CN106929854A - A kind of method that salt acid etch changes metallic nickel surface wettability - Google Patents
A kind of method that salt acid etch changes metallic nickel surface wettability Download PDFInfo
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- CN106929854A CN106929854A CN201710220626.7A CN201710220626A CN106929854A CN 106929854 A CN106929854 A CN 106929854A CN 201710220626 A CN201710220626 A CN 201710220626A CN 106929854 A CN106929854 A CN 106929854A
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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
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- Organic Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
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Abstract
The invention discloses a kind of method that salt acid etch 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) configuration concentration is 10~20wt% hydrochloric acid solutions, and metal nickel sheet is placed in hydrochloric acid solution, and chemical etching is then carried out in more than 30 DEG C of water-bath, and etch period is 21~56h；(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 hydrochloric 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 that a kind of salt acid etch changes
The method for becoming 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 to nickel such as usual organic acid, hydrochloric acid and alkaline solution is extremely slow.It is excellent based on these
Performance, metallic nickel is widely used in the fields such as aviation, military affairs, specific alloy, catalyst, but likewise, metallic nickel is also a kind of
Water wetted material.Hydrophobically modified for nickel is rarely reported, and current relevant report mainly has：Miao Fahong etc. is anti-using low-temperature hydrothermal
The nickel hydroxide super-hydrophobic coat with flower-like microsphere structure should be on a glass substrate prepared with stearic acid surface-modified method；
And with nickel hydroxide coating as presoma, by 400 DEG C of heat treatments and stearic acid surface-modified, obtained the super-hydrophobic painting of nickel oxide
Layer；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 super
Hydrophobic surface.But these schemes are substantially all to be needed to additionally introduce hydrophobic performance of the low-surface energy substance to improve matrix；And
In the case where matrix surface chemical composition is not changed, the hydrophobic performance of metal nickel surface can not be directly improved.
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 salt acid etch
Method, be suitable for improve 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 salt acid etch 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 room temperature condition；
(2) it is 10~20wt% hydrochloric acid solutions using 36%~38% hydrochloric acid and deionized water configuration concentration, and by gold
Category nickel sheet is placed in hydrochloric acid solution, and chemical etching is then carried out in more than 30 DEG C of water-bath, and etch period is 21~56h, and
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 wet performance changes.
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), is overturn per 5min in drying course
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 acidified
Etching technics is learned, metallic nickel is chemically reacted with hydrochloric acid solution, special structure and pattern is formed in metal surface, improved
Surface roughness, so as to effectively enhance the hydrophobicity of metal nickel surface.The present invention to metal nickel surface due to that need not carry out
Modification, thus the hydrophobic surface of generation will not also change metallic nickel itself chemical composition and chemical property, not influence it subsequently to make
With.
(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, it is raw in hydrochloric acid etching process
Into product H2And Ni2+、Cl-Influence to environment less, will not bring serious pollution；Meanwhile, in etching process, pass through
Turn-over, can make nickel sheet two sides all with hydrochloric acid reaction so that the wetability on nickel sheet two sides is approached, it is too big to be unlikely to gap, influence
Subsequently use.
(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 30 DEG C of Static Contact angular measurement figures of etching 42h of 10.2wt% hydrochloric acid solutions.
Fig. 3 is 30 DEG C of Static Contact angular measurement figures of etching 42h of 15.03wt% hydrochloric acid solutions.
Fig. 4 is 30 DEG C of Static Contact angular measurement figures of etching 42h of 20.0wt% hydrochloric acid solutions.
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 salt
The mode of acid etch, with reference to cleaning, changes the wet performance of metal nickel surface, improves its hydrophobicity.Main stream of the invention
Journey 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) it is 10~20wt% hydrochloric acid solutions using 36%~38% hydrochloric acid and deionized water configuration concentration, and by gold
Category nickel sheet is placed in hydrochloric acid solution, and chemical etching is then carried out in more than 30 DEG C of water-bath, and etch period is 21~56h, and
And in etching process, a metal nickel sheet surface is overturn every 1h；
(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, overturn per 5min in drying course
Metal nickel sheet surface, drying time is 30min.
The technology of the present invention effect is illustrated with several 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.
Hydrochloric acid solution is configured：Hydrochloric acid solution is prepared by 36%~38% hydrochloric acid and deionized water, 5ml is measured respectively
36%~38% hydrochloric acid and 15ml deionized waters, is configured to the hydrochloric acid solution of 10.2wt%.
Nickel salts acid etch：Metal nickel sheet after surface clean is put into the beaker containing 10.2wt% hydrochloric acid solutions
In, 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 42h is taken out from hydrochloric acid solution, deionized water is first used
Rinse 3 times；It is placed in again in the beaker containing 15ml absolute ethyl alcohols, 30 DEG C of ultrasonic cleaning 10min are rinsed 3 times with absolute ethyl alcohol；Connect
And be placed in the beaker containing 15ml deionized waters, 30 DEG C of ultrasonic cleaning 10min are rinsed 3 times with water ion water；Finally it is placed in 40
DEG C heating plate on slowly dry, turn over a face per 5min in drying course, drying terminates after 30min.
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.The liquid that contact angle test is used is deionized water,
Sample per one side respectively test 3~5 points, in test each droplet size in 5~10 μ L, in partial test result such as Fig. 2
It is shown.Each test point, is averaged by three measuring and calculating, and its contact angle numerical value is respectively 137.85 °, 144.49 °.Thus
It can be seen that, by after hydrochloric acid chemical etching, metal nickel surface has significant hydrophobicity.
Case 2
The hydrochloric acid and 14ml deionized waters of 8.5ml 36%~38% are measured respectively, and the hydrochloric acid for being configured to 15.03wt% is molten
Liquid.Metal nickel sheet after etching 42h in 30 DEG C of hydrochloric acid solutions of 15.03wt% is taken out, JY-82 is placed in after cleaning, drying and is regarded
On the sample stage of frequency contact angle measurement, the static contact angle of metal nickel surface is measured.Contact angle tests the liquid for using
Ionized water, every one side of sample tests 3 points respectively, and, in 5~10 μ L, partial test result is as schemed for each droplet size in test
Shown in 3.Each test point, is averaged by three measuring and calculating, its contact angle numerical value be respectively 136.75 °, 143.32 ° and
142.57°.As can be seen here, by after hydrochloric acid chemical etching, metal nickel surface has significant hydrophobicity.
Case 3
The hydrochloric acid and 8.5ml deionized waters of 9ml36%~38% are measured respectively, are configured to the hydrochloric acid solution of 20.0wt%.
Metal nickel sheet after etching 42h in 30 DEG C of hydrochloric acid solutions of 20.0wt% is taken out, JY-82 videos is placed in after cleaning, drying and is connect
On the sample stage of feeler measuring instrument, the static contact angle of metal nickel surface is measured.The liquid that contact angle test is used is deionization
Water, sample per one side respectively test 3 points, in test each droplet size in 5~10 μ L, in partial test result such as Fig. 4
It is shown.Each test point, is averaged by three measuring and calculating, its contact angle numerical value be respectively 141.39 °, 144.35 ° and
143.0°.As can be seen here, by after hydrochloric acid chemical etching, metal nickel surface has significant hydrophobicity.
The present invention performs etching treatment by hydrochloric acid solution to metal nickel surface, forms coarse micro- in metal nickel surface
Structure is seen, so as to change the wettability of metallic nickel only by way of improving surface roughness, makes dredging for metal nickel surface
It is aqueous to be improved, thus, you can the service life under effectively extending metallic nickel in humidity or containing water vapor conditions, open up
The range of application of nickel wide.
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 salt acid etch 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 room temperature condition；
(2) it is 10~20wt% hydrochloric acid solutions using 36%~38% hydrochloric acid and deionized water configuration concentration, and by metallic nickel
Piece is placed in hydrochloric acid solution, and chemical etching is then carried out in more than 30 DEG C of water-bath, and etch period is 21~56h, 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 wet performance changes.
2. the method that a kind of salt acid etch according to claim 1 changes metallic nickel surface wettability, it is characterised in that
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), is overturn once per 5min in drying course
Metal nickel sheet surface, drying time is 30min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710220626.7A CN106929854B (en) | 2017-04-06 | 2017-04-06 | A kind of method that salt acid etch changes metallic nickel surface wettability |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710220626.7A CN106929854B (en) | 2017-04-06 | 2017-04-06 | A kind of method that salt acid etch changes metallic nickel surface wettability |
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| CN106929854A true CN106929854A (en) | 2017-07-07 |
| CN106929854B CN106929854B (en) | 2019-04-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2017
- 2017-04-06 CN CN201710220626.7A patent/CN106929854B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 李晶等: "金属基超疏水制备方法与应用浅述", 《长春理工大学学报（自然科学版）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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