CN105568330B - A kind of preparation method of base steel antiscale superficial layer - Google Patents
A kind of preparation method of base steel antiscale superficial layer Download PDFInfo
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- CN105568330B CN105568330B CN201610014036.4A CN201610014036A CN105568330B CN 105568330 B CN105568330 B CN 105568330B CN 201610014036 A CN201610014036 A CN 201610014036A CN 105568330 B CN105568330 B CN 105568330B
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- steel
- antiscale
- curved beam
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
Abstract
The invention discloses a kind of preparation method of base steel antiscale superficial layer, is a kind of method for preparing hydrophobic antiscale ormolu layer in steel surface, belongs to metal material surface antiscale field.The present invention is using steel as substrate, first in one layer of ormolu layer of steel surface electro-deposition, sample is immersed in the beaker equipped with potassium hydroxide and ammonium persulfate mixed solution again, and beaker is put into held for some time in the water-bath of certain temperature, then at room temperature, above-mentioned processed steel curved beam is immersed into a few hours in certain density perfluoro caprylic acid ethanol solution, is dried at room temperature after taking-up, you can obtain antiscale superficial layer.The antiscale superficial layer and water and the contact angle of glycerine that method using the present invention obtains are more than 150 °, and both roll angles are respectively less than 5 °；The antiscale sample is in CaCl2And NaHCO3Fouling pattern in the mixed solution of composition be it is needle-shaped, it is similar to aragonite structure, there is preferable antiscale with respect to the rhombohedron calcite structure on steel matrix surface.
Description
Technical field
The invention belongs to metal material surface antiscale field, and being related to one kind preparation in steel matrix has antiscale superficial layer
Method.
Background technology
Super hydrophobic surface causes the extensive concern of researcher due to its special wetability, as biomimetic micro-nano
One of hot spot in technology.In recent years, emerged in large numbers a large amount of related super-hydrophobic documents and patent, but the document in relation to super-amphiphobic with
Patent is relatively fewer, particularly realizes ultra-amphosphobic in steel surface.Super-double-hydrophobic surface refers to not only super-hydrophobic but also superoleophobic table
Face, that is, the surface obtained contact with water and oil is all higher than 150 °, and has less roll angle.Super-double-hydrophobic surface can be real
Existing automatically cleaning, so as to fulfill antipollution and erosion-resisting ability；The resistance of water or oil can be reduced, so as to reduce conveying cost；
Etc..
Steel are quite varied as a kind of important engineering material, application.But in having wet environment existing for oxygen
It is particularly easy to be corroded, reduces the service life of steel.According to traditional anticorrosion technique, one layer of electro-deposition in metal surface
Metal layer can reduce the probability that is corroded of steel surface；Ormolu is electrodeposited into steel surface as a kind of antiscaling alloy
The scale formation of steel surface can be reduced；Surface with ultra-amphosphobic can reduce the contact with surface of water and other greasy dirts and
Stick, improve steel surface from clear property.Have the ormolu layer of ultra-amphosphobic can be with so preparing one layer in steel surface
Make its surface that there is self-cleaning property, anticorrosive property and antiscale at the same time, and then preferably protect steel base.
The present invention is by a series of simple processes, in the super-amphiphobic ormolu that steel surface is prepared for having antiscale
Layer, develops a kind of deposition layer with ultra-amphosphobic energy, Corrosion Protection and scale-preventing performance.Meanwhile in the present invention
Method is simple, and production cost is low, does not have particular/special requirement to the shape of substrate sample, has potential application in industrialized production
Value.
The content of the invention
It is an object of the invention to provide it is a kind of it is simple and effective steel surface prepare with antiscale coating method,
So that steel surface has the function of good antiscale property, the service life of steel is improved.
To achieve the above object, the method sequentially comprises the following steps：
1st, the pre-treatment of steel substrate：The steel processed and ormolu (brass) sample are polished light with waterproof abrasive paper
It is sliding, and the sample polished is sequentially placed into progress ultrasonic cleaning 5min in acetone, absolute ethyl alcohol, to remove specimen surface
Grease and pollutant；Then cleaned base steel bottom sample is subjected to surface alkali cleaning oil removing successively and acid-wash activation is handled：Alkali
It is that the steel curved beam that will be polished smooth is put into the sodium hydroxide containing 30g/L, the sodium carbonate of 20g/L, the sodium phosphate of 20g/L to remove oil
(60 DEG C) processing 15min in the mixed aqueous solution formed with the sodium metasilicate of 10g/L, acid-wash activation processing is by after alkali cleaning oil removing
Steel curved beam is put into activation 15s in the dilute sulfuric acid aqueous solution (room temperature) that volume fraction is 10%.
2nd, acid copper zinc alloy layer：Configure the cupric sulfate pentahydrate containing 10-35g/L, the white vitriol of 7-33g/L, 50-
The mixed solution of the sodium potassium tartrate tetrahydrate of 150g/L and the sodium hydroxide of 30-70g/L, by the steel cleaned up in step 1 and copper zinc
Alloy (brass) sample, which is immersed in the good mixed solution of above-mentioned configuration, carries out electrodeposition process, and the steel curved beam handled well is the moon
Pole, the ormolu sample polished smooth are that the distance between anode, two electrodes is 2cm, electrodeposition time 30-90min, temperature
Spend for 20-40 DEG C, current density 0.4-5A/dm2, after reaction, quickly with a large amount of clear water rinse steel curved beam, and with dry
Machine dries up, and subsequently enters in next step.
3rd, hydrothermal processes：Steel curved beam of the surface in step 2 covered with ormolu layer is immersed in equipped with potassium hydroxide and
In the beaker of ammonium persulfate mixed aqueous solution, and beaker is put into 20-80 DEG C of water-bath and keeps the temperature 5-50min, reaction terminates
Afterwards, steel curved beam is taken out and cleaned, dry；The concentration of the potassium hydroxide is 0.5-3.5mol/L, the concentration of ammonium persulfate
For 0.08-0.16mol/L.
4th, low energy is modified：The sample obtained in step 3 is put into the perfluoro caprylic acid absolute ethyl alcohol of 0.005-0.02mol/L
6-72h is soaked in solution, is put into culture dish after taking-up, dries at ambient temperature.
Water and glycerine are dripped to contact angle determination is carried out on dirty proof layer obtained above, contact angle is all higher than 150 °, rolling
Dynamic angle is less than 10 °, and the dirty proof layer is placed remain within more than 6 months keep its super lyophoby in atmosphere.
The preparation method of antiscale superficial layer in the present invention, technique is simple, easy to operate, and production cost is low, and production efficiency is high,
And there is good prospects for commercial application without particular/special requirement to the shape of substrate sample：Available for table in pipeline made of steel
Face, reduces resistance, improves infusion efficiency, reduces conveying cost；For steel-product and equipment surface, its surface can be increased
Automatically cleaning and corrosion resistance, reduce maintenance cost, etc..
Brief description of the drawings
The invention will be further described below in conjunction with the accompanying drawings.
Fig. 1 is the SEM figures of the dirty proof layer of X90 pipeline steel surfaces in the embodiment of the present invention；
Fig. 2 is contact angle of the drop in the dirty proof layer of X90 pipeline steel surfaces：(a) contact angle of water is 154.59 °, (b) third
The contact angle of triol is 153.59 °；
Fig. 3 is the SEM figures of the calcium carbonate crystal of the X90 pipe line steel specimen surfaces polished smooth；
Fig. 4 is the SEM figures of the calcium carbonate crystal of the antiscale layer surface obtained in the embodiment of the present invention.
Embodiment
With reference to specific embodiment, the present invention is further explained.Following embodiments are merely to illustrate the present invention, and do not have to
In restriction protection scope of the present invention.The modifications and adaptations that technical staff makes according to the present invention in practical applications, still fall within
Protection scope of the present invention.
The preparation method of antiscale superficial layer, is completed by following steps successively in the present embodiment：
(1) it is substrate sample to choose the X90 pipe line steels that size is 20 × 50 × 3mm, and size is the copper zinc of 20 × 50 × 5mm
Alloy (brass) is to electrode samples, is polished smooth the X90 pipe line steels processed and brass sample with waterproof abrasive paper, and will polishing
Good sample is sequentially placed into ultrasonic cleaning 5min in acetone, absolute ethyl alcohol, to remove the grease of specimen surface and pollutant；
(2) above-mentioned cleaned steel curved beam is submerged initially in the sodium hydroxide containing 30g/L, the sodium carbonate of 20g/L, 20g/L
Sodium phosphate and 10g/L sodium metasilicate composition mixed aqueous solution in (60 DEG C) alkali cleaning oil removing 15min, sample rushes through a large amount of clear water
After washing, the H that volume fraction is 10% is put into2SO4(room temperature) acid-wash activation 15s in aqueous solution, cleans after taking-up, is dry, to carry
The combination power of high deposition layer and steel substrate surface；
(3) by the above-mentioned X90 pipelines steel curved beam handled well and brass sample be immersed in the cupric sulfate pentahydrate containing 30g/L,
Electro-deposition is carried out in the mixed aqueous solution of the sodium hydroxide of the white vitriol of 12g/L, the sodium potassium tartrate tetrahydrate of 100g/L and 50g/L
Processing, wherein steel curved beam is cathode (effective dimensions is 20 × 35 × 3mm), and brass sample is the distance between anode, two electrodes
For 2cm, electrodeposition time 60min, electrodeposition temperature is 23 DEG C, and electro-deposition current density is 0.8A/dm2, after reaction,
Steel curved beam quickly is rinsed with a large amount of clear water, and is dried up with hair-dryer, is subsequently entered in next step；
(4) X90 steel curved beam of the surface that step (3) obtains covered with ormolu layer is immersed in equipped with 2.5mol/L's
In the beaker of the ammonium persulfate mixed solution of potassium hydroxide and 0.12mol/L, and beaker is put into 60 DEG C of water-bath and is kept the temperature
30min, steel curved beam after reaction, taken out and cleaned, dry；
(5) the X90 steel curved beams that step (4) obtains are entered in the perfluoro caprylic acid ethanol solution of 0.01mol/L and soaked
60h is steeped, is put into after taking-up in culture dish, dries to obtain super-double-hydrophobic surface at ambient temperature, its surface topography is shown in Fig. 1；This
The contact angle of surface and water can reach 154.59 ° (Fig. 2 (a)), and the contact angle with glycerine is 153.59 ° (Fig. 2 (b)), and two
The roll angle of person is respectively less than 5 °.
(6) the antiscale sample for obtaining step (5) and the X90 steel matrix samples polished smooth are respectively put into 100mL and contain
There is the CaCl of 0.01mol/L2With the NaHCO of 0.01mol/L3In the mixed solution of composition, continue 6h at 70 DEG C.Sample takes out
Dry at ambient temperature afterwards, find calcium carbonate crystal particle that steel matrix surface is formed mainly using hexagonal prism and rhombohedron as
It is main, (Fig. 3) similar with calcite structure；And bar-shaped, acicular texture is presented in antiscale superficial layer, similar to aragonite structure, particle gathers
Collection forms loose media, and crystal draw ratio substantially becomes larger (Fig. 4), and aragonite crystalline scale is unstable and is easy to remove, and shows this antiscale table
Surface layer has preferable antiscale.
Claims (1)
1. a kind of preparation method of base steel antiscale superficial layer, it is characterised in that including following steps：
(1) steel substrate sample is chosen, base steel bottom sample is polishing to 2000# with waterproof abrasive paper, then carries out steel curved beam successively
Surface alkali cleaning oil removing and acid-wash activation processing；
(2) steel curved beam after processing in step (1) is immersed in electrodeposit liquid and carries out electrodeposition process, electric depositing solution is to contain
There are the cupric sulfate pentahydrate of 10-35g/L, the white vitriol of 7-33g/L, the sodium potassium tartrate tetrahydrate of 50-150g/L and 30-70g/L
The mixed aqueous solution of sodium hydroxide composition, steel curved beam is cathode, and ormolu (brass) sample polished smooth is anode, and electricity is heavy
The product time is 30-90min, and temperature is 20-40 DEG C, current density 0.4-5A/dm2, after reaction, quickly with a large amount of clear water
Steel curved beam is rinsed, and is dried up with hair-dryer；
(3) steel curved beam of the surface covered with ormolu layer that electro-deposition in step (2) obtains is immersed in and is equipped with concentration
In beaker of the potassium hydroxide and concentration of 0.5-3.5mol/L for the ammonium persulfate mixed aqueous solution of 0.04-0.14mol/L, and will
Beaker, which is put into 20-80 DEG C of water-bath, keeps the temperature 5-50min, after reaction, steel curved beam is taken out and is cleaned, dry；
(4) steel curved beam after processing in step (3) is put into the perfluoro caprylic acid absolute ethyl alcohol that concentration is 0.005-0.02mol/L
6-72h is soaked in solution and carries out low energy modification, then steel curved beam is taken out and is put into culture dish, dries, obtains at ambient temperature
To antiscale superficial layer.
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| CN106193189B (en) * | 2016-07-20 | 2020-01-10 | 王淑芬 | Efficient condensed air water collecting system and method |
| CN106987875B (en) * | 2017-03-03 | 2019-05-07 | 四川农业大学 | A kind of preparation method of super-hydrophobic-superoleophobic material |
| CN107400910B (en) * | 2017-06-01 | 2019-04-19 | 中国南方电网有限责任公司超高压输电公司贵阳局 | A kind of electroplating technology that high voltage direct current converter valve screening electrodes detecting probe surface finish can be improved |
| CN110791785B (en) * | 2019-11-06 | 2020-10-16 | 山东科技大学 | Electrodeposition layer-lyophobic-super-slippery triple film with composite anticorrosion function and preparation method and application thereof |
| CN111736378A (en) | 2020-06-17 | 2020-10-02 | Tcl华星光电技术有限公司 | Substrate, preparation method thereof and display panel |
| CN112376089B (en) * | 2020-10-09 | 2022-03-22 | 江苏大学 | Preparation method of stainless steel super-hydrophobic surface with infiltration anisotropy |
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| CN1477237A (en) * | 2003-07-10 | 2004-02-25 | 上海交通大学 | Brass-plating process in alkaline solution and its electroplating solution formula |
| JP4057626B2 (en) * | 2006-08-11 | 2008-03-05 | 株式会社神戸製鋼所 | Electrical Zn-plated steel sheet with excellent stain resistance |
| KR101569460B1 (en) * | 2013-02-08 | 2015-11-16 | 국민대학교 산학협력단 | superamphiphobic structure and method of manufacturing the same |
| CN104878430A (en) * | 2015-04-17 | 2015-09-02 | 大连理工大学 | Process method for preparing super-amphiphobic zinc surface |
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