CN106929856A - A kind of method that hf etching changes metallic nickel surface wettability - Google Patents
A kind of method that hf etching changes metallic nickel surface wettability Download PDFInfo
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- CN106929856A CN106929856A CN201710220630.3A CN201710220630A CN106929856A CN 106929856 A CN106929856 A CN 106929856A CN 201710220630 A CN201710220630 A CN 201710220630A CN 106929856 A CN106929856 A CN 106929856A
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- metal nickel
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- C—CHEMISTRY; METALLURGY
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
-
- C—CHEMISTRY; METALLURGY
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
-
- C—CHEMISTRY; METALLURGY
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The present invention discloses a kind of method that hf etching changes metallic nickel surface wettability, including：(1) metal nickel surface is cleaned using ultrasonic cleaning mode, by the greasy dirt and Impurity removal on metal nickel sheet surface；(2) metal nickel sheet is placed in >=40% hydrofluoric acid solution in, chemical etching is then carried out in more than 30 DEG C of water-bath, etch period is 7~28h, and in etching process, a metal nickel sheet surface is overturn every 1h；(3) the metal nickel sheet after etching is taken out and rinses drying, obtain the metal nickel sheet after changing wet performance.The present invention performs etching treatment by hydrofluoric acid solution to metal nickel surface, coarse microstructure is formed in metal nickel surface, so as to change the wettability of metallic nickel only by way of improving surface roughness, it is improved the hydrophobicity of metal nickel surface, and then the service life under effectively extending metallic nickel in humidity or containing water vapor conditions, widen the range of application of nickel.
Description
Technical field
The present invention relates to it is a kind of change metallic nickel surface wettability method, and in particular to be a kind of hf etching
The method for changing metallic nickel surface wettability.
Background technology
The wettability of material surface, is one of intrinsic property of material.So-called moistening is exactly exist less on the surface of solid
Perhaps during liquid, new solid-liquid interface for producing instead of before gas-liquid/solid interface phenomenon.Wettability of the surface is generally divided into two
Kind：Hydrophily and hydrophobicity.Hydrophily refers to that material has affinity to water, general inoganic solids, metal and its oxide
Deng its surface tension is all larger, frequently referred to high-energy solid surface, is easily soaked by liquid, with significant hydrophily.Hydrophobicity is
Refer to that material has repulsive interaction to water, the general material with low-surface-energy, such as fluoride etc., all with significant hydrophobic
Property；Hydrophobic or even super hydrophobic surface, because it is in sides such as self-cleaning surface, anticorrosive, Drag Reduction and the lossless conveyings of microfluid
The potential using value in face and receive much concern.
Material surface hydrophobically modified, typically all uses two kinds of approach：1) low-surface energy substance modification of surfaces is used, in metal
Surface forms a hydrophobic coating, organic molecule, high polymer generally using some low-surface-energies or containing hydrophobic grouping etc.；2)
Change the microstructure on surface, surface roughness is improved, so as to improve the hydrophobicity on surface；Certainly, under the conditions of some, also have by
Above two method combines the hydrophobicity for improving material.
In metal material surface wetting Journal of Sex Research, hydrophobic surface is just prepared for metal without low-surface-energy modification
Using important in inhibiting；Because under certain conditions, it is undesirable that introduce organic matter, and some organic matters also bring along
Environmental pollution, for example, fluorinated material.This requires that its surface microscopic shape can only be changed by modified to metallic surface structures
Looks, improve surface roughness, make its surface that multiple dimensioned microstructure is presented, and are intercoupled by its configuration of surface, special construction
The hydrophobicity on surface is realized in effect.How to be prepared on metallic matrix without in decorative layer hydrophobic surface always hydrophobic performance research
Focus and difficult point.
Metallic nickel has good mechanical strength and chemical stability higher, and nickel is difficult to be oxidized in atmosphere, right
The resistance to corrosion of bronsted lowry acids and bases bronsted lowry is very strong, and the etch of usual organic acid, hydrochloric acid, hydrofluoric acid and alkaline solution to nickel is extremely slow.Based on these
Excellent performance, metallic nickel is widely used in the fields such as aviation, military affairs, specific alloy, catalyst, but likewise, metallic nickel
It is a kind of water wetted material.Hydrophobically modified for nickel is rarely reported, and current relevant report mainly has：Miao Fahong etc. uses low temperature
Hydro-thermal reaction and stearic acid surface-modified method, prepare the nickel hydroxide with flower-like microsphere structure super-hydrophobic on a glass substrate
Coating；And with nickel hydroxide coating as presoma, by 400 DEG C of heat treatments and stearic acid surface-modified, obtained nickel oxide and surpassed
Hydrophobic coating；The luxuriant and bdautiful grade in field is prepared for the nanostructured of nickel using the method that plating, chemical plating are combined in fine copper matrix surface, obtains
Obtained super hydrophobic surface.But these schemes are substantially all to be needed to additionally introduce hydrophobicity of the low-surface energy substance to improve matrix
Energy；And in the case where matrix surface chemical composition is not changed, can not directly improve the hydrophobic performance of metal nickel surface.
The content of the invention
For above-mentioned the deficiencies in the prior art, metallic nickel surface wettability is changed the invention provides a kind of hf etching
The method of energy, is suitable for improving metallic nickel hydrophobic properties of the surface.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of method that hf etching changes metallic nickel surface wettability, comprises the following steps：
(1) metal nickel surface is cleaned using ultrasonic cleaning mode, by the greasy dirt on metal nickel sheet surface and absorption
Impurity removal, specific cleaning process is：
A () is cleaned by ultrasonic more than 10min using absolute ethyl alcohol to metal nickel sheet surface；
B () takes out metal nickel sheet, and metal nickel sheet then is immersed in into 30 DEG C, 1M with pure flushing three times with anhydrous
In NaOH solution, soak time is more than 30min；
(c) ultrasound more than 30min in 30 DEG C, the NaOH solution of 1M by metal nickel sheet；
D () takes out metal nickel sheet, be each cleaned by ultrasonic 20min with acetone and absolute ethyl alcohol respectively；
E () takes out metal nickel sheet, rinsed three times with absolute ethyl alcohol, is then air-dried under greenhouse experiment；
(2) metal nickel sheet is placed in hydrofluoric acid solution of the mass fraction more than or equal to 40%, then in more than 30 DEG C
Water-bath in carry out chemical etching, etch period is 7~28h, and in etching process, a metal nickel sheet is overturn every 1h
Surface；
(3) the metal nickel sheet after etching is taken out and rinses drying, obtain the metal nickel sheet after changing wet performance.
Specifically, the step (3) comprises the following steps：
(3a) takes out metal nickel sheet, and uses deionized water rinsing；
(3b) is placed in anhydrous with pure, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then rinsed with absolute ethyl alcohol after rinsing
Three times；
(3c) is placed in deionized water after rinsing, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then uses deionized water rinsing
Three times；
Be placed in metal nickel sheet after flushing in 40 DEG C of heating plate and slowly dry by (3d), and is turned over per 5min in drying course
Turn a metal nickel sheet surface, drying time is 30min.
Compared with prior art, the invention has the advantages that：
(1) present invention process is simple, simple operation, low to raw material and equipment requirement, and it passes through using simple hydrofluoric acid
Chemical etching process, metallic nickel is chemically reacted with hydrofluoric acid solution, and special structure and pattern is formed in metal surface,
Surface roughness is improved, so as to effectively enhance the hydrophobicity of metal nickel surface.The present invention is due to need not be to metal nickel surface
Modified, thus the hydrophobic surface of generation will not also change metallic nickel itself chemical composition and chemical property, not influence thereafter
It is continuous to use.
(2) present invention carries out cleaning to metal nickel surface and is divided into two steps, and first step alkali cleaning can be produced in process
Greasy dirt, adsorption matter get rid of, second step can be gone the oxide layer of metal nickel sheet Surface Creation directly by acid etch
Remove, it is not necessary to the extra oxide layer tried to except its surface, saved time and cost.Also, during hf etching,
The product H of generation2And Ni2+、F-Influence to environment less, will not bring serious pollution；Meanwhile, in etching process, lead to
Turn-over is crossed, nickel sheet two sides can be made all to be reacted with hydrofluoric acid, so that the wetability on nickel sheet two sides is approached, it is too big to be unlikely to gap,
Influence is subsequently used.
(3) cost performance of the present invention is high, practical, repeated and selective good, very with application prospect, is suitable in boat
Popularization and application in the fields such as sky, military affairs, specific alloy, catalyst.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Fig. 2 is the Static Contact angular measurement figure after metal nickel sheet alkali cleaning.
Fig. 3 is the Static Contact angular measurement figure that 30 DEG C of hydrofluoric acid solutions etch 7h.
Fig. 4 is the Static Contact angular measurement figure that 30 DEG C of hydrofluoric acid solutions etch 14h.
Fig. 5 is the Static Contact angular measurement figure that 30 DEG C of hydrofluoric acid solutions etch 28h.
Specific embodiment
The invention will be further described with embodiment for explanation below in conjunction with the accompanying drawings, and mode of the invention includes but not only limits
In following examples.
Embodiment
As shown in figure 1, the invention provides a kind of method for changing metallic nickel surface wettability, it mainly employs hydrogen
The mode of fluoric acid etching, with reference to cleaning, changes the wet performance of metal nickel surface, improves its hydrophobicity.It is of the invention main
Flow is as follows：
(1) metal nickel surface is cleaned using ultrasonic cleaning mode, by the greasy dirt on metal nickel sheet surface and absorption
Impurity removal, specific cleaning process is：
A () is cleaned by ultrasonic more than 10min using absolute ethyl alcohol to metal nickel sheet surface；
B () takes out metal nickel sheet, and rinsed three times with absolute ethyl alcohol, and metal nickel sheet then is immersed in into 30 DEG C, 1M
In NaOH solution, soak time is more than 30min；
(c) ultrasound more than 30min in 30 DEG C, the NaOH solution of 1M by metal nickel sheet；
D () takes out metal nickel sheet, be each cleaned by ultrasonic 20min with acetone and absolute ethyl alcohol respectively；
E () takes out metal nickel sheet, rinsed three times with absolute ethyl alcohol, is then air-dried under room temperature condition；
(2) metal nickel sheet is placed in hydrofluoric acid solution of the mass fraction more than or equal to 40%, then in more than 30 DEG C
Water-bath in carry out chemical etching, etch period is 7~28h, and in etching process, a metal nickel sheet is overturn every 1h
Surface；
(3) metal nickel sheet is taken out, and uses deionized water rinsing；
(4) it is placed in absolute ethyl alcohol after rinsing, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then is rinsed with absolute ethyl alcohol
Three times；
(5) it is placed in deionized water after rinsing, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then uses deionized water rinsing
Three times；
(6) the metal nickel sheet after flushing is placed in 40 DEG C of heating plate and is slowly dried, and turned over per 5min in drying course
Turn a metal nickel sheet surface, drying time is 30min.
The technology of the present invention effect is illustrated with two test cases below.Test case is 99.99% from purity
High-purity nickel sheet, size be 10mm × 10mm × 1mm.
Case 1
Metallic nickel surface clean：Metal nickel sheet is placed in the beaker containing 15ml absolute ethyl alcohols first, is cleaned by ultrasonic
10min, taking-up absolute ethyl alcohol is rinsed 3 times repeatedly；Metal nickel sheet is placed in the NaOH solution of 20ml, 1M again, at 30 DEG C
30min is soaked in water-bath, then in 30 DEG C of ultrasound 30min；Then metal nickel sheet is taken out and is placed in the acetone soln of 10ml,
30 DEG C of ultrasonic cleaning 20min；Metal nickel sheet is placed in the ethanol solution of 15ml again then, in 30 DEG C of ultrasonic cleaning
20min；Finally metal nickel sheet is taken out, is rinsed repeatedly with absolute ethyl alcohol 3 times.
Metallic nickel is etched：Metal nickel sheet after surface clean is put into the polytetrafluoro for filling HF acid (content >=40%) solution
In ethene beaker, beaker is placed in 30 DEG C of water-bath, in etching process, nickel sheet surface is overturn per hour.
Metallic nickel cleaning, drying：The metal nickel sheet that 30 DEG C etch after 7h is taken out from hydrofluoric acid solution, deionization is first used
Water is rinsed 3 times；It is placed in again in the polytetrafluoroethylene beaker containing 15ml absolute ethyl alcohols, 30 DEG C of ultrasonic cleaning 10min use anhydrous second
Alcohol is rinsed 3 times；Then it is placed in the glass beaker containing 15ml deionized waters, 30 DEG C of ultrasonic cleaning 10min are rushed with water ion water
Wash 3 times；Finally it is placed in 40 DEG C of heating plate and slowly dries, a face is turned over per 5min in drying course, knot is dried after 30min
Beam.
By the metal nickel sheet after drying, (the prosperous testing machine testing equipment in Chengde has to be placed in JY-82 video contacts angle measuring instrument
Limit company) sample stage on, measure metal nickel surface static contact angle, Fig. 2 be metal nickel sheet alkali cleaning after static contact angle
Measurement figure.The contact angle liquid that uses of test is deionized water, and sample tests 3~5 points respectively per one side, in test each
, in 5~10 μ L, partial test result is as shown in Figure 3 for droplet size.Each test point, is averaged by three measuring and calculating,
Its contact angle numerical value is respectively 105.72 °, 110.09 ° and 108.73 °.As can be seen here, by after hydrofluoric acid chemical etching, metal
Nickel surface shows hydrophobicity.
Case 2
Metal nickel sheet after 14h will be etched in 30 DEG C, HF acid (content >=40%) solution is taken out, and is placed in after cleaning, drying
On the sample stage of JY-82 video contact angle measuring instruments, the static contact angle of metal nickel surface is measured.The liquid that contact angle test is used
Body is deionized water, and every one side of sample tests 3 points respectively, and each droplet size is in 5~10 μ L, partial test knot in test
Fruit is as shown in Figure 4.Each test point, is averaged by three measuring and calculating, its contact angle numerical value be respectively 123.22 °,
129.19 ° and 128.24 °.As can be seen here, by after hydrofluoric acid chemical etching, metal nickel surface has obvious hydrophobicity.
Case 3
Metal nickel sheet after 28h will be etched in 30 DEG C, HF acid (content >=40%) solution is taken out, and is placed in after cleaning, drying
On the sample stage of JY-82 video contact angle measuring instruments, the static contact angle of metal nickel surface is measured.The liquid that contact angle test is used
Body is deionized water, and every one side of sample tests 3 points respectively, and each droplet size is in 5~10 μ L, partial test knot in test
Fruit is as shown in Figure 5.Each test point, is averaged by three measuring and calculating, its contact angle numerical value be respectively 136.22 °,
138.03 ° and 137.05 °.As can be seen here, by after hydrofluoric acid chemical etching, metal nickel surface has obvious hydrophobicity.
The present invention performs etching treatment by hydrofluoric acid solution to metal nickel surface, forms coarse in metal nickel surface
Microstructure, so as to change the wettability of metallic nickel only by way of improving surface roughness, makes metal nickel surface
Hydrophobicity is improved, thus, you can the service life under effectively extending metallic nickel in humidity or containing water vapor conditions,
Widen the range of application of nickel.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit protection model of the invention
Enclose, it is all body design thought of the invention and mentally make have no the change of essential meaning or polishing, what it was solved
Technical problem is still consistent with the present invention, should be included within protection scope of the present invention.
Claims (2)
1. a kind of method that hf etching changes metallic nickel surface wettability, it is characterised in that comprise the following steps：
(1) metal nickel surface is cleaned using ultrasonic cleaning mode, by the greasy dirt on metal nickel sheet surface and the impurity of absorption
Remove, specific cleaning process is：
A () is cleaned by ultrasonic more than 10min using absolute ethyl alcohol to metal nickel sheet surface；
B () takes out metal nickel sheet, and with anhydrous with pure flushing three times, then by metal nickel sheet be immersed in 30 DEG C, the NaOH of 1M it is molten
In liquid, soak time is more than 30min；
(c) ultrasound more than 30min in 30 DEG C, the NaOH solution of 1M by metal nickel sheet；
D () takes out metal nickel sheet, be each cleaned by ultrasonic 20min with acetone and absolute ethyl alcohol respectively；
E () takes out metal nickel sheet, rinsed three times with absolute ethyl alcohol, is then air-dried under greenhouse experiment；
(2) metal nickel sheet is placed in hydrofluoric acid solution of the mass fraction more than or equal to 40%, then in more than 30 DEG C of water
Chemical etching is carried out in bath, etch period is 7~28h, and in etching process, a metal nickel sheet table is overturn every 1h
Face；
(3) the metal nickel sheet after etching is taken out and rinses drying, obtain the metal nickel sheet after changing wet performance.
2. the method that a kind of hf etching according to claim 1 changes metallic nickel surface wettability, its feature exists
In the step (3) comprises the following steps：
(3a) takes out metal nickel sheet, and uses deionized water rinsing；
(3b) is placed in anhydrous with pure, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then rinse three with absolute ethyl alcohol after rinsing
Time；
(3c) is placed in deionized water after rinsing, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then with deionized water rinsing three
Time；
Be placed in metal nickel sheet after flushing in 40 DEG C of heating plate and slowly dry by (3d), and the upset one per 5min in drying course
Minor metal nickel sheet surface, drying time is 30min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710220630.3A CN106929856B (en) | 2017-04-06 | 2017-04-06 | A kind of method that hf etching changes metallic nickel surface wettability |
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| CN201710220630.3A CN106929856B (en) | 2017-04-06 | 2017-04-06 | A kind of method that hf etching changes metallic nickel surface wettability |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108211817A (en) * | 2017-12-29 | 2018-06-29 | 广东工业大学 | A kind of manufacturing method of aluminum metal filter membrane |
| CN113667969A (en) * | 2021-08-18 | 2021-11-19 | 南京信息工程大学 | Composite method for regulating and controlling metal surface wettability |
| CN115354328A (en) * | 2022-08-26 | 2022-11-18 | 深圳市赛尔美电子科技有限公司 | Preparation method of heating element and electronic cigarette |
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| CN103409754A (en) * | 2013-07-29 | 2013-11-27 | 西安交通大学 | Etching-based surface super-hydrophobicity treatment technology for aluminium material |
| CN104846376A (en) * | 2015-05-29 | 2015-08-19 | 清华大学 | Preparation method of metal-based super-hydrophobic surface |
| CN105413994A (en) * | 2015-12-15 | 2016-03-23 | 大连理工大学 | Preparation method for super-hydrophobic surface with bionic micro-nano composite structure |
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2017
- 2017-04-06 CN CN201710220630.3A patent/CN106929856B/en not_active Expired - Fee Related
Patent Citations (3)
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|---|---|---|---|---|
| CN103409754A (en) * | 2013-07-29 | 2013-11-27 | 西安交通大学 | Etching-based surface super-hydrophobicity treatment technology for aluminium material |
| CN104846376A (en) * | 2015-05-29 | 2015-08-19 | 清华大学 | Preparation method of metal-based super-hydrophobic surface |
| CN105413994A (en) * | 2015-12-15 | 2016-03-23 | 大连理工大学 | Preparation method for super-hydrophobic surface with bionic micro-nano composite structure |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108211817A (en) * | 2017-12-29 | 2018-06-29 | 广东工业大学 | A kind of manufacturing method of aluminum metal filter membrane |
| CN108211817B (en) * | 2017-12-29 | 2020-08-18 | 广东工业大学 | Manufacturing method of aluminum metal filtering membrane |
| CN113667969A (en) * | 2021-08-18 | 2021-11-19 | 南京信息工程大学 | Composite method for regulating and controlling metal surface wettability |
| CN115354328A (en) * | 2022-08-26 | 2022-11-18 | 深圳市赛尔美电子科技有限公司 | Preparation method of heating element and electronic cigarette |
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