CN104562052B - A kind of preparation method of stainless steel surfaces ordered micro-cellular structure - Google Patents
A kind of preparation method of stainless steel surfaces ordered micro-cellular structure Download PDFInfo
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- CN104562052B CN104562052B CN201410821884.7A CN201410821884A CN104562052B CN 104562052 B CN104562052 B CN 104562052B CN 201410821884 A CN201410821884 A CN 201410821884A CN 104562052 B CN104562052 B CN 104562052B
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Abstract
The present invention relates to a kind of preparation method of stainless steel surfaces ordered micro-cellular structure, belong to surface micro-structure preparing technical field, this method is a kind of electrochemical etching method, stainless steel after degreasing, electrochemical polish, nitric acid Passivation Treatment is put into the group water solution that phosphoric acid concentration is 15 50g/L, uses constant flow method in current density for 5 50A/dm2, temperature is to corrode 30 120min under 05 DEG C of process conditions, and acquisition aperture is homogeneous, the 550nm of aperture 200, the ordered micro-cellular structure that 13 μm of hole depth.The microcellular structure is in stainless steel surfaces in-situ preparation, in the absence of spallation problems；Microcellular structure any surface finish, stainless steel remain to keep original bright looking；Microcellular structure is by amorphous Cr2O3, Fe2O3Form, there is the wear and corrosion behavior better than stainless steel bulk material；Electrochemical corrosion and electrochemical polish can be carried out in plain electrolysers, and equipment is simple, and preparation cost is low, easily be promoted.
Description
Technical field
The present invention relates to a kind of preparation method of microcellular structure, and in particular to a kind of stainless steel surfaces ordered micro-cellular structure
Preparation method, belong to surface micro-structure preparing technical field.
Background technology
Stainless steel has the premium properties such as attractive in appearance, corrosion-resistant, the good, easy processing of ductility, in building, medicine equipment, food
The fields such as processing, household electrical appliance are using quite varied, such as building and ornament materials, elevator ＆ stairs handrail, railing, bio-medical material
Material, implantation material, operating theater instruments, food processing machinery, dining car, food-shelf, tank, cabinet, kitchen cabinet, laundry machine liner, shower
Device, water tank, door handle etc..
In recent years, more and more researchers turn one's attention to the preparation of stainless steel surfaces microcellular structure, to further open up
Its wide functional application.Such as, stainless steel surfaces microcellular structure can increase the absorptivity to light, its reflectivity be reduced, for too
Positive energy heat collector, it is possible to increase the utilization rate of solar energy；For coronary artery bracket bracket for eluting medicament, medicine is inserted into stainless steel watch
In the micropore of face, by discharging medicine during use, inflammatory reaction can be suppressed, control the generation of Vascular Restenosis after Balloom；For
Building surface, surface microporous structure can absorb microwave, infrared ray, sound wave, eliminate Contamination of Electromagnetic Wave, noise pollution, simultaneously
Also there is heat-insulating property；Microcellular structure is prepared on stainless steel tableware and cooking utensils surface, antiseptic elements are deposited in micropore, can be stainless
Steel part surface prepares antibacterial functions layer, is multiplied so as to suppress bacterium.
At present, the method that stainless steel surfaces prepare micropore mainly has chemical corrosion method and vacuum aluminum-coated+anodic oxidation compound
Method.Chemical corrosion method is that stainless steel is placed in certain acid solution, and a scale is formed to the corrosiveness of stainless steel surfaces using acid
Very little and micro- hole of density, hemispherical, 0.5-2 μm of the opening diameter in micro- hole, micro- hole depth is shallower and skewness, for above-mentioned
Functional material effect is undesirable.Vacuum aluminum-coated+anodizing is first deposited in stainless steel surfaces using physical vaporous deposition
A thin layer aluminium, nano-porous alumina microcellular structure, micro-pore diameter 25- are then prepared on aluminium coat surface using anodic oxidation
100nm, hole density are up to 109/cm2, it is good for above-mentioned functional material effect, but due to being deposited between aluminium coat and stainless steel substrate
In sharp interface, aluminium coat is easily peeled off from substrate surface.
Chinese invention 2005100241969, tubular reducing stainlss steel micro porous film and preparation method thereof disclose a kind of tubular type
Reducing stainlss steel micro porous film and preparation method thereof.The preparation method of this kind of film is that the stainless steel powder powder material for selecting different size is done
Supporting layer and key-course, by slurry made of the powder of stainless steel of two kinds of different sizes, synthesize on mould, burnt through high temperature
After knot, precision height is obtained, flux is big, the stainless steel microporous barrier containing reducing.This kind of film is particularly suitable for use in extreme environment
Working condition, such as high temperature, high pressure, high viscosity, high solids, easily pollution, it is desirable to long-term continuous operation, it is necessary to automatic backflushing and
The strict filtration condition such as cleaning and regeneration.In industrial technical fields such as chemical industry, environmental protection, atomic energy, medicine, food processings, have
Huge market potential.
The content of the invention
It is an object of the invention to provide a kind of process in stainless steel surfaces in-situ preparation ordered micro-cellular structure.This hair
The stainless steel surfaces micro-pore diameter of bright preparation is 200-550nm, and aperture is homogeneous, and hole depth is big（1-3 μm), pore arrangement is orderly, micro-
Pore structure is integral with matrix, and in the absence of spallation problems, and technique is simple, and it is low to prepare cost.Micropore knot prepared by the present invention
Structure has larger hole depth/aperture ratio, is adapted to prepare above-mentioned functional material.
The present invention mainly prepares equally distributed microcellular structure by electrochemical corrosive process in stainless steel surfaces：Will be stainless
After steel carries out degreasing, electrochemical polish, Passivation Treatment, it is rotten that electrochemistry is carried out to stainless steel curved beam using DC current regulator power supply
Erosion, makees anode by stainless steel curved beam, and high purity graphite piece makees negative electrode, is placed in the aqueous solution that phosphoric acid concentration is 15-50g/L and carries out electricity
Chemical attack.Electrochemical corrosive process：Negative electrode is with annode area than 3:1, cathode anode spacing 50mm, 0-5 DEG C of solution temperature, adopt
Electrochemical corrosion, current density 5-50A/dm are carried out with galvanostatic method2, etching time 30-120min.By controlling solution to match somebody with somebody
The technological parameters such as side, solution temperature, corrosion electric current density, etching time obtain the microcellular structure of certain pore size and thickness；
Comprise the following steps that：
（1）Stainless steel pre-processes：
1）Stainless steel is put into cleaner for metal and is cleaned by ultrasonic 15min, carries out ungrease treatment；
2）Electrochemical polish is carried out to the stainless steel after degreasing using DC current regulator power supply, obtains specular surface；Electricity
Surface with chemical polishing technology：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1, between cathode anode
Away from 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine form it is water-soluble
Liquid, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 minutes, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：The stainless steel curved beam after Passivation Treatment is carried out using DC current regulator power supply
Electrochemical corrosion, obtain ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode,
Negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is the water-soluble of 15-50g/L
Liquid, 0-5 DEG C of solution temperature, using galvanostatic method, current density 5-50A/dm2, etching time 30-120min；
, can be micro- by adjusting the phosphoric acid concentration size control of electrochemical corrosive liquid according to the purposes of stainless steel products and requirement
Bore dia, adjust electrochemical corrosion time control micropore depth；
Between each step, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step.
The technical characterstic of the present invention：1）Electrochemical corrosion is also used using the weaker phosphate aqueous solution of corrosivity, the present invention
The strong acid of various concentrations is crossed, if sulfuric acid, nitric acid are as corrosive liquid, but corrosion rate is too fast, and serious intercrystalline corrosion easily occurs
Or general corrosion, it is difficult to obtain equally distributed microcellular structure；2）Solution temperature is strict controlled in 0-5 DEG C in corrosion process, temperature
Higher easily generation intercrystalline corrosion or general corrosion are spent, is not easy to obtain equally distributed microcellular structure；3）Before electrochemical corrosion, first
Stainless steel is passivated processing in 50% salpeter solution, makes the fine and close oxide-film of stainless steel surfaces generation, through many experiments
Research finds that previously generating dense oxidation film helps to protect stainless steel that intercrystalline corrosion does not occur on electrochemical corrosion surface at initial stage
Or general corrosion, be advantageous to the generation of stainless steel surfaces ordered micro-cellular structure.
The microcellular structure formation mechenism of the present invention：Electrochemical corrosion course initial stage, protected by surface compact oxide-film, no
The general corrosion of rust steel surface is suppressed.But because the resistance of dense oxidation film is larger, under electric field action, dense oxidation film
There is random breakdown phenomenon in surface, causes surface electric field distribution uneven, and current strength is high at breakdown, accelerates dense oxidation film
Electrochemical corrosion, initially form micropore.Because stainless steel is anode, new passivating film (sun is still constantly formed in micropore bottom
React pole：,,MForCr、FeDeng）, therefore there is passivation-corruption in micropore bottom
- being passivated again-cyclic process corroded again is lost, causes hole constantly to develop to vertical-depth.Because power line is concentrated mainly on bottom hole,
So electrochemical corrosion occurs mainly in micropore bottom, and chemical attack mainly occurs for hole wall（,MForCr、FeDeng）, the main H in by solution of chemical attack+Ion concentration controls, so by controlling phosphorus acid content in solution, can
To control the dissolution velocity of hole wall, the microcellular structure of different pore size is obtained.The homogenization of micro-pore diameter is mainly by microporous layers
The effect of stress, reaching the homogenization of stress distribution causes., can be by controlling electrification according to the purposes of stainless steel products and requirement
Learn the microcellular structure that etching process prepares different pore size size and hole depth.
It is of the invention compared with existing stainless steel surfaces microcellular structure technology of preparing, advantage is：
（1）In stainless steel surfaces in-situ preparation microcellular structure, in the absence of spallation problems, and technique is simple.
（2）The microcellular structure aperture of preparation is homogeneous, and hole depth is big, and hole is evenly distributed.
（3）Stainless steel after electrochemical corrosion still keeps higher surface smoothness.
（4）Surface microporous structure is mainly by amorphous Cr2O3, Fe2O3Form, have better than stainless steel bulk material
Wear-resisting, decay resistance.
（5）Electrochemical corrosion and electrochemical polish can be carried out in plain electrolysers, and equipment is simple, and preparation cost is low,
Easily promote.
Brief description of the drawings
Fig. 1 is electrochemical corrosion device schematic diagram prepared by stainless steel surfaces microcellular structure；
Fig. 2 is the stainless steel surfaces microcellular structure SEM photograph prepared in embodiment 1；
Fig. 3 is the stainless steel surfaces microcellular structure SEM photograph prepared in embodiment 2；
Fig. 4 is the stainless steel surfaces microcellular structure SEM photograph prepared in embodiment 6；
Label declaration in figure：1st, anode；2nd, negative electrode；3rd, oxidation solution；4th, frozen water mixing bath；5th, stirrer；6th, temperature display
Screen；7th, temperature control magnetic stirring apparatus；8th, constant voltage dc source.
Embodiment
The present invention is described in further details below by example, these examples are only used for illustrating the present invention, and unlimited
The scope of the present invention processed.
For the stainless steel that the present invention uses for SUS304 type stainless steels, the chemical reagent of use is that analysis is pure, prepares solution
Water is deionized water.Electrochemical polish and electrochemical corrosion apparatus use WYK-15010K DC current regulator power supplies
（Voltage 0-150V, electric current 0-10A）, it is 0-5 DEG C to keep solution temperature, using with refrigeration in electrochemical corrosion course
The equipment of device.Meanwhile solution temperature is set to keep uniform using magnetic agitation.
Embodiment 1
The preparation method of stainless steel surfaces ordered micro-cellular structure mainly includes the following steps that：
（1）Stainless steel pre-processes：
1）Sample by 1mm thickness stainless steel plate wire cuttings into 30mm × 20mm；
2）Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；
3) electrochemical polish is carried out to the stainless steel after degreasing using WYK-15010K DC current regulator power supplies, obtains mirror
Face surface；Electrochemical polishing process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1,
Cathode anode spacing 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine
The aqueous solution of composition, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；Each step
Between, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 min, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：Using WYK-15010K DC current regulator power supplies to stainless after Passivation Treatment
Steel curved beam carries out electrochemical corrosion, obtains ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, Gao Chunshi
Ink sheet makees negative electrode, and negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is 15g/L
The aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 5A/dm2, etching time 120min；According to stainless
The purposes of steel part and requirement, micro-pore diameter, adjustment electrification can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid
Learn etching time control micropore depth.
Embodiment 2
The preparation method of stainless steel surfaces ordered micro-cellular structure mainly includes the following steps that：
（1）Stainless steel pre-processes：
1）Sample by 1mm thickness stainless steel plate wire cuttings into 30mm × 20mm；
2）Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；
3) electrochemical polish is carried out to the stainless steel after degreasing using WYK-15010K DC current regulator power supplies, obtains mirror
Face surface；Electrochemical polishing process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1,
Cathode anode spacing 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine
The aqueous solution of composition, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；Each step
Between, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 minutes, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：Using WYK-15010K DC current regulator power supplies to stainless after Passivation Treatment
Steel curved beam carries out electrochemical corrosion, obtains ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, Gao Chunshi
Ink sheet makees negative electrode, and negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is 15g/L
The aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 12.5A/dm2, etching time 120min；According to not
The purposes of rust steel part and requirement, micro-pore diameter, adjustment electricity can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid
Chemical attack time control micropore depth.
Embodiment 3
The preparation method of stainless steel surfaces ordered micro-cellular structure mainly includes the following steps that：
（1）Stainless steel pre-processes：
1）Sample by 1mm thickness stainless steel plate wire cuttings into 30mm × 20mm；
2）Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；
3) electrochemical polish is carried out to the stainless steel after degreasing using WYK-15010K DC current regulator power supplies, obtains mirror
Face surface；Electrochemical polishing process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1,
Cathode anode spacing 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine
The aqueous solution of composition, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；Each step
Between, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 minutes, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：Using WYK-15010K DC current regulator power supplies to stainless after Passivation Treatment
Steel curved beam carries out electrochemical corrosion, obtains ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, Gao Chunshi
Ink sheet makees negative electrode, and negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is 15g/L
The aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 25A/dm2, etching time 120min；According to stainless
The purposes of steel part and requirement, micro-pore diameter, adjustment electrification can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid
Learn etching time control micropore depth.
Embodiment 4
The preparation method of stainless steel surfaces ordered micro-cellular structure mainly includes the following steps that：
（1）Stainless steel pre-processes：
1）Sample by 1mm thickness stainless steel plate wire cuttings into 30mm × 20mm；
2）Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；
3) electrochemical polish is carried out to the stainless steel after degreasing using WYK-15010K DC current regulator power supplies, obtains mirror
Face surface；Electrochemical polishing process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1,
Cathode anode spacing 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine
The aqueous solution of composition, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；Each step
Between, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 minutes, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：Using WYK-15010K DC current regulator power supplies to stainless after Passivation Treatment
Steel curved beam carries out electrochemical corrosion, obtains ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, Gao Chunshi
Ink sheet makees negative electrode, and negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is 15g/L
The aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 37.5A/dm2, etching time 120min；According to not
The purposes of rust steel part and requirement, micro-pore diameter, adjustment electricity can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid
Chemical attack time control micropore depth.
Embodiment 5
The preparation method of stainless steel surfaces ordered micro-cellular structure mainly includes the following steps that：
（1）Stainless steel pre-processes：
1）Sample by 1mm thickness stainless steel plate wire cuttings into 30mm × 20mm；
2）Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；
3) electrochemical polish is carried out to the stainless steel after degreasing using WYK-15010K DC current regulator power supplies, obtains mirror
Face surface；Electrochemical polishing process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1,
Cathode anode spacing 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine
The aqueous solution of composition, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；Each step
Between, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 minutes, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：Using WYK-15010K DC current regulator power supplies to stainless after Passivation Treatment
Steel curved beam carries out electrochemical corrosion, obtains ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, Gao Chunshi
Ink sheet makees negative electrode, and negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is 15g/L
The aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 50A/dm2, etching time 120min；According to stainless
The purposes of steel part and requirement, micro-pore diameter, adjustment electrification can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid
Learn etching time control micropore depth.
Embodiment 6
The preparation method of stainless steel surfaces ordered micro-cellular structure mainly includes the following steps that：
（1）Stainless steel pre-processes：
1）Sample by 1mm thickness stainless steel plate wire cuttings into 30mm × 20mm；
2）Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；
3) electrochemical polish is carried out to the stainless steel after degreasing using WYK-15010K DC current regulator power supplies, obtains mirror
Face surface；Electrochemical polishing process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1,
Cathode anode spacing 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine
The aqueous solution of composition, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；Each step
Between, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 minutes, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：Using WYK-15010K DC current regulator power supplies to stainless after Passivation Treatment
Steel curved beam carries out electrochemical corrosion, obtains ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, Gao Chunshi
Ink sheet makees negative electrode, and negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is 30g/L
The aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 5A/dm2, etching time 120min；According to stainless
The purposes of steel part and requirement, micro-pore diameter, adjustment electrification can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid
Learn etching time control micropore depth.
Embodiment 7
The preparation method of stainless steel surfaces ordered micro-cellular structure mainly includes the following steps that：
（1）Stainless steel pre-processes：
1）Sample by 1mm thickness stainless steel plate wire cuttings into 30mm × 20mm；
2）Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；
3) electrochemical polish is carried out to the stainless steel after degreasing using WYK-15010K DC current regulator power supplies, obtains mirror
Face surface；Electrochemical polishing process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1,
Cathode anode spacing 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine
The aqueous solution of composition, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；Each step
Between, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 minutes, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：Using WYK-15010K DC current regulator power supplies to stainless after Passivation Treatment
Steel curved beam carries out electrochemical corrosion, obtains ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, Gao Chunshi
Ink sheet makees negative electrode, and negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is 30g/L
The aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 12.5A/dm2, etching time 120min；According to not
The purposes of rust steel part and requirement, micro-pore diameter, adjustment electricity can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid
Chemical attack time control micropore depth.
Embodiment 8
The preparation method of stainless steel surfaces ordered micro-cellular structure mainly includes the following steps that：
（1）Stainless steel pre-processes：
1）Sample by 1mm thickness stainless steel plate wire cuttings into 30mm × 20mm；
2）Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；
3) electrochemical polish is carried out to the stainless steel after degreasing using WYK-15010K DC current regulator power supplies, obtains mirror
Face surface；Electrochemical polishing process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, and negative electrode is with annode area than 3:1,
Cathode anode spacing 50mm, it by concentration is 300ml/L H that electrolytic polishing liquid, which is,2SO4, 600ml/L H3PO4, 30ml/L glycerine
The aqueous solution of composition, 85 DEG C of polishing fluid temperature, using constant flow method, current density 50A/dm2, polishing time 3min；Each step
Between, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step；
（2）Passivation for stainless steel processing：Polished stainless steel is put into 50% salpeter solution and is passivated processing, is obtained
Obtain fine and close oxide-film；Passivation technology：Passivation time is 20 minutes, and temperature is room temperature.Rinsed well after passivation with deionized water
Place into and electrochemical corrosion is carried out in the phosphoric acid solution prepared；
（3）Stainless steel electrochemical corrodes：Using WYK-15010K DC current regulator power supplies to stainless after Passivation Treatment
Steel curved beam carries out electrochemical corrosion, obtains ordered micro-cellular structure；Electrochemical corrosive process：Stainless steel curved beam makees anode, Gao Chunshi
Ink sheet makees negative electrode, and negative electrode is with annode area than 3:1, cathode anode spacing 50mm, electrochemical corrosive liquid are that phosphoric acid concentration is 50g/L
The aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 5A/dm2, etching time 120min；According to stainless
The purposes of steel part and requirement, micro-pore diameter, adjustment electrification can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid
Learn etching time control micropore depth.
The electrochemical corrosive process condition of the embodiment of the present invention is as shown in table 1, the microcellular structure ginseng prepared under different process
Number is as shown in table 2：
The electrochemical corrosive process parameter of table 1
The microcellular structure parameter of table 2
Above-described embodiment is used for explaining this explanation, rather than limits the invention, in the spirit and right of the present invention
It is required that protection domain in, to any modifications and changes for making of the present invention, both fall within protection scope of the present invention.
Claims (5)
- A kind of 1. preparation method of stainless steel surfaces ordered micro-cellular structure, it is characterised in that：Comprise the following steps：（1）Stainless steel pre-processes：1）Stainless steel degreasing processing：Stainless steel is put into 836 type cleaner for metals and is cleaned by ultrasonic 15min, carries out ungrease treatment；2）Stainless steel electrochemical polishes：Electrochemical polish is carried out to the stainless steel after degreasing using DC current regulator power supply, obtained Obtain specular surface, electrochemical polishing process：Using constant flow method, stainless steel makees anode, and high purity graphite piece makees negative electrode, electrolytic polishing liquid It is 300ml/L H for concentration2SO4, 600ml/L H3PO4, the aqueous solution of 30ml/L glycerine composition, 85 DEG C of polishing fluid temperature；（2）Passivation for stainless steel processing：The stainless steel that electrochemical polish is crossed, which is put into salpeter solution, is passivated processing, is caused Close oxide-film, passivation technology：Passivation time is 20 min, and temperature is room temperature；（3）Stainless steel electrochemical corrodes：Rinsed well after passivation with deionized water, electrification is carried out using DC current regulator power supply Corrosion is learned, obtains ordered micro-cellular structure, electrochemical corrosive process：Stainless steel curved beam makees anode, and high purity graphite piece makees negative electrode, electrification Learn corrosive liquid phosphate aqueous solution, 0-5 DEG C of solution temperature, using galvanostatic method, current density 5-50A/dm2, etching time 30- 120min；Step（1）With step（3）Described negative electrode and the area of anode are than 3:1；Step（1）With step（3）Described cathode anode spacing is 50mm；Step（1）The current density 50A/dm of described constant flow method2, polishing time 3min；Step（1）Described DC current regulator power supply voltage 0-150V, electric current 0-10A.
- A kind of 2. preparation method of stainless steel surfaces ordered micro-cellular structure according to claim 1, it is characterised in that：Step （2）Described passivation technology is：The volumetric concentration of salpeter solution is 50%, and passivation time 20min, temperature is room temperature.
- A kind of 3. preparation method of stainless steel surfaces ordered micro-cellular structure according to claim 1, it is characterised in that：Step （3）The mass concentration of described phosphate aqueous solution is 15-50g/L.
- A kind of 4. preparation method of stainless steel surfaces ordered micro-cellular structure according to claim 1, it is characterised in that：It is described Purposes and requirement of the microcellular structure according to stainless steel products, can be controlled by adjusting the phosphoric acid concentration size of electrochemical corrosive liquid Micro-pore diameter, adjust electrochemical corrosion time control micropore depth.
- A kind of 5. preparation method of stainless steel surfaces ordered micro-cellular structure according to claim 1, it is characterised in that：The party Between each step described in method, stainless steel curved beam is both needed to after being cleaned up with deionized water, then carries out next step.
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| CN105350065B (en) * | 2015-10-10 | 2018-01-26 | 东莞市卓越新材料科技有限公司 | The preparation method of stainless steel foil and its stainless steel foil of acquisition and steel plastic film |
| CN105926027A (en) * | 2016-05-23 | 2016-09-07 | 沈阳富创精密设备有限公司 | Corrosion resistance stainless steel electrolytic polishing technology |
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| CN108941805B (en) * | 2018-08-09 | 2020-02-21 | 广东工业大学 | Method for preparing surface microstructure by electrochemical polarization of stainless steel |
| CN112921389B (en) * | 2019-12-06 | 2022-02-08 | 中国科学院上海硅酸盐研究所 | Electrochemical polishing solution for copper foil surface pretreatment and application thereof |
| CN111803252B (en) * | 2020-08-27 | 2023-11-14 | 广东工业大学 | Stainless steel, preparation method thereof and drug eluting stent |
| CN112522773B (en) * | 2020-11-04 | 2022-01-28 | 东南大学 | Preparation method of stainless steel with antibacterial surface |
| CN112730171B (en) * | 2020-12-30 | 2022-12-09 | 成都市海瑞产品质量技术检测有限公司 | Grain size detection method for low-carbon high-alloy material |
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