CN103409779A - Method for preparing super-hydrophobic surface by nano-composite electro-brush plating - Google Patents

Method for preparing super-hydrophobic surface by nano-composite electro-brush plating Download PDF

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CN103409779A
CN103409779A CN2013103204720A CN201310320472A CN103409779A CN 103409779 A CN103409779 A CN 103409779A CN 2013103204720 A CN2013103204720 A CN 2013103204720A CN 201310320472 A CN201310320472 A CN 201310320472A CN 103409779 A CN103409779 A CN 103409779A
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concentration
plating
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composite
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CN103409779B (en
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刘洪涛
汪雪梅
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China University of Mining and Technology CUMT
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China University of Mining and Technology CUMT
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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
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/04—Electroplating with moving electrodes
    • C25D5/06—Brush or pad plating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
    • 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
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt

Abstract

A method for preparing a super-hydrophobic surface by nano-composite electro-brush plating belongs to the method for preparing of the super-hydrophobic surface. The method comprises the following steps: step1, preparation of plating: firstly, polishing carbon steel basal body, wherein the surface roughness Ra is 0.8, and then drying after cleaning; sedimentating double-layered nano-composite plating with micro-nano double coarse structure on the carbon steel basal body according to the process order of electrocleaning-second actification-third actification-bottom layer plating-plating of nanometer C/Ni composite plating-plating of nanometer Cu/Ni composite plating, using deionized water to wash after each step is finished, and then conducting next step; placing brush plated sample into alcohol, washing for 30 min in an ultrasonic cleaner, placing in a drying box at the temperature of 60 DEG C to dry for 1 h; step2, surface chemical modification: placing dried sample in prepared silicon fluoride solution to soak for 40 min at the temperature of 60 DEG C, wherein the mass ratio of Actyflon-G607 and absolute ethyl alcohol is 1:49, and taking out to dry in the drying box at the temperature of 100 DEG C for 1 h.

Description

A kind of nano combined Brush Plating prepares the method for super hydrophobic surface
Technical field
The present invention relates to a kind of method for preparing hydrophobic surface, particularly a kind of nano combined Brush Plating prepares the method for super hydrophobic surface.
Background technology
Super hydrophobic surface, due to the performance that many excellences are arranged, such as self-cleaning function, waterproof, freezing, protection against corrosion etc., all has broad application prospects in a lot of fields.The super hydrophobic surface of knowing the most is exactly lotus leaf, and lotus leaf has excellent ultra-hydrophobicity and outstanding self-cleaning function.The preparation of super hydrophobic surface and applied research are all scientist's study hotspots all the time.The researchist has summed up two methods that prepare super hydrophobic surface: a kind of is the micro-nano dual coarse structure of preparation on the material of low surface energy, a kind of be surface can be higher material on first prepare micro-nano dual coarse structure, with the material of low surface energy, it is modified again, show to obtain surperficial energy to reduce coarse structure.For smooth solid material, though it have minimum surface can, it reaches 120 ° with the contact angle of water also multipotency, at the micro-nano dual coarse structure of material surface structure, is therefore the key for preparing super hydrophobic surface.
At present existing many methods that prepare super hydrophobic surface in metallic surface, as solution soaking method, electrochemical deposition method, chemical corrosion method, anonizing, chemical deposition etc.But also there are many deficiencies in existing technology, as not high as surperficial physical strength, the technological process more complicated, surface abrasion resistance persistence deficiency, higher to the requirement of equipment, be difficult to realize large-scale preparation.Therefore super hydrophobic surface still is in the basic research stage at present, and the practical application of its mass-producing is restricted.
Summary of the invention
The objective of the invention is to provide a kind of nano combined Brush Plating to prepare the method for super hydrophobic surface, solve the surperficial physical strength existed in current super hydrophobic surface preparation process not high, the technological process more complicated, surface abrasion resistance persistence deficiency, be difficult to the problem that realizes prepared by big area.
The object of the present invention is achieved like this: the super hydrophobic surface method of preparation is divided two steps:
Step 1, nano-composite plate preparation: at first by the plain steel polishing, surface roughness Ra 0.8, clean post-drying;
The required clean liquid of electricity of preparation Brush Plating, No. two activation solutions, No. three activation solutions, special nickel solution, the compound Ni plating solution of nanometer C particle, the compound Ni plating solution of nanometer Cu;
Process sequence according to-No. tri-activation-plating bottom-plating nanometer C/Ni composite deposite-plating nanometer Cu/Ni composite deposites of clean-No. bis-activation of electricity deposits the double-layer nanometer composite deposite with micro-nano dual coarse structure on plain steel, after each step completes, use the deionized water rinsing sample, so carry out again next step;
The brush-plating technique parameter of each operation: the clean operation of electricity applies voltage+6V, time 30s, speed of relative movement 4-8m/min; No. two activation procedures, apply voltage-6V, time 30s, speed of relative movement 5-10m/min; No. three activation procedures, apply voltage-8V, time 30s, speed of relative movement 5-10m/min; Plating bottom operation, apply voltage+10V, time 90s, speed of relative movement 6-8m/min; Plating nanometer C/Ni composite deposite operation, apply voltage+15V, time 90s, speed of relative movement 6-8m/min; Plating nanometer Cu/Ni composite deposite operation, apply voltage+15V, time 90s, speed of relative movement 8-12m/min;
The sample that brush plating is complete is put into alcohol, and cleans 30 minutes in ultrasonic cleaner, then puts into 60 ℃ of drying bakers oven dry 1 hour;
Step 2, surface chemical modification:
The sample of oven dry is put into to the silicon fluoride solution of preparation, in silicon fluoride solution, the mass ratio of ten trifluoro octyl group Trimethoxy silanes and dehydrated alcohol is 1:49, soaks 40 minutes under 60 ℃, takes out in the baking oven of 100 ℃ and dries 1 hour, gets final product;
The clean liquid of described electricity comprises: sodium hydroxide (NaOH), concentration 25.0g/L, sodium carbonate (Na 2CO 3), concentration 21.7g/L, tertiary sodium phosphate (Na 3PO 4), concentration 50.0g/L and sodium-chlor (NaCI), concentration 2.4g/L;
Described No. two activation solutions comprise: hydrochloric acid (HCI), concentration 25.0g/L and sodium-chlor (NaCI), concentration 140.0g/L;
Described No. three activation solutions comprise: nickelous chloride (NiCl 2.6H 2O), concentration 3.0g/L, trisodium citrate (Na 3C 6H 5O 7.2H 2O), concentration 142.2g/L, citric acid (H 3C 6H 5O 7), concentration 94.2g/L and ammonium oxalate (NaCI), concentration 0.1g/L;
Described special nickel solution comprises: NiSO 47H2O, concentration 400g/L, NiCl 26H 2O, concentration 20g/L, CH 3COOH, concentration 68g/L and HCl (concentration 30%), concentration 20g/L;
The compound Ni plating solution of described nanometer C particle comprises: NiSO 46H 2O, concentration 254g/L, NH 3H 2O(NH 3Content 25% ︿ 28%), concentration 105mL/L, (NH4) 3C 6H 5O 7, concentration 56g/L, CH 3COONH 4, concentration 23g/L, sodium lauryl sulphate (CH 3(CH 2) 10CH 2OSO 3Na), concentration 0.1g/L, ammonium oxalate (C 2H 8N 2O 4H 2O), concentration 0.1g/L and nano-carbon powder, concentration 15g/L;
The compound Ni plating solution of described nanometer Cu particle comprises: NiSO 46H 2O, concentration 254g/L, NH 3H 2O(NH 3Content 25% ︿ 28%), concentration 105mL/L, (NH 4) 3C 6H 5O 7, concentration 56g/L, CH 3COONH 4, concentration 23g/L, CH 3COOH, concentration 56g/L, sodium lauryl sulphate (CH 3(CH 2) 10CH 2OSO 3Na), concentration 0.1g/L, ammonium oxalate (C 2H 8N 2O 4H 2O) concentration 0.1g/L, copper nanoparticle, concentration 5g/L and additive X, concentration 56g/L.
Beneficial effect, owing to having adopted such scheme, adopt nano combined Brush Electroplating Technique to prepare super hydrophobic surface, to super hydrophobic surface big area technology of preparing and apply significant.Applied fully that the equipment that Brush Electroplating Technique has is light, technique flexibly, the coating kind is various, coat binding strength is high, efficient and can prepare big area coating advantage, adopt suitable processing condition brush plating nanometer C/Ni and bis-layers of composite deposite of nanometer Cu/Ni on plain steel can prepare super hydrophobic surface, coating surface is micro-nano dual coarse structure, similar to the lotus leaf surface microtexture; When operating voltage is 15V, brush plating speed is 8m/min, when nano copper particle concentration is the 5g/L left and right, is optimal processing parameter, and the contact angle maximum of coating can reach 155.5 ± 0.9 °, and roll angle is 5 °; Coating has been compared frictional behaviour and corrosion resistance nature preferably with the matrix carbon steel.Can be to the protection of surface, naval vessel and hull surface equipment.Naval vessel moves in water, its surface will be subject to the corrosion of the oxygen in water and atmosphere, after the plating nano-deposit, realizes surface super hydrophobic, reduces the corrosion to matrix of water and oxygen.Solved the surperficial physical strength existed in current super hydrophobic surface preparation process not high, the technological process more complicated, surface abrasion resistance persistence deficiency, be difficult to the problem that realizes prepared by big area.
Advantage:
1, can realize the big area preparation of super hydrophobic surface, for the industrial applications of super hydrophobic surface provides feasibility;
2, equipment is simple and reliable.Brush electroplating device is only a brush plating power supply, and volume is little, lightweight, easily mobile, can be portable, and price is low;
3, coating surface is micro-nano dual coarse structure, similar to the lotus leaf surface microtexture, and the contact angle of coating can reach 155.5 ± 0.9 °, and roll angle is only 5 °, and hydrophobic effect is good.
4, coating has been compared frictional behaviour and corrosion resistance nature preferably, long perfomance life with the matrix carbon steel.
Embodiment
Embodiment 1: the super hydrophobic surface method of preparation is divided two steps:
Step 1, nano-composite plate preparation:
At first by the polishing of Q345 plain steel, surface roughness Ra 0.8, clean post-drying.
The required clean liquid of electricity of preparation Brush Plating, No. two activation solutions, No. three activation solutions, special nickel solution, the compound Ni plating solution of nanometer C particle, the compound Ni plating solution of nanometer Cu;
Process sequence according to-No. tri-activation-plating bottom-plating nanometer C/Ni composite deposite-plating nanometer Cu/Ni composite deposites of clean-No. bis-activation of electricity deposits the double-layer nanometer composite deposite with micro-nano dual coarse structure on plain steel, after each step completes, use the deionized water rinsing sample, so carry out again next step;
The brush-plating technique parameter of each operation: the clean operation of electricity applies voltage+6V, time 30s, speed of relative movement 4-8m/min; No. two activation procedures, apply voltage-6V, time 30s, speed of relative movement 5-10m/min; No. three activation procedures, apply voltage-8V, time 30s, speed of relative movement 5-10m/min; Plating bottom operation, apply voltage+10V, time 90s, speed of relative movement 6-8m/min; Plating nanometer C/Ni composite deposite operation, apply voltage+15V, time 90s, speed of relative movement 6-8m/min; Plating nanometer Cu/Ni composite deposite operation, apply voltage+15V, time 90s, speed of relative movement 8-12m/min;
The sample that brush plating is complete is put into alcohol, and cleans 30 minutes in ultrasonic cleaner, then puts into 60 ℃ of drying bakers oven dry 1 hour;
Step 2, surface chemical modification:
The sample of oven dry is put into to the silicon fluoride solution of preparation, in silicon fluoride solution, the mass ratio of ten trifluoro octyl group Trimethoxy silanes and dehydrated alcohol is 1:49, soaks 40 minutes under 60 ℃, takes out in the baking oven of 100 ℃ and dries 1 hour, gets final product;
The clean liquid of described electricity comprises: sodium hydroxide (NaOH), concentration 25.0g/L, sodium carbonate (Na 2CO 3), concentration 21.7g/L, tertiary sodium phosphate (Na 3PO 4), concentration 50.0g/L and sodium-chlor (NaCI), concentration 2.4g/L;
Described No. two activation solutions comprise: hydrochloric acid (HCI), concentration 25.0g/L and sodium-chlor (NaCI), concentration 140.0g/L;
Described No. three activation solutions comprise: nickelous chloride (NiCl 2.6H 2O), concentration 3.0g/L, trisodium citrate (Na 3C 6H 5O 7.2H 2O), concentration 142.2g/L, citric acid (H 3C 6H 5O 7), concentration 94.2g/L and ammonium oxalate (NaCI), concentration 0.1g/L;
Described special nickel solution comprises: NiSO 47H2O, concentration 400g/L, NiCl 26H 2O, concentration 20g/L, CH 3COOH, concentration 68g/L and HCl (concentration 30%), concentration 20g/L;
The compound Ni plating solution of described nanometer C particle comprises: NiSO 46H 2O, concentration 254g/L, NH 3H 2O(NH 3Content 25% ︿ 28%), concentration 105mL/L, (NH4) 3C 6H 5O 7, concentration 56g/L, CH 3COONH 4, concentration 23g/L, sodium lauryl sulphate (CH 3(CH 2) 10CH 2OSO 3Na), concentration 0.1g/L, ammonium oxalate (C 2H 8N 2O 4H 2O), concentration 0.1g/L and nano-carbon powder, concentration 15g/L;
The compound Ni plating solution of described nanometer Cu particle comprises: NiSO 46H 2O, concentration 254g/L, NH 3H 2O(NH 3Content 25% ︿ 28%), concentration 105mL/L, (NH 4) 3C 6H 5O 7, concentration 56g/L, CH 3COONH 4, concentration 23g/L, CH 3COOH, concentration 56g/L, sodium lauryl sulphate (CH 3(CH 2) 10CH 2OSO 3Na), concentration 0.1g/L, ammonium oxalate (C 2H 8N 2O 4H 2O) concentration 0.1g/L, copper nanoparticle, concentration 5g/L and additive X, concentration 56g/L.

Claims (1)

1. a nano combined Brush Plating prepares the method for super hydrophobic surface, and it is characterized in that: the super hydrophobic surface method of preparation is divided two steps:
Step 1, nano-composite plate preparation:
At first by the polishing of Q345 plain steel, surface roughness Ra 0.8, clean post-drying;
The required clean liquid of electricity of preparation Brush Plating, No. two activation solutions, No. three activation solutions, special nickel solution, the compound Ni plating solution of nanometer C particle, the compound Ni plating solution of nanometer Cu;
Process sequence according to-No. tri-activation-plating bottom-plating nanometer C/Ni composite deposite-plating nanometer Cu/Ni composite deposites of clean-No. bis-activation of electricity deposits the double-layer nanometer composite deposite with micro-nano dual coarse structure on plain steel, after each step completes, use the deionized water rinsing sample, so carry out again next step;
The brush-plating technique parameter of each operation: the clean operation of electricity applies voltage+6V, time 30s, speed of relative movement 4-8m/min; No. two activation procedures, apply voltage-6V, time 30s, speed of relative movement 5-10m/min; No. three activation procedures, apply voltage-8V, time 30s, speed of relative movement 5-10m/min; Plating bottom operation, apply voltage+10V, time 90s, speed of relative movement 6-8m/min; Plating nanometer C/Ni composite deposite operation, apply voltage+15V, time 90s, speed of relative movement 6-8m/min; Plating nanometer Cu/Ni composite deposite operation, apply voltage+15V, time 90s, speed of relative movement 8-12m/min;
The sample that brush plating is complete is put into alcohol, and cleans 30 minutes in ultrasonic cleaner, then puts into 60 ℃ of drying bakers oven dry 1 hour;
Step 2, surface chemical modification:
The sample of oven dry is put into to the silicon fluoride solution of preparation, in silicon fluoride solution, the mass ratio of ten trifluoro octyl group Trimethoxy silanes and dehydrated alcohol is 1:49, soaks 40 minutes under 60 ℃, takes out in the baking oven of 100 ℃ and dries 1 hour, gets final product;
The clean liquid of described electricity comprises: sodium hydroxide (NaOH), concentration 25.0g/L, sodium carbonate (Na 2CO 3), concentration 21.7g/L, tertiary sodium phosphate (Na 3PO 4), concentration 50.0g/L and sodium-chlor (NaCI), concentration 2.4g/L;
Described No. two activation solutions comprise: hydrochloric acid (HCI), concentration 25.0g/L and sodium-chlor (NaCI), concentration 140.0g/L;
Described No. three activation solutions comprise: nickelous chloride (NiCl 2.6H 2O), concentration 3.0g/L, trisodium citrate (Na 3C 6H 5O 7.2H 2O), concentration 142.2g/L, citric acid (H 3C 6H 5O 7), concentration 94.2g/L and ammonium oxalate (NaCI), concentration 0.1g/L;
Described special nickel solution comprises: NiSO 47H2O, concentration 400g/L, NiCl 26H 2O, concentration 20g/L, CH 3COOH, concentration 68g/L and HCl (concentration 30%), concentration 20g/L;
The compound Ni plating solution of described nanometer C particle comprises: NiSO 46H 2O, concentration 254g/L, NH 3H 2O(NH 3Content 25% ︿ 28%), concentration 105mL/L, (NH4) 3C 6H 5O 7, concentration 56g/L, CH 3COONH 4, concentration 23g/L, sodium lauryl sulphate (CH 3(CH 2) 10CH 2OSO 3Na), concentration 0.1g/L, ammonium oxalate (C 2H 8N 2O 4H 2O), concentration 0.1g/L and nano-carbon powder, concentration 15g/L;
The compound Ni plating solution of described nanometer Cu particle comprises: NiSO 46H 2O, concentration 254g/L, NH 3H 2O(NH 3Content 25% ︿ 28%), concentration 105mL/L, (NH 4) 3C 6H 5O 7, concentration 56g/L, CH 3COONH 4, concentration 23g/L, CH 3COOH, concentration 56g/L, sodium lauryl sulphate (CH 3(CH 2) 10CH 2OSO 3Na), concentration 0.1g/L, ammonium oxalate (C 2H 8N 2O 4H 2O) concentration 0.1g/L, copper nanoparticle, concentration 5g/L and additive X, concentration 56g/L.
CN201310320472.0A 2013-07-26 2013-07-26 A kind of nano combined brush is coated with the method for standby super hydrophobic surface Active CN103409779B (en)

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PCT/CN2014/072214 WO2015010464A1 (en) 2013-07-26 2014-02-19 Method for preparing super-hydrophobic surface by means of nanocomposite electro brush plating

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CN103952732A (en) * 2014-04-11 2014-07-30 华南理工大学 Metal super-hydrophobic surface and preparation method thereof
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CN104532337A (en) * 2015-01-09 2015-04-22 中国矿业大学 Electro erosion method for rapidly preparing iron base super-hydrophobic surface in large area
CN104746118A (en) * 2015-04-20 2015-07-01 中国矿业大学 Method for preparing super-hydrophobic coating on steel substrate by virtue of Fe-based nano composite brush electroplating
CN105386101A (en) * 2015-12-23 2016-03-09 长春理工大学 Steel-base coupling bionic self-cleaning surface and preparation method thereof
CN105386090A (en) * 2015-11-09 2016-03-09 广东工业大学 Method for manufacturing ultra-oleophobic metal surface with recessed micropores
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CN107326406A (en) * 2017-07-04 2017-11-07 苏州热工研究院有限公司 A kind of protection of flow passage components narrow gap position erosion resistance layer, restorative procedure
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