CN106929856B - 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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- CN106929856B CN106929856B CN201710220630.3A CN201710220630A CN106929856B CN 106929856 B CN106929856 B CN 106929856B CN 201710220630 A CN201710220630 A CN 201710220630A CN 106929856 B CN106929856 B CN 106929856B
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- metal nickel
- nickel sheet
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- dehydrated alcohol
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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 Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- ing And Chemical Polishing (AREA)
Abstract
A kind of method that the present invention discloses hf etching change metallic nickel surface wettability, comprising: (1) metal nickel surface is cleaned using ultrasonic cleaning mode, the greasy dirt on metal nickel sheet surface and impurity are removed；(2) metal nickel sheet is placed in >=40% hydrofluoric acid solution, chemical etching is then carried out in 30 DEG C or more of water-bath, etch period is 7~28h, and in etching process, overturns a metal nickel sheet surface every 1h；(3) drying is taken out and rinsed to the metal nickel sheet after etching, obtain the metal nickel sheet after changing wet performance.The present invention performs etching processing to metal nickel surface by hydrofluoric acid solution, coarse microstructure is formed in metal nickel surface, to only change the wettability of metallic nickel by way of improving surface roughness, it is improved the hydrophobicity of metal nickel surface, and then service life of the metallic nickel under humidity or containing water vapor conditions is effectively extended, widen the application range 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
Change the method for metallic nickel surface wettability.
Background technique
The wettability of material surface is one of intrinsic property of material.So-called moisten is exactly to exist less on the surface of solid
Perhaps when liquid, the phenomenon that newly generated solid-liquid interface is instead of gas-liquid/solid interface before.Wettability of the surface is generally divided into two
Kind: hydrophily and hydrophobicity.Hydrophily refers to that material has affinity, general inoganic solids, metal and its oxide to water
Deng, surface tension is all larger, frequently referred to high-energy solid surface, easily soaked by liquid, have significant hydrophily.Hydrophobicity is
Refer to that material has repulsive interaction, the general substance with low-surface-energy to water, such as fluoride etc. all has significant hydrophobic
Property；Hydrophobic or even super hydrophobic surface, since 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 be concerned.
Material surface hydrophobically modified is generally used two kinds of approach: 1) low-surface energy substance modification of surfaces is used, in metal
Surface forms a hydrophobic coating, generallys use some low-surface-energies or organic molecule, high polymer containing hydrophobic grouping etc.；2)
Change the microstructure on surface, surface roughness is improved, to improve the hydrophobicity on surface；Certainly, under the conditions of certain, 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 certain organic matters are also brought along
Environmental pollution, for example, fluorine-containing substance.This requires can only change its surface microscopic shape by being modified to metallic surface structures
Looks improve surface roughness, make its surface that multiple dimensioned microstructure be presented, and are intercoupled by its configuration of surface, special construction
The hydrophobicity on surface is realized in effect.How to prepare on metallic matrix without decorative layer hydrophobic surface is always in hydrophobic performance research
Hot and difficult issue.
Metallic nickel has good mechanical strength and higher chemical stability, and nickel is not easy to be oxidized in air, right
The resistance to corrosion of bronsted lowry acids and bases bronsted lowry is very strong, and usual organic acid, hydrochloric acid, hydrofluoric acid and alkaline solution are extremely slow to the etch of nickel.Based on these
Excellent performance, metallic nickel are 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.Be rarely reported for the hydrophobically modified of nickel, current relevant report mainly has: it is equal using low temperature that seedling is sent out macro
Hydro-thermal reaction and stearic acid surface-modified method, it is super-hydrophobic to prepare the nickel hydroxide with flower-like microsphere structure on a glass substrate
Coating；And using nickel hydroxide coating as presoma, by 400 DEG C of heat treatments and stearic acid surface-modified, it is super nickel oxide has been obtained
Hydrophobic coating；The luxuriant and bdautiful equal method combined using plating, chemical plating in field is prepared for the nanostructure of nickel in fine copper matrix surface, obtains
Obtained super hydrophobic surface.But these schemes are substantially all the hydrophobicity for needing to additionally introduce low-surface energy substance to improve matrix
Energy；And the hydrophobic performance of metal nickel surface cannot be directly improved in the case where not changing matrix surface chemical composition.
Summary of the invention
In view of the above shortcomings of the prior art, the present invention provides a kind of hf etchings to change metallic nickel surface wettability
The method of energy, suitable for raising metallic nickel hydrophobic properties of the surface.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of method that hf etching changes metallic nickel surface wettability, comprising 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 are as follows:
(a) 10min or more is cleaned by ultrasonic to metal nickel sheet surface using dehydrated alcohol；
(b) metal nickel sheet is taken out, and with anhydrous then metal nickel sheet is immersed in by 30 DEG C, 1M with pure flushing three times
In NaOH solution, soaking time is 30min or more；
(c) by metal nickel sheet in 30 DEG C, the NaOH solution of 1M ultrasound 30min or more；
(d) metal nickel sheet is taken out, is respectively cleaned by ultrasonic 20min with acetone and dehydrated alcohol respectively；
(e) metal nickel sheet is taken out, is rinsed three times, is then carried out under greenhouse experiment air-dried with dehydrated alcohol；
(2) metal nickel sheet is placed in hydrofluoric acid solution of the mass fraction more than or equal to 40%, then in 30 DEG C or more
Water-bath in carry out chemical etching, etch period is 7~28h, and in etching process, overturns a metal nickel sheet every 1h
Surface；
(3) drying is taken out and rinsed to the metal nickel sheet after etching, obtain the metal nickel sheet after changing wet performance.
Specifically, the step (3) the following steps are included:
(3a) takes out metal nickel sheet, and is rinsed with deionized water；
(3b) flushing is placed on anhydrous in pure, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then rinsed with dehydrated alcohol
Three times；
(3c) flushing is placed in deionized water, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then rinsed with deionized water
Three times；
Metal nickel sheet after flushing is placed in 40 DEG C of heating plate and slowly dries by (3d), and every 5min is turned in drying course
Turn a metal nickel sheet surface, drying time 30min.
Compared with prior art, the invention has the following advantages:
(1) present invention process is simple, operation is convenient, low to raw material and equipment requirement, by using simple hydrofluoric acid
Chemical etching process chemically reacts metallic nickel and hydrofluoric acid solution, and special structure and pattern are formed in metal surface,
Surface roughness is improved, to effectively enhance the hydrophobicity of metal nickel surface.The present invention is not due to needing to metal nickel surface
It is modified, thus the hydrophobic surface generated will not change metallic nickel itself chemical component and chemical property, not influence thereafter
It is continuous to use.
(2) present invention, which clean to metal nickel surface, is divided into two steps, and first step alkali cleaning can will generate in process
Greasy dirt, adsorption matter get rid of, second step directly passes through acid etch, the oxide layer of metal nickel sheet Surface Creation can be gone
It removes, does not need the oxide layer for additionally trying to remove its surface, saved time and cost.Also, during hf etching,
The product H of generation2And Ni2+、F-Influence to environment is little, will not bring serious pollution；Meanwhile in etching process, lead to
Turn-over is crossed, nickel sheet two sides can be made all to react with hydrofluoric acid, to keep the wetability on nickel sheet two sides close, it is too big to be unlikely to gap,
Influence subsequent use.
(3) cost performance of the present invention is high, practical, repeated and selectivity is good, has very much application prospect, suitable for navigating
It is promoted and applied in the fields such as sky, military affairs, specific alloy, catalyst.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Fig. 2 is the Static Contact angular measurement figure after the alkali cleaning of metal nickel sheet.
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 with reference to the accompanying drawing, and mode of the invention includes but not only limits
In following embodiment.
Embodiment
As shown in Figure 1, mainly using hydrogen the present invention provides a kind of method for changing metallic nickel surface wettability
The mode of fluoric acid etching changes the wet performance of metal nickel surface, improves its hydrophobicity in conjunction with cleaning process.The present invention is main
Process 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 are as follows:
(a) 10min or more is cleaned by ultrasonic to metal nickel sheet surface using dehydrated alcohol；
(b) metal nickel sheet is taken out, and is rinsed three times with dehydrated alcohol, metal nickel sheet is then immersed in 30 DEG C, 1M
In NaOH solution, soaking time is 30min or more；
(c) by metal nickel sheet in 30 DEG C, the NaOH solution of 1M ultrasound 30min or more；
(d) metal nickel sheet is taken out, is respectively cleaned by ultrasonic 20min with acetone and dehydrated alcohol respectively；
(e) metal nickel sheet is taken out, is rinsed three times with dehydrated alcohol, it is then air-dried in carrying out under room temperature；
(2) metal nickel sheet is placed in hydrofluoric acid solution of the mass fraction more than or equal to 40%, then in 30 DEG C or more
Water-bath in carry out chemical etching, etch period is 7~28h, and in etching process, overturns a metal nickel sheet every 1h
Surface；
(3) metal nickel sheet is taken out, and is rinsed with deionized water；
(4) it rinses and is placed in dehydrated alcohol, and be cleaned by ultrasonic 10min under the conditions of 30 DEG C, then rinsed with dehydrated alcohol
Three times；
(5) it rinses and is placed in deionized water, and be cleaned by ultrasonic 10min under the conditions of 30 DEG C, then rinsed with deionized water
Three times；
(6) the metal nickel sheet after flushing is placed in 40 DEG C of heating plate and is slowly dried, and every 5min is turned in drying course
Turn a metal nickel sheet surface, drying time 30min.
The technology of the present invention effect is illustrated with two test cases below.It is 99.99% that test case, which selects purity,
High-purity nickel sheet, having a size of 10mm × 10mm × 1mm.
Case 1
Metal nickel sheet: being placed in the beaker containing 15ml dehydrated alcohol by metallic nickel surface clean first, ultrasonic cleaning
10min takes out and uses dehydrated alcohol repeated flushing 3 times；Metal nickel sheet is placed in the NaOH solution of 20ml, 1M again, at 30 DEG C
30min is impregnated in water-bath, then in 30 DEG C of ultrasound 30min；Then the taking-up of metal nickel sheet is placed in the acetone soln of 10ml,
30 DEG C of ultrasonic cleaning 20min；Then metal nickel sheet is placed in the ethanol solution of 15ml again, is cleaned by ultrasonic at 30 DEG C
20min；Finally metal nickel sheet is taken out, with dehydrated alcohol repeated flushing 3 times.
Metallic nickel etching: the metal nickel sheet after surface clean is put into the polytetrafluoro for filling sour (content >=40%) solution of HF
It in ethylene beaker, places the beaker in 30 DEG C of water-bath, in etching process, overturns nickel sheet surface per hour.
Metallic nickel cleaning, drying: the metal nickel sheet after 30 DEG C of etching 7h is taken out from hydrofluoric acid solution, first uses deionization
Water rinses 3 times；It is placed in the polytetrafluoroethylene beaker containing 15ml dehydrated alcohol again, 30 DEG C of ultrasonic cleaning 10min, with anhydrous second
Alcohol rinses 3 times；Then it is placed in the glass beaker containing 15ml deionized water, 30 DEG C of ultrasonic cleaning 10min, is rushed with water ion water
It washes 3 times；It is finally placed in 40 DEG C of heating plate and slowly dries, every 5min turns over a face in drying course, dries knot after 30min
Beam.
By the metal nickel sheet after drying, being placed in JY-82 video contact angle measuring instrument, (the prosperous testing machine detection device in Chengde has
Limit company) sample stage on, measure metal nickel surface static contact angle, Fig. 2 be the alkali cleaning of metal nickel sheet after static contact angle
Measurement figure.The liquid that contact angle test uses is deionized water, and every one side of sample tests 3~5 points respectively, each in test
For droplet size in 5~10 μ L, partial test result is as shown in Figure 3.Each test point, is averaged by calculating three times,
Its contact angle numerical value is respectively 105.72 °, 110.09 ° and 108.73 °.It can be seen that after hydrofluoric acid chemical etching, metal
Nickel surface shows hydrophobicity.
Case 2
Metal nickel sheet after 14h will be etched in 30 DEG C, sour (content >=40%) solution of HF is taken out, and cleaning, drying is placed on
On the sample stage of JY-82 video contact angle measuring instrument, the static contact angle of metal nickel surface is measured.The liquid that contact angle test uses
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 calculating three times, contact angle numerical value is respectively 123.22 °,
129.19 ° and 128.24 °.It can be seen that metal nickel surface has apparent hydrophobicity after hydrofluoric acid chemical etching.
Case 3
Metal nickel sheet after 28h will be etched in 30 DEG C, sour (content >=40%) solution of HF is taken out, and cleaning, drying is placed on
On the sample stage of JY-82 video contact angle measuring instrument, the static contact angle of metal nickel surface is measured.The liquid that contact angle test uses
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 calculating three times, contact angle numerical value is respectively 136.22 °,
138.03 ° and 137.05 °.It can be seen that metal nickel surface has apparent hydrophobicity after hydrofluoric acid chemical etching.
The present invention performs etching processing to metal nickel surface by hydrofluoric acid solution, is formed in metal nickel surface coarse
Microstructure makes metal nickel surface to only change the wettability of metallic nickel by way of improving surface roughness
Hydrophobicity is improved, in this way, can effectively extend service life of the metallic nickel under humidity or containing water vapor conditions,
Widen the application range 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 in body design thought of the invention and mentally make have no the change of essential meaning or polishing, solved
Technical problem is still consistent with the present invention, should all be included within protection scope of the present invention.
Claims (1)
1. a kind of method that hf etching changes metallic nickel surface wettability, which comprises 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
Removal, specific cleaning process are as follows:
(a) 10min or more is cleaned by ultrasonic to metal nickel sheet surface using dehydrated alcohol；
(b) metal nickel sheet is taken out, and is rinsed three times with dehydrated alcohol, then metal nickel sheet is immersed in the NaOH solution of 1M,
Soaking time is 30min or more；
(c) metal nickel sheet is taken out, then carries out ultrasonic cleaning 30min or more again；
(d) the metal nickel sheet after ultrasonic cleaning is taken out, then uses acetone and each self-cleaning 20min of dehydrated alcohol respectively；
(e) metal nickel sheet is rinsed three times with dehydrated alcohol again, is then carried out under greenhouse experiment air-dried；
(2) metal nickel sheet is placed in hydrofluoric acid solution of the mass fraction more than or equal to 40%, then in 30 DEG C or more of water
Chemical etching is carried out in bath, etch period is 7~14h, and in etching process, overturns a metal nickel sheet table every 1h
Face；
(3) drying is taken out and rinsed to the metal nickel sheet after etching, obtain the metal nickel sheet after changing wet performance, specifically include
Following steps:
(3a) takes out metal nickel sheet, and is rinsed three times with deionized water；
(3b) flushing is placed in dehydrated alcohol, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then rinses three with dehydrated alcohol
Time；
(3c) flushing is placed in deionized water, and is cleaned by ultrasonic 10min under the conditions of 30 DEG C, then rinses three with deionized water
Time；
Metal nickel sheet after flushing is placed in 40 DEG C of heating plate and slowly dries by (3d), and every 5min overturning one in drying course
Minor metal nickel sheet surface, drying time 30min.
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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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| 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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| CN103409754A (en) * | 2013-07-29 | 2013-11-27 | 西安交通大学 | Etching-based surface super-hydrophobicity treatment technology for aluminium material |
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| 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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| CN103409754A (en) * | 2013-07-29 | 2013-11-27 | 西安交通大学 | Etching-based surface super-hydrophobicity treatment technology for aluminium material |
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| 金属基超疏水制备方法与应用浅述;李晶等;《长春理工大学学报（自然科学版）》;20141215;第37卷(第6期);第27-31、35页 |
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