and the compression stress retention value is 10～100Mpa, is preferably 30Mpa and impresses; It is 10～100Mpa that stress to be compressed reaches the compression stress retention value, is preferably to stop heating behind the 30Mpa.Impression finishes the back for guaranteeing the impression effect, and pressurize was taken out after 1～2 minute.
(5) the amorphous metal surface behind the impression has micron-sized ordered array, like Fig. 4, Fig. 5, shown in Figure 6, for guaranteeing to reach super-hydrophobic experiment effect, amorphous metal is put into the absolute ethyl alcohol sonic oscillation more than 2 minutes, removes the oil stain on amorphous metal surface.
(6) reative cell of will the amorphous metal after above-mentioned steps is handled putting into low temperature plasma surface treatment appearance, it is 9～20pa that a parameter back of the body end vacuum is set, and is preferably 10pa; Parameter one tunnel air inflow 10～1000 standard ml/min are set one time, are preferably 100 standard ml/min, 10～100 a seconds parameter stability time; Be preferably 20 seconds, 100～300 watts of parameter high frequency powers are preferably 200 watts; 10～1000 seconds discharge time of parameter, be preferably 600 seconds; Two times parameter back of the body end vacuum 8～20pa are preferably 8pa, two times parameter one tunnel air inflow 0 standard ml/min; Two times 10～100 seconds parameter stability times are preferably 15 seconds, 100～300 watts of two times parameter high frequency powers; Preferred 180 watts, two times 10～1000 seconds discharge times of parameter, preferred 40 seconds; By the time light extinguishes instrument and sends buzzing in the reative cell of daughter surface treatment appearance such as low temperature, and processing procedure finishes.
(7) take out through plasma treated amorphous metal, put into the mixed solution that gathers perfluoroalkyl siloxanes-ethanol and soak more than 24 hours.Wherein, gathering the mass fraction that gathers the perfluoroalkyl siloxanes in the mixed solution of perfluoroalkyl siloxanes-ethanol is 1%～5% (preferred 5%).
(8) will pass through the amorphous metal that step 7 handled washes more than 4～5 times with absolute ethyl alcohol repeatedly; Put into dry 1～4 hour (being preferably 2 hours) of baking oven of 80 ℃～110 ℃ (preferred 90 ℃); Obtain the film of surface coverage one strata perfluoroalkyl siloxanes; This film thickness is 30～40nm, promptly obtains super-hydrophobic amorphous metal of the present invention surface.The contact angle that contact angle measurement is measured this amorphous metal surface is 150 °～155 °, and is as shown in Figure 8, with the contact angle (CA) 40 °～90 ° (its contact angle size is 84 °, like Fig. 7) of common amorphous metal bigger difference arranged.Super hydrophobic surface is meant and the contact angle of the water surface greater than 150 °.
The preparation method of a kind of amorphous metal super hydrophobic surface that the present invention proposes for cerium base, rare earth based at the bottom of, the amorphous metal of substrates such as magnesium base, palladium base, platinum base or zirconium base all is suitable for.
Embodiment 1:
Present embodiment is the preparation method of cerium Base Metal amorphous super hydrophobic surface, specifically comprises several steps:
(1) processing of cerium Base Metal amorphous surfaces.(constituent is Ce with a side surface of cerium Base Metal amorphous
69Al
10Cu
20Co
1) successively with the smooth even curface that obtains of No. 400, No. 800, No. 1200 sand papering; For preventing the oxidation and the crystallization of cerium Base Metal amorphous surfaces; In bruting process, splash into absolute ethyl alcohol (analyzing alcohol, the mass fraction of ethanol>=99.7%), play lubrication simultaneously.After cerium Base Metal amorphous surfaces has golden colour lustre, stop polishing, the cerium Base Metal amorphous after the polishing is put into absolute ethyl alcohol, ultrasonic concussion is cleaned and was taken out in 2 minutes, dries up subsequent use.
(2) processing of silicon chip surface.The silicon chip template that the experiment impression uses is monocrystalline silicon, and thickness 0.3mm, the specification of silicon chip are 20um * 10um; As shown in Figures 2 and 3, wherein 20um represents the length of side of uniform array on the silicon chip, and 10um represents the spacing between the uniform array on the silicon chip; The silicon chip template is put into absolute ethyl alcohol; Ultrasonic concussion was cleaned 2 minutes, removed surperficial oil stain, dried up subsequent use.
(3) cerium Base Metal amorphous surfaces is smooth one side makes progress, and one of the regular array of silicon chip faces down and places on the smooth surface of cerium Base Metal amorphous.
(4) resistance-heated furnace is put into universal testing machine, stop heating when resistance-heated furnace is begun to be warming up to 120 ℃, the reative cell that the cerium Base Metal amorphous in the step (3) and silicon chip are put into resistance-heated furnace; Keep silicon chip to place on the smooth surface of cerium Base Metal amorphous; Regulate the universal testing machine parameter, selecting control model is displacement control, and speed is 0.186mm/min; Maintenance stage control model is a Load Control; Keeping the beginning standard is compression stress, and the compression stress retention value is that 30Mpa impresses, and it is to stop heating behind the 30Mpa that stress to be compressed reaches the compression stress retention value.Impression finishes the back for guaranteeing the impression effect, and pressurize was taken out after 1 minute.
(5) the cerium Base Metal amorphous surfaces behind the impression has micron-sized ordered array; Like Fig. 4, Fig. 5 and shown in Figure 6; For guaranteeing to reach super-hydrophobic experiment effect, cerium Base Metal amorphous was put into the absolute ethyl alcohol sonic oscillation 2 minutes, remove the oil stain of cerium Base Metal amorphous surfaces.
(6) reative cell of will the cerium Base Metal amorphous after above-mentioned steps is handled putting into low temperature plasma surface treatment appearance; It is 9pa that a parameter back of the body end vacuum is set; Parameter one tunnel air inflow 10 standard ml/min are set one time; A 10 seconds parameter stability time, 100 watts of parameter high frequency powers, 10 seconds discharge time of parameter; Two times parameter back of the body end vacuum 8pa; Two times parameter one tunnel air inflow 0 standard ml/min, two times 10 seconds parameter stability times, 100 watts of two times parameter high frequency powers; Two times 10 seconds discharge times of parameter, light extinguishes and represent the processing procedure end in the reative cell of daughter surface treatment appearance such as low temperature by the time.
(7) take out through plasma treated cerium Base Metal amorphous, put into the mixed solution that gathers perfluoroalkyl siloxanes-ethanol and soaked 24 hours.Wherein, gathering the mass fraction that gathers the perfluoroalkyl siloxanes in the mixed solution of perfluoroalkyl siloxanes-ethanol is 1%.
(8) will pass through the cerium Base Metal amorphous that step 7 handled washes 4 times with absolute ethyl alcohol repeatedly; Put into 80 ℃ dry 1 hour of baking oven; Obtain the film of surface coverage one strata perfluoroalkyl siloxanes, this film thickness is 30nm, promptly obtains the cerium Base Metal amorphous super hydrophobic surface of present embodiment.The contact angle that contact angle measurement is measured this amorphous metal surface is 151 °, and is as shown in Figure 8.
Embodiment 2:
Present embodiment proposes a kind of preparation method of cerium Base Metal amorphous super hydrophobic surface, comprises following step:
(1) processing of cerium Base Metal amorphous surfaces.(constituent is Ce with a side surface of cerium Base Metal amorphous
69Al
10Cu
20Co
1) successively with the smooth even curface that obtains of No. 400, No. 800, No. 1200 sand papering; For preventing the oxidation and the crystallization of cerium Base Metal amorphous surfaces; In bruting process, splash into absolute ethyl alcohol (analyzing alcohol, the mass fraction of ethanol>=99.7%), play lubrication simultaneously.After there is golden colour lustre on the amorphous metal surface, stop polishing, the cerium Base Metal amorphous after the polishing is put into absolute ethyl alcohol, ultrasonic concussion is cleaned and was taken out in 5 minutes, dries up subsequent use.
(2) processing of silicon chip surface.The silicon chip template that the experiment impression uses is monocrystalline silicon, and thickness 1mm, the specification of silicon chip are 30um * 15um; Wherein 30um represents the length of side of uniform array on the silicon chip; 15um represents the spacing between the uniform array on the silicon chip, and the silicon chip template is put into absolute ethyl alcohol, and ultrasonic concussion was cleaned 5 minutes; Remove surperficial oil stain, dry up subsequent use.
(3) cerium Base Metal amorphous surfaces is smooth one side makes progress, and one of the regular array of silicon chip faces down and places on the smooth surface of amorphous metal.
(4) resistance-heated furnace is put into universal testing machine, stop heating when resistance-heated furnace is begun to be warming up to 130 ℃, the reative cell that the cerium Base Metal amorphous in the step (3) and silicon chip are put into resistance-heated furnace; Keep silicon chip to place on the smooth surface of cerium Base Metal amorphous; Regulate the universal testing machine parameter, selecting control model is displacement control, and speed is 0.50mm/min; Maintenance stage control model is a Load Control; Keeping the beginning standard is compression stress, and the compression stress retention value is that 10Mpa impresses, and it is to stop heating behind the 10Mpa that stress to be compressed reaches the compression stress retention value.Impression finishes the back for guaranteeing the impression effect, and pressurize was taken out after 2 minutes.
(5) the cerium Base Metal amorphous surfaces behind the impression has micron-sized ordered array, for guaranteeing to reach super-hydrophobic experiment effect, cerium Base Metal amorphous is put into the absolute ethyl alcohol sonic oscillation 5 minutes, removes the oil stain of cerium Base Metal amorphous surfaces.
(6) reative cell of will the cerium Base Metal amorphous after above-mentioned steps is handled putting into low temperature plasma surface treatment appearance; It is 20pa that a parameter back of the body end vacuum is set; Parameter one tunnel air inflow 1000 standard ml/min are set one time; A 100 seconds parameter stability time, 300 watts of parameter high frequency powers, 1000 seconds discharge time of parameter; Two times parameter back of the body end vacuum 20pa; Two times parameter one tunnel air inflow 0 standard ml/min; Two times 100 seconds parameter stability times; 300 watts of two times parameter high frequency powers, two times 1000 seconds discharge times of parameter, light extinguishes and represent the processing procedure end in the reative cell of daughter surface treatment appearance such as low temperature by the time.
(7) take out through plasma treated cerium Base Metal amorphous, put into the mixed solution that gathers perfluoroalkyl siloxanes-ethanol and soaked 30 hours.Wherein, gathering the mass fraction that gathers the perfluoroalkyl siloxanes in the mixed solution of perfluoroalkyl siloxanes-ethanol is 5%.
(8) will pass through the cerium Base Metal amorphous that step 7 handled washes 5 times with absolute ethyl alcohol repeatedly; Put into 110 ℃ dry 4 hours of baking oven; Obtain the film of surface coverage one strata perfluoroalkyl siloxanes, this film thickness is 40nm, promptly obtains the cerium Base Metal amorphous super hydrophobic surface of present embodiment.
Embodiment 3:
Present embodiment proposes a kind of preparation method of cerium Base Metal amorphous super hydrophobic surface, specifically comprises several steps:
(1) processing of cerium Base Metal amorphous surfaces.With a side surface of cerium Base Metal amorphous successively with the smooth even curface that obtains of No. 400, No. 800, No. 1200 sand papering; For preventing the oxidation and the crystallization of cerium Base Metal amorphous surfaces; In bruting process, splash into absolute ethyl alcohol and (analyze alcohol; The mass fraction of ethanol >=99.7%), plays lubrication simultaneously.After cerium Base Metal amorphous surfaces has golden colour lustre, stop polishing, the cerium Base Metal amorphous after the polishing is put into absolute ethyl alcohol, ultrasonic concussion is cleaned and was taken out in 10 minutes, dries up subsequent use.
(2) processing of silicon chip surface.The silicon chip template that the experiment impression uses is monocrystalline silicon, and thickness 0.5mm, the specification of silicon chip are 30um * 10um; Wherein 30um represents the length of side of uniform array on the silicon chip; 10um represents the spacing between the uniform array on the silicon chip, and the silicon chip template is put into absolute ethyl alcohol, and ultrasonic concussion was cleaned 10 minutes; Remove surperficial oil stain, dry up subsequent use.
(3) cerium Base Metal amorphous surfaces is smooth one side makes progress, and one of the regular array of silicon chip faces down and places on the smooth surface of cerium Base Metal amorphous.
(4) resistance-heated furnace is put into universal testing machine, stop heating when resistance-heated furnace is begun to be warming up to 70 ℃, the reative cell that the cerium Base Metal amorphous in the step (3) and silicon chip are put into resistance-heated furnace; Keep silicon chip to place on the smooth surface of cerium Base Metal amorphous; Regulate the universal testing machine parameter, selecting control model is displacement control, and speed is 0.01mm/min; Maintenance stage control model is a Load Control; Keeping the beginning standard is compression stress, and the compression stress retention value is that 100Mpa impresses, and it is to stop heating behind the 100Mpa that stress to be compressed reaches the compression stress retention value.Impression finishes the back for guaranteeing the impression effect, and pressurize was taken out after 1.5 minutes.
(5) the cerium Base Metal amorphous surfaces behind the impression has micron-sized ordered array, for guaranteeing to reach super-hydrophobic experiment effect, cerium Base Metal amorphous is put into the absolute ethyl alcohol sonic oscillation 10 minutes, removes the oil stain of cerium Base Metal amorphous surfaces.
(6) reative cell of will the cerium Base Metal amorphous after above-mentioned steps is handled putting into low temperature plasma surface treatment appearance; It is 10pa that a parameter back of the body end vacuum is set; Parameter one tunnel air inflow 100 standard ml/min are set one time; A 20 seconds parameter stability time, 200 watts of parameter high frequency powers, 600 seconds discharge time of parameter; Two times parameter back of the body end vacuum 18pa; Two times parameter road air inflow 0 standard ml/min, two times 15 seconds parameter stability times, 180 watts of two times parameter high frequency powers; Two times 40 seconds discharge times of parameter, light extinguishes and represent the processing procedure end in the reative cell of daughter surface treatment appearance such as low temperature by the time.
(7) take out through plasma treated cerium Base Metal amorphous, put into the mixed solution that gathers perfluoroalkyl siloxanes-ethanol and soak more than 36 hours.Wherein, gathering the mass fraction that gathers the perfluoroalkyl siloxanes in the mixed solution of perfluoroalkyl siloxanes-ethanol is 2%.
(8) will pass through the cerium Base Metal amorphous that step 7 handled washes 6 times with absolute ethyl alcohol repeatedly; Put into 90 ℃ dry 2 hours of baking oven; Obtain the film of surface coverage one strata perfluoroalkyl siloxanes, this film thickness is 35nm, obtains cerium Base Metal amorphous super hydrophobic surface.
Embodiment 4:
Present embodiment proposes a kind of preparation method of cerium Base Metal amorphous super hydrophobic surface, specifically comprises several steps:
(1) processing of cerium Base Metal amorphous surfaces.With a side surface of cerium Base Metal amorphous successively with the smooth even curface that obtains of No. 400, No. 800, No. 1200 sand papering; For preventing the oxidation and the crystallization of cerium Base Metal amorphous surfaces; In bruting process, splash into absolute ethyl alcohol and (analyze alcohol; The mass fraction of ethanol >=99.7%), plays lubrication simultaneously.After cerium Base Metal amorphous surfaces has golden colour lustre, stop polishing, the cerium Base Metal amorphous after the polishing is put into absolute ethyl alcohol, ultrasonic concussion is cleaned and was taken out in 6 minutes, dries up subsequent use.
(2) processing of silicon chip surface.The silicon chip template that the experiment impression uses is monocrystalline silicon, and thickness 0.8mm, the specification of silicon chip are 30um * 20um; Wherein 30um represents the length of side of uniform array on the silicon chip; 20um represents the spacing between the uniform array on the silicon chip, and the silicon chip template is put into absolute ethyl alcohol, and ultrasonic concussion was cleaned 8 minutes; Remove surperficial oil stain, dry up subsequent use.
(3) cerium Base Metal amorphous surfaces is smooth one side makes progress, and one of the regular array of silicon chip faces down and places on the smooth surface of cerium Base Metal amorphous.
(4) resistance-heated furnace is put into universal testing machine, stop heating when resistance-heated furnace is begun to be warming up to 80 ℃, the reative cell that the amorphous metal in the step (3) and silicon chip are put into resistance-heated furnace; Keep silicon chip to place on the smooth surface of amorphous metal; Regulate the universal testing machine parameter, selecting control model is displacement control, and speed is 0.20mm/min; Maintenance stage control model is a Load Control; Keeping the beginning standard is compression stress, and the compression stress retention value is that 50Mpa impresses, and it is to stop heating behind the 50Mpa that stress to be compressed reaches the compression stress retention value.Impression finishes the back for guaranteeing the impression effect, and pressurize was taken out after 1 minute.
(5) the cerium Base Metal amorphous surfaces behind the impression has micron-sized ordered array, for guaranteeing to reach super-hydrophobic experiment effect, amorphous metal is put into the absolute ethyl alcohol sonic oscillation 3 minutes, removes the oil stain of cerium Base Metal amorphous surfaces.
(6) reative cell of will the cerium Base Metal amorphous after above-mentioned steps is handled putting into low temperature plasma surface treatment appearance; It is 15pa that a parameter back of the body end vacuum is set; Parameter one tunnel air inflow 500 standard ml/min are set one time; A 50 seconds parameter stability time, 150 watts of parameter high frequency powers, 100 seconds discharge time of parameter; Two times parameter back of the body end vacuum 10pa; Two times parameter one tunnel air inflow 0 standard ml/min; Two times 50 seconds parameter stability times; 110 watts of two times parameter high frequency powers, two times 100 seconds discharge times of parameter, light extinguishes and represent the processing procedure end in the reative cell of daughter surface treatment appearance such as low temperature by the time.
(7) take out through plasma treated cerium Base Metal amorphous, put into the mixed solution that gathers perfluoroalkyl siloxanes-ethanol and soak more than 24 hours.Wherein, gathering the mass fraction that gathers the perfluoroalkyl siloxanes in the mixed solution of perfluoroalkyl siloxanes-ethanol is 3%.
(8) will pass through the cerium Base Metal amorphous that step 7 handled washes 7 times with absolute ethyl alcohol repeatedly; Put into 100 ℃ dry 3 hours of baking oven; Obtain the film of surface coverage one strata perfluoroalkyl siloxanes, this film thickness is 38nm, obtains the cerium Base Metal amorphous super hydrophobic surface of present embodiment.
Embodiment 5:
Present embodiment proposes a kind of preparation method of cerium Base Metal amorphous super hydrophobic surface, specifically comprises several steps:
(1) processing of cerium Base Metal amorphous surfaces.With a side surface of cerium Base Metal amorphous successively with the smooth even curface that obtains of No. 400, No. 800, No. 1200 sand papering; For preventing the oxidation and the crystallization of cerium Base Metal amorphous surfaces; In bruting process, splash into absolute ethyl alcohol and (analyze alcohol; The mass fraction of ethanol >=99.7%), plays lubrication simultaneously.After cerium Base Metal amorphous surfaces has golden colour lustre, stop polishing, the cerium Base Metal amorphous after the polishing is put into absolute ethyl alcohol, ultrasonic concussion is cleaned and was taken out in 8 minutes, dries up subsequent use.
(2) processing of silicon chip surface.The silicon chip template that the experiment impression uses is monocrystalline silicon, and thickness 0.9mm, the specification of silicon chip are 20um * 20um; Wherein 20um represents the length of side of uniform array on the silicon chip; 20um represents the spacing between the uniform array on the silicon chip, and the silicon chip template is put into absolute ethyl alcohol, and ultrasonic concussion was cleaned 10 minutes; Remove surperficial oil stain, dry up subsequent use.
(3) cerium Base Metal amorphous surfaces is smooth one side makes progress, and one of the regular array of silicon chip faces down and places on the smooth surface of cerium Base Metal amorphous.
(4) resistance-heated furnace is put into universal testing machine, stop heating when resistance-heated furnace is begun to be warming up to 100 ℃, the reative cell that the cerium Base Metal amorphous in the step (3) and silicon chip are put into resistance-heated furnace; Keep silicon chip to place on the smooth surface of cerium Base Metal amorphous; Regulate the universal testing machine parameter, selecting control model is displacement control, and speed is 0.40mm/min; Maintenance stage control model is a Load Control; Keeping the beginning standard is compression stress, and the compression stress retention value is that 100Mpa impresses, and it is to stop heating behind the 10Mpa that stress to be compressed reaches the compression stress retention value.Impression finishes the back for guaranteeing the impression effect, and pressurize was taken out after 1 minute.
(5) the cerium Base Metal amorphous surfaces behind the impression has micron-sized ordered array, for guaranteeing to reach super-hydrophobic experiment effect, cerium Base Metal amorphous is put into the absolute ethyl alcohol sonic oscillation 2 minutes, removes the oil stain on amorphous metal surface.
(6) reative cell of will the cerium Base Metal amorphous after above-mentioned steps is handled putting into low temperature plasma surface treatment appearance; It is 18pa that a parameter back of the body end vacuum is set; Parameter one tunnel air inflow 800 standard ml/min are set one time; A 80 seconds parameter stability time, 250 watts of parameter high frequency powers, 800 seconds discharge time of parameter; Two times parameter back of the body end vacuum 16pa; Two times parameter one tunnel air inflow 0 standard ml/min; Two times 80 seconds parameter stability times; 250 watts of two times parameter high frequency powers, two times 500 seconds discharge times of parameter, light extinguishes and represent the processing procedure end in the reative cell of daughter surface treatment appearance such as low temperature by the time.
(7) take out through plasma treated cerium Base Metal amorphous, put into the mixed solution that gathers perfluoroalkyl siloxanes-ethanol and soak more than 24 hours.Wherein, gathering the mass fraction that gathers the perfluoroalkyl siloxanes in the mixed solution of perfluoroalkyl siloxanes-ethanol is 4%.
(8) will pass through the cerium Base Metal amorphous that step 7 handled washes 4 times with absolute ethyl alcohol repeatedly; Put into 105 ℃ dry 3 hours of baking oven; Obtain the film of surface coverage one strata perfluoroalkyl siloxanes, this film thickness is 40nm, obtains the cerium Base Metal amorphous super hydrophobic surface of present embodiment.
Embodiment 6:
Present embodiment proposes a kind of preparation method of amorphous metal super hydrophobic surface and the difference of embodiment 1 only is the material of the amorphous metal in the step 1 is replaced by rare-earth based alloy La by cerium Base Metal amorphous
55Al
25Ni
20, other each steps and embodiment 1 are identical.
Embodiment 7:
The difference that present embodiment proposes a kind of preparation method and embodiment 1 of amorphous metal super hydrophobic surface only is that the material of the amorphous metal in the step 1 is replaced by the magnesium-base metal amorphous by cerium Base Metal amorphous, and (constituent is Mg
65Cu
25Gd
10), other each steps and embodiment 1 are identical.
Embodiment 8:
The difference that present embodiment proposes a kind of preparation method and embodiment 1 of amorphous metal super hydrophobic surface only is that the material of the amorphous metal in the step 1 is replaced by the palladium-based metal amorphous by cerium Base Metal amorphous, and (constituent is Pd
40Cu
30P
20Ni
10), other each steps and embodiment 1 are identical.
Embodiment 9:
The difference that present embodiment proposes a kind of preparation method and embodiment 1 of amorphous metal super hydrophobic surface only is that the material of the amorphous metal in the step 1 is replaced by platinum Base Metal amorphous by cerium Base Metal amorphous, and (constituent is Pt
57.5Cu
14.7Ni
5.3P
22.5), other each steps and embodiment 1 are identical.
Embodiment 10:
The difference that present embodiment proposes a kind of preparation method and embodiment 1 of amorphous metal super hydrophobic surface only is that the material of the amorphous metal in the step 1 is replaced by the zirconium-based metallic amorphous by cerium Base Metal amorphous, and (constituent is Zr
41.2Ti
13.8Cu
12.5Ni
10Be
22.5), other each steps and embodiment 1 are identical.
Claims (7)
1. the preparation method of an amorphous metal super hydrophobic surface is characterized in that: specifically comprise several steps:
(1) processing on amorphous metal surface: with a side surface of the amorphous metal smooth even curface that obtains of sand papering successively, in bruting process, splash into absolute ethyl alcohol, the amorphous metal after the polishing is put into absolute ethyl alcohol, dry up subsequent use after ultrasonic concussion is cleaned;
(2) processing of silicon chip surface: will test with the silicon chip template and put into absolute ethyl alcohol, ultrasonic concussion was cleaned more than 2 minutes, removed surperficial oil stain, dried up subsequent use;
(3) with the ganoid one side of amorphous metal upwards, one of the regular array of silicon chip faces down and places on the smooth surface of amorphous metal;
(4) resistance-heated furnace is put into universal testing machine, resistance-heated furnace is begun to heat up, stop heating during to 70～130 ℃; With the reative cell that the amorphous metal in the step (3) and silicon chip are put into resistance-heated furnace, keep silicon chip to place on the smooth surface of amorphous metal, regulate the universal testing machine parameter; Selecting control model is displacement control, 0.01～0.50mm/min, and keeping the stage control model is Load Control; Keeping the beginning standard is compression stress; The compression stress retention value is that 10～100Mpa impresses, and it is to stop heating behind 10～100Mpa that stress to be compressed reaches the compression stress retention value, and pressurize was taken out after 1～2 minute;
(5) will impress the back amorphous metal and put into the absolute ethyl alcohol sonic oscillation more than 2 minutes;
(6) amorphous metal is put into the reative cell of low temperature plasma surface treatment appearance; It is 9～20pa that a parameter back of the body end vacuum is set; Parameter one tunnel air inflow 10～1000 standard ml/min are set one time; 10～100 a seconds parameter stability time, 100～300 watts of parameter high frequency powers, 10～1000 seconds discharge time of parameter; Two times parameter back of the body end vacuum 8～20pa; Two times parameter one tunnel air inflow 0 standard ml/min; Two times 10～100 seconds parameter stability times, 100～300 watts of two times parameter high frequency powers, two times 10～1000 seconds discharge times of parameter; Treat that light extinguishes in the reative cell of daughter surface treatment appearance such as low temperature, processing procedure finishes;
(7) take out through plasma treated amorphous metal, put into and gather perfluoroalkyl siloxanes-alcohol mixed solution and soak more than 24 hours;
(8) will pass through the amorphous metal that step (7) handled washes more than 4～5 times with absolute ethyl alcohol repeatedly; After putting into 80 ℃～110 ℃ baking oven drying; Obtain the film of surface coverage one strata perfluoroalkyl siloxanes; Obtain the amorphous metal super hydrophobic surface, realize the preparation of amorphous metal super hydrophobic surface.
2. the preparation method of a kind of amorphous metal super hydrophobic surface according to claim 1; It is characterized in that: the silicon chip in the described step (2) is a monocrystalline silicon; Thickness 0.3mm～1mm; The specification of silicon chip is 20um * 10um, and 20um is the length of side of uniform array on the silicon chip, and 10um is the spacing between the uniform array on the silicon chip.
3. the preparation method of a kind of amorphous metal super hydrophobic surface according to claim 1 is characterized in that: gathering the mass fraction that gathers the perfluoroalkyl siloxanes in perfluoroalkyl siloxanes-alcohol mixed solution in the described step (7) is 1%～5%.
4. the preparation method of a kind of amorphous metal super hydrophobic surface according to claim 1 is characterized in that: described step (4) medium velocity is 0.186mm/min, and the compression stress retention value is 30Mpa.
5. the preparation method of a kind of amorphous metal super hydrophobic surface according to claim 1; It is characterized in that: it is 10Mpa that a parameter back of the body end vacuum is set in the described step (6); Parameter one tunnel air inflow 100 standard ml/min are set one time; A 20 seconds parameter stability time, 200 watts of parameter high frequency powers, 600 seconds discharge time of parameter; Two times parameters back of the body end vacuum 8Mpa, two times parameter one tunnel air inflow 0 standard ml/min, two times 15 seconds parameter stability times, 180 watts of two times parameter high frequency powers, two times 40 seconds discharge times of parameter.
6. the preparation method of a kind of amorphous metal super hydrophobic surface according to claim 1 is characterized in that: at the bottom of described amorphous metal is cerium base, rare earth based, the amorphous metal of magnesium base, palladium base, platinum base or the substrate of zirconium base.
7. the preparation method of a kind of amorphous metal super hydrophobic surface according to claim 6 is characterized in that: described cerium Base Metal amorphous is Ce
69A1
10Cu
20Co
1, rare-earth based alloy is La
55Al
25Ni
20, the magnesium-base metal amorphous is Mg
65Cu
25Gd
10, the palladium-based metal amorphous is Pd
40Cu
30P
20Ni
10, platinum Base Metal amorphous is Pt
57.5Cu
14.7Ni
5.3P
22.5, the zirconium-based metallic amorphous is Zr
41.2Ti
13.8Cu
12.5Ni
10Be
22.5
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| CN110560888B (en) * | 2019-10-23 | 2020-07-10 | 山东大学 | Method for roughening and functionalizing surface of metal material by utilizing laser shock forming technology and application thereof |
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