CN109518238A - The method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite - Google Patents
The method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite Download PDFInfo
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- CN109518238A CN109518238A CN201811507444.9A CN201811507444A CN109518238A CN 109518238 A CN109518238 A CN 109518238A CN 201811507444 A CN201811507444 A CN 201811507444A CN 109518238 A CN109518238 A CN 109518238A
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- nickel
- electroplate liquid
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- hydrophobic
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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
- C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- 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
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The present invention discloses the method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite.240~280g/L of nickel sulfate, 40~60g/L of nickel chloride, 40~60g/L of boric acid and saccharin 5~10g/L solvent are placed in container by the present invention first, distilled water is added, temperature is controlled at 40~65 DEG C, it is uniform that concussion is sufficiently stirred, ammonium hydroxide is added to control pH 3.8~4.5, as basic electroplate liquid；Nickel powder and silicon carbide are put into ball mill with the ratio of 5:1 and mixed, the mixed-powder of 2~20 g/L is then taken to be added in electroplate liquid；Again using the conductive metals such as stainless steel, copper as cathode, pure nickel or graphitic carbon are electroplated in the environment of vertical magnetic field as anode.Workpiece will have been plated after the completion of plating to be cleaned with distilled water, has been dried up, i.e., the nickel carbon SiClx composite deposite with super hydrophobic functional is obtained in surface of workpiece.Electroplating bath components of the invention are simple, and it is convenient to prepare, and process is sufficiently stable, and the contact angle of prepared coating is in 150~160 ° of ranges, and roll angle is less than 10 °.
Description
Technical field
The present invention relates to a kind of electro-deposition processing technology, it is multiple to prepare super-hydrophobic nickel carbon SiClx for specifically metal surface
The method for closing coating.
Background technique
The contact angle that super hydrophobic surface generally refers to water is greater than 150 °, and roll angle is less than 10 °.Nature has many super-hydrophobic
Phenomenon, such as lotus leaf surface, cicada and the wing of butterfly all have apparent superhydrophobic characteristic.Super hydrophobic surface has waterproof, prevents
Mist, snow defence, anti-pollution, anti-oxidant, anticorrosion and automatically cleaning and important features are waited, it is all in scientific research and production, life etc.
There is extremely wide application prospect in multi-field.Anti-corrosion of the super-hydrophobic technology for building industry, auto industry, metal industry etc.
Antirust and antifouling also there is very much realistic meaning.
One kind that jet-electrodeposited method is deposited as Local electrochemical have current density is big, current efficiency is high, locality is strong,
Simple process, it is at low cost the advantages that, in jet-electrodeposited method process, electrolyte sprayed in the form of high-speed jet cathode into
Row electro-deposition, this strong turbulent fluxus formae, accelerates the mixing speed of solution, reduces the thickness of diffusion layer, enhance
Activation polarization, greatly improves limiting current density, deposition rate of metal greatly improves, and realizes the part of higher efficiency
Electro-deposition.Cooperate induced by magnetic field technology, to quickly prepare super-hydrophobic coating.Application number 201811253935.5 discloses one kind
Nano-nickel powder, deposition process is added in the device and method that induced by magnetic field scan electrodepositing prepares super-hydrophobic coating in electroplate liquid
Middle addition magnetic field auxiliary device obtains super-hydrophobic nano nickel coating.
As previously mentioned, nickel metal is widely used in the industrial circles such as electrical and Aeronautics and Astronautics field, but since its is hydrophilic
Property influences its anti-corrosion, automatically cleaning and the performances such as anti-icing.Silicon carbide makees new ceramics, has splendid abrasion resistance and hardness, can be into
The wearability that one step increases super-hydrophobic coating improves its service life.This patent, which has been invented to have in metallic substrate surface preparation for the first time, to be surpassed
The nickel carbon SiClx composite deposite of hydrophobic performance, preparation method is simple, low in cost, and is easy to industrialization large-scale production.
Summary of the invention
The present invention is the nickel carbon SiClx mixed-powder being added into electroplate liquid, in perpendicular magnetic by lower-cost method
It is electroplated in the environment of field, in the method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite.
The present invention uses following technical proposal:
The method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite, including the following steps::
1) workpiece pre-processes: workpiece first being used to 400 mesh, 800 mesh and the polishing of 1200 mesh sand paper, is then cleaned by ultrasonic with dehydrated alcohol
10min is finally cleaned with pure water, and drying obtains treated workpiece；
2) configure electroplate liquid: by 240~280g/L of nickel sulfate, 40~60g/L of nickel chloride, 40~60g/L of boric acid and saccharin 5~
10g/L solvent is placed in container, and distilled water is added, and concussion is sufficiently stirred uniformly, as basic electroplate liquid；
3) nickel powder (250nm) and silicon carbide powder (50nm) are put into ball mill with 5: 1 ratio and are mixed；
4) mixed powder is added in electroplate liquid, is stirred evenly；
5) existed as anode using the electroplate liquid that step 4) mixes using treated workpiece as cathode, pure nickel or graphitic carbon
It is electroplated in the environment of vertical magnetic field, cathode-workpiece coating is cleaned after plating, drying, obtain the nickel carbon of super hydrophobic functional
SiClx coating.
Preferentially, in step 1, the workpiece is copper, stainless steel conductive metallic material.
Preferentially, in step 2, the pH of electroplate liquid is controlled 3.8~4.5.
Preferentially, in step 3, the revolving speed of ball mill will be controlled in 100-200rpm, and ratio of grinding media to material will be controlled 3: 1~4:
1, the time of ball milling is 4-6h.
Preferentially, in step 4, the control of mixed-powder concentration uses 100~200 revs/min of magnetic force in 2~20g/L, stirring
Blender stirs 30~60min.
Preferentially, in steps of 5, vertical magnetic field refers to that magnetic direction is identical as direction of an electric field, and magnetic field will be uniform magnetic field,
For current density of the magnetic field strength in 50~500mT, electroplating process in 50~500A/dm2, electroplating time is 20~40min.
Preferentially, in steps of 5, the temperature of electroplate liquid is controlled at 40~65 DEG C in electroplating process.
The invention has the following beneficial effects:
1, preparation method of the invention can prepare super-hydrophobic nickel carbon SiClx Composite Coatings on all conductive metallic material surfaces
Layer.
2, a small amount of nickel carbon SiClx mixed-powder need to be only added in the present invention in electroplate liquid, and concentration is controlled in 2-10g/L,
Cost is significantly reduced, environmental pollution is reduced it is not necessary that other reagents are added compared to other super-hydrophobic coating technologies of preparing.
3, the vertical magnetic field that the present invention only needs intensity weaker can prepare composite deposite.
4, the coating obtained by the present invention has superhydrophobic property, no longer needs to be chemically modified.
5, content of the silicon carbide in coating greatly improved in the present invention, and cladding wearability is good.
6, nickel carbon SiClx coating surface is smooth, uniform, has superhydrophobic characteristic, contact angle is in 150~165 ° of ranges, rolling
Angle is moved less than 10 °.Super-hydrophobic nickel carbon SiClx composite deposite prepared by the present invention can be applied to a variety of industrial part outer surfaces and
Metal pipe internal wall etc. needs automatically cleaning, corrosion-resistant, freezing and reduces the various occasions such as water resistance.
Detailed description of the invention
Fig. 1 a~Fig. 1 d is respectively the contact angle figure of super-hydrophobic nickel carbon SiClx composite deposite obtained by Examples 1 to 4.
Fig. 2 a~Fig. 2 d is respectively the scanning electron microscope (SEM) photograph of coating surface obtained by example example 1~4.
Specific embodiment
Further detailed description is done to the present invention below with reference to example, but the scope of protection of present invention is not limited to
This.
Embodiment 1
The method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite, the specific steps are as follows:
Copper sheet workpiece is first used into 400 mesh, 800 mesh and the polishing of 1200 mesh sand paper, is then cleaned by ultrasonic with dehydrated alcohol
10min is finally cleaned with pure water, drying, for use.
Nickel sulfate 260g/L, nickel chloride 40g/L, boric acid 40g/L and saccharin 5g/L solvent are placed in container, is added and steams
Concussion is sufficiently stirred uniformly, as basic electroplate liquid in distilled water.
Nickel powder (250nm) and silicon carbide powder (50nm) are put into ball mill with 5: 1 ratio, rotational speed of ball-mill is
The time of 200rpm, ratio of grinding media to material 4: 1, ball milling are 4h, and mixed powder are added in electroplate liquid, concentration 2g/L,
30min is stirred under 100 revs/min with magnetic stirring apparatus.
Using treated copper sheet as cathode, pure nickel is in magnetic field strength as anode, using the electroplate liquid mixed
It is electroplated in the environment of 50mT vertical magnetic field, using DC power supply, current density 100A/cm2Copper is taken out after plating 30min
Piece is cleaned, drying with pure water, and obtaining contact angle is 152.8 °, the super-hydrophobic nickel carbon SiClx composite deposite that roll angle is 8 °,
Its contact angle figure is as shown in Figure 1a, and coating surface morphology is as shown in Figure 2 a.
Embodiment 2
The method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite, the specific steps are as follows:
Copper sheet workpiece is first used into 400 mesh, 800 mesh and the polishing of 1200 mesh sand paper, is then cleaned by ultrasonic with dehydrated alcohol
10min is finally cleaned with pure water, drying, for use.
Nickel sulfate 260g/L, nickel chloride 40g/L, boric acid 40g/L and saccharin 5g/L solvent are placed in container, is added and steams
Concussion is sufficiently stirred uniformly, as basic electroplate liquid in distilled water.
Nickel powder (250nm) and silicon carbide powder (50nm) are put into ball mill with 5: 1 ratio, rotational speed of ball-mill is
The time of 200rpm, ratio of grinding media to material 4: 1, ball milling are 4h, and mixed powder are added in electroplate liquid, concentration 4g/L,
30min is stirred under 100 revs/min with magnetic stirring apparatus.
Using treated copper sheet as cathode, pure nickel is in magnetic field strength as anode, using the electroplate liquid mixed
It is electroplated in the environment of 100mT vertical magnetic field, using DC power supply, current density is to take out after 30min is electroplated in 150A/cm2
Copper sheet is cleaned, drying with pure water, and obtaining contact angle is 157.3 °, the super-hydrophobic nickel carbon SiClx Composite Coatings that roll angle is 5 °
Layer, contact angle figure is as shown in Figure 1 b, and coating surface morphology is as shown in Figure 2 b.
Embodiment 3
The method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite, the specific steps are as follows:
Stainless steel work-piece is first used to 400 mesh, 800 mesh and the polishing of 1200 mesh sand paper, is then cleaned by ultrasonic with dehydrated alcohol
10min is finally cleaned with pure water, drying, for use.
Nickel sulfate 260g/L, nickel chloride 40g/L, boric acid 40g/L and saccharin 5g/L solvent are placed in container, is added and steams
Concussion is sufficiently stirred uniformly, as basic electroplate liquid in distilled water.
Nickel powder (250nm) and silicon carbide powder (50nm) are put into ball mill with 5: 1 ratio, rotational speed of ball-mill is
The time of 200rpm, ratio of grinding media to material 4: 1, ball milling are 4h, and mixed powder are added in electroplate liquid, concentration 6g/L,
30min is stirred under 100 revs/min with magnetic stirring apparatus.
Using treated copper sheet as cathode, pure nickel is in magnetic field strength as anode, using the electroplate liquid mixed
It is electroplated in the environment of 150mT vertical magnetic field, using DC power supply, current density 100A/cm2It is taken out after plating 30min
Copper sheet is cleaned, drying with pure water, and obtaining contact angle is 150.5 °, the super-hydrophobic nickel carbon SiClx Composite Coatings that roll angle is 7 °
Layer, as illustrated in figure 1 c, coating surface morphology is as shown in Figure 2 c for contact angle figure.
Embodiment 4
The method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite, the specific steps are as follows:
Stainless steel work-piece is first used to 400 mesh, 800 mesh and the polishing of 1200 mesh sand paper, is then cleaned by ultrasonic with dehydrated alcohol
10min is finally cleaned with pure water, drying, for use.
Nickel sulfate 260g/L, nickel chloride 40g/L, boric acid 40g/L and saccharin 5g/L solvent are placed in container, is added and steams
Concussion is sufficiently stirred uniformly, as basic electroplate liquid in distilled water.
Nickel powder (250nm) and silicon carbide powder (50nm) are put into ball mill with 5: 1 ratio, rotational speed of ball-mill is
The time of 200rpm, ratio of grinding media to material 4: 1, ball milling are 4h, and mixed powder are added in electroplate liquid, concentration 8g/L,
30min is stirred under 100 revs/min with magnetic stirring apparatus.
Using treated copper sheet as cathode, pure nickel is in magnetic field strength as anode, using the electroplate liquid mixed
It is electroplated in the environment of 200mT vertical magnetic field, using DC power supply, current density 150A/cm2It is taken out after plating 30min
Copper sheet is cleaned, drying with pure water, and obtaining contact angle is 158.1 °, the super-hydrophobic nickel carbon SiClx Composite Coatings that roll angle is 3 °
Layer, contact angle figure is as shown in Figure 1 d, and coating surface morphology is as shown in Figure 2 d.
Claims (7)
1. the method that metal surface prepares super-hydrophobic nickel carbon SiClx composite deposite, it is characterised in that the following steps are included:
1) workpiece pre-processes: workpiece first being used to 400 mesh, 800 mesh and the polishing of 1200 mesh sand paper, is then cleaned by ultrasonic with dehydrated alcohol
10min is finally cleaned with pure water, and drying obtains treated workpiece；
2) configure electroplate liquid: by 240~280g/L of nickel sulfate, 40~60g/L of nickel chloride, 40~60g/L of boric acid and saccharin 5~
10g/L solvent is placed in container, and distilled water is added, and concussion is sufficiently stirred uniformly, as basic electroplate liquid；
3) nickel powder (250nm) and silicon carbide powder (50nm) are put into ball mill with 5: 1 ratio and are mixed；
4) mixed powder is added in electroplate liquid, is stirred evenly；
5) existed as anode using the electroplate liquid that step 4) mixes using treated workpiece as cathode, pure nickel or graphitic carbon
It is electroplated in the environment of vertical magnetic field, cathode-workpiece coating is cleaned after plating, drying, obtain the nickel carbon of super hydrophobic functional
SiClx coating.
2. according to claims 1, step 2) the stirring concussion uses 100~300W power ultrasonic, 10~20min of ultrasound,
100~200 revs/min of 20~30min of magnetic stirrer.
3. the pH of step 2) electroplate liquid is controlled 3.8~4.5 according to claims 1.
4. the revolving speed of step 3) ball mill will be controlled in 100-200rpm, and ratio of grinding media to material will be controlled 3: 1 according to claims 1
~4: 1, the time of ball milling is 4-6h.
5. the control of step 4) mixed-powder concentration uses 100~200 revs/min in 2~20g/L, stirring according to claims 1
30~60min of magnetic stirrer.
6. step 5) vertical magnetic field refers to that magnetic direction is identical as direction of an electric field according to claims 1, magnetic field will be even strong magnetic
, current density of the magnetic field strength in 50~500mT, electroplating process in 50~500A/dm2, electroplating time is 20~
40min。
7. the temperature of electroplate liquid is controlled at 40~65 DEG C in step 5) electroplating process according to claims 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112941494A (en) * | 2021-03-10 | 2021-06-11 | 宿辉 | A kind of (SiC) with lotus leaf effectPPreparation method of super-hydrophobic membrane layer |
| CN114932236A (en) * | 2022-05-18 | 2022-08-23 | 江苏大学 | Preparation method of continuous laser direct forming super-hydrophobic nickel-based surface |
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| CN102677132A (en) * | 2012-05-28 | 2012-09-19 | 大连理工大学 | Method for preparing super-hydrophobic coating of metallic matrix |
| CN106591899A (en) * | 2016-11-17 | 2017-04-26 | 哈尔滨工程大学 | Magnesium-lithium alloy super-hydrophobic coating with photoinduced hydrophily-hydrophobicity conversion function and preparation method for magnesium-lithium alloy super-hydrophobic coating |
| CN107502003A (en) * | 2016-06-14 | 2017-12-22 | 中国科学院理化技术研究所 | A kind of preparation method of hydrophobic inorganic powder body material |
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2018
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Patent Citations (3)
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| CN102677132A (en) * | 2012-05-28 | 2012-09-19 | 大连理工大学 | Method for preparing super-hydrophobic coating of metallic matrix |
| CN107502003A (en) * | 2016-06-14 | 2017-12-22 | 中国科学院理化技术研究所 | A kind of preparation method of hydrophobic inorganic powder body material |
| CN106591899A (en) * | 2016-11-17 | 2017-04-26 | 哈尔滨工程大学 | Magnesium-lithium alloy super-hydrophobic coating with photoinduced hydrophily-hydrophobicity conversion function and preparation method for magnesium-lithium alloy super-hydrophobic coating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112941494A (en) * | 2021-03-10 | 2021-06-11 | 宿辉 | A kind of (SiC) with lotus leaf effectPPreparation method of super-hydrophobic membrane layer |
| CN114932236A (en) * | 2022-05-18 | 2022-08-23 | 江苏大学 | Preparation method of continuous laser direct forming super-hydrophobic nickel-based surface |
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Application publication date: 20190326 |