CN105483715A - Template-3D etching preparation method of magnesium metal surface micro-nano composite hierarchical hole material - Google Patents
Template-3D etching preparation method of magnesium metal surface micro-nano composite hierarchical hole material Download PDFInfo
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- CN105483715A CN105483715A CN201510907086.0A CN201510907086A CN105483715A CN 105483715 A CN105483715 A CN 105483715A CN 201510907086 A CN201510907086 A CN 201510907086A CN 105483715 A CN105483715 A CN 105483715A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/22—Acidic compositions for etching magnesium or alloys thereof
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/30—Anodisation of magnesium or alloys based thereon
Abstract
The invention discloses a template-3D etching preparation method of a magnesium metal surface micro-nano composite hierarchical hole material, relates to a method for preparing micro-nano composite hierarchical holes in the magnesium metal surface, and solves the problems that a conventional femtosecond laser hole-forming method has certain requirement on the self size and shape of a sample, and is high in price and low in productivity. The method comprises the steps of polishing a magnesium metal material step by step, carrying out ultrasonic cleaning and deionized water cleaning, and drying; with the magnesium metal material adopted as an anode and a stainless steel plate adopted as a cathode, carrying out micro-arc oxidation treatment in an electrolyte, and establishing an overgrown micro-nano oxide micro-bulge template stretching into a magnesium matrix; removing a micro-arc oxidation coating under the ultrasonic assistance through a chromic acid solution, further etching the oxide micro-bulge template stretching into the magnesium matrix, copying a pit position of the bulge body, and forming micro-nano holes; and carrying out ultrasonic cleaning through deionized water, and drying to obtain the magnesium metal surface micro-nano composite hierarchical hole material.
Description
Technical field
The present invention relates to a kind of method being prepared by magnesium based metal to micro-nano combined multi-stage hole.
Background technology
Magnesium metal has aboundresources, and nontoxicity is easily degraded, many inherent advantages such as low price, and in aerospace, the field such as chemical industry, military project has a wide range of applications.To meet special military service function or increase its work-ing life be a kind of usual manner to reach to carry out surface modification to the magnesium alloy under a particular job environment.Magnesium based metal prepares micro-nano combined multi-stage hole, can be used for the micro-hole of medicine carrying of medical embedded magnesium metal device (support, screws, hone lamella), can be used for the lubricating oil reservoir in power lubrication field, can be used for the micro-structure surface of imitative lotus leaf super hydrophobic surface.
The normal laser processing that adopts is at metallic surface manufacturing array vesicular structure at present, and femtosecond laser pore-creating mode has certain requirement for the own size shape of sample etc., and price is high, and productivity is low, is not suitable for producing in enormous quantities.
Summary of the invention
Template-the 3D that the object of this invention is to provide a kind of magnesium based metal micro-nano combined multi-stage Porous materials etches preparation method, certain requirement is had for the own size shape of sample etc. to solve existing femtosecond laser pore-creating mode, and price is high, productivity is low, is not suitable for the problem produced in enormous quantities.
The present invention is undertaken by following steps: one, polished step by step respectively with 240#, 600# and 1200# abrasive paper for metallograph by magnesium metallic substance, then acetone and each ultrasonic cleaning 5 ~ 20min of dehydrated alcohol is at room temperature used successively, adopt washed with de-ionized water afterwards, dry, obtain pretreated magnesium metallic substance; Two, the magnesium metallic substance after processing step one is as anode, use stainless steel plate as negative electrode, temperature is 20 ~ 50 DEG C in the electrolytic solution, operating frequency is 400 ~ 1200Hz, dutycycle is under the condition of 4 ~ 20%, differential arc oxidation process 2 ~ 10min, thus adopt micro-arc discharge mode to build hypertrophy micro-nano oxide compound micro-" convex " the body template going deep into magnesium matrix at magnesium metal and differential arc oxidation coating interface; Three, use chromic acid solution under ultrasonic wave added, remove differential arc oxidation coating and etch oxide compound micro-" convex " the body template going deep into magnesium matrix further, the position, hole copying " convex " body forms micro-nano hole; Wherein, the concentration of chromic acid solution is 100 ~ 300g/L, and at room temperature the ultrasonic wave added treatment time is 30 ~ 60min; Four, use deionized water ultrasonic cleaning 5 ~ 20min, dry 10 ~ 20min at 60 ~ 80 DEG C and obtain magnesium based metal micro-nano combined multi-stage Porous materials.
Micro-nano hierarchical porous structure constructed by the present invention adopts liquid plasma micro-arc discharge means, and technique is simple, easy to operate, can realize batch production.Comprise electrical parameter and electrolyte type by the concrete implementing process controlling micro discharges, can realize regulating and controlling the size of micro-nano multi-stage porous, comprise for aperture, the regulation and control of hole depth, thus the multi-stage porous type of different demand can be obtained.To form micro-" convex " body and chromic acid in interface by secondary micro-arc discharge to etch and remove micro-" convex " body, can control aperture size further, and the hierarchical porous structure of more horn of plenty can be formed at magnesium based metal.The present invention, for the size no requirement (NR) of sample, can be implemented in the preparation that all kinds of shape face realizes hierarchical porous structure.Adopt chromic acid corrosion oxide skin, to magnesium matrix not damaged, easy to clean, chromic acid noresidue after corrosion.Magnesium based metal hierarchical porous structure applied range of the present invention, can be used for the micro-hole of medicine carrying of medical embedded magnesium metal device (support, screws, hone lamella), can be used for the lubricating oil reservoir in power lubrication field, can be used for the micro-structure surface of imitative lotus leaf super hydrophobic surface.
Accompanying drawing explanation
Fig. 1 be embodiment one prepare magnesium metal and micro-arc discharge oxide skin interface form oxide compound micro-" convex " body template cross-sectional scans photo.In figure, Reference numeral 1 indicates resin; 2 indication coatings; 3 instruction matrixes; 4 instruction interfacial oxide micro-" convex " structures.Fig. 2 be embodiment one prepare magnesium metal and micro-arc discharge oxide skin interface form oxide compound micro-" convex " body template schematic diagram.In figure, Reference numeral 5 indicates interface oxide compound micro-" convex " body; 6 instruction micro-arc discharge zone of oxidation; 7 instruction magnesium metal base bodies; 8 instruction one-level pore structures; 9 instruction second hole structures; Fig. 3 is the scanning electron photomicrograph of magnesium based metal one-level hole second hole prepared by embodiment one.10 instruction one-level holes in Fig. 3; 11 instruction second holes.
Embodiment
Embodiment one: illustrate present embodiment below in conjunction with Fig. 1 to Fig. 3.Present embodiment is undertaken by following steps: one, polished step by step respectively with 240#, 600# and 1200# abrasive paper for metallograph by magnesium metallic substance, then acetone and each ultrasonic cleaning 5 ~ 20min of dehydrated alcohol is at room temperature used successively, adopt washed with de-ionized water afterwards, dry, obtain pretreated magnesium metallic substance; Two, the magnesium metallic substance after processing step one is as anode, use stainless steel plate as negative electrode, temperature is 20 ~ 50 DEG C in the electrolytic solution, operating frequency is 400 ~ 1200Hz, dutycycle is under the condition of 4 ~ 20%, differential arc oxidation process 2 ~ 10min, thus adopt micro-arc discharge mode to build hypertrophy micro-nano oxide compound micro-" convex " the body template going deep into magnesium matrix at magnesium metal and differential arc oxidation coating interface; Three, use chromic acid solution under ultrasonic wave added, remove differential arc oxidation coating and etch oxide compound micro-" convex " the body template going deep into magnesium matrix further, the position, hole copying " convex " body forms micro-nano hole; Wherein, the concentration of chromic acid solution is 100 ~ 300g/L, and at room temperature the ultrasonic wave added treatment time is 30 ~ 60min; Four, use deionized water ultrasonic cleaning 5 ~ 20min, dry 10 ~ 20min at 60 ~ 80 DEG C and obtain magnesium based metal micro-nano combined multi-stage Porous materials; Five, reaming to magnesium based metal and further multipolarity process are completed for the magnesium based metal micro-nano combined multi-stage Porous materials repeating step two, three, four of completing steps two, step 3 and step 4, namely complete the preparation of magnesium based metal micro-nano combined multi-stage Porous materials.
Magnesium metal prepared by present embodiment and micro-arc discharge oxide skin interface form the cross-sectional scans photo of oxide compound micro-" convex " body as shown in Figure 1, and template schematic diagram as shown in Figure 2.
Magnesium based metal one-level hole prepared by present embodiment, the scanning electron photomicrograph of second hole as shown in Figure 3.Micro-nano hierarchical porous structure constructed by the present invention adopts micro-arc discharge to form micro-" convex " body template-3D lithographic method, and technique is simple, easy to operate, can realize batch production.Comprise electrical parameter and electrolyte type by the concrete implementing process controlling micro-arc discharge, can realize regulating and controlling the size of micro-nano multi-stage porous, comprise and aperture and depth size are controlled, thus the multi-stage porous type of different demand can be obtained; To form micro-" convex " body and chromic acid in interface by secondary micro-arc discharge to etch and remove micro-" convex " body, can control aperture size further, and the hierarchical porous structure of more horn of plenty can be formed at magnesium based metal.The present invention, for the size no requirement (NR) of sample, can be implemented in the preparation that all kinds of shape face realizes hierarchical porous structure.Adopt chromic acid corrosion oxide skin, to magnesium matrix not damaged, easy to clean, chromic acid noresidue after corrosion.Magnesium based metal hierarchical porous structure applied range of the present invention, can be used for the micro-hole of medicine carrying of medical embedded magnesium metal device (support, screws, hone lamella), can be used for the lubricating oil reservoir in power lubrication field, can be used for the micro-structure surface of imitative lotus leaf super hydrophobic surface.
Thinking of the present invention is the feature utilizing metallic surface discharge oxidation under liquid plasma, namely discharge at big area magnesium based metal homogeneous spark, and the corresponding oxide compound of electric discharge differential of the arc speckle displacement is to micro-" convex " body of metallic matrix hypertrophy, controls micro-arc discharge parameter and can obtain controlled micro-" convex " body of size at film base interface; And then with the template of micro-" convex " body of hypertrophy as multistage micro-nano hole, adopt again in ultrasonic wave added chromic acid solution and oxide coating and oxide compound micro-" convex " body going deep into magnesium matrix are etched away, the position, hole copying " convex " body forms micro-nano hole, thus forms the multistage poromerics of micro-nano in magnesium based metal high-level efficiency, big area.This processing method is simple, is applicable to suitability for industrialized production.
For the chromic acid solution used in process of the present invention, have certain toxicity, and can cause the problems such as environmental pollution, after being used to complete, can add sodium bisulfite in chromic acid solution to the pH of waste liquid is 7.5 ~ 8.5, makes chromic acid form Cr (OH)
3chemical waste liquid treatment process is adopted to reclaim after precipitation.Chromic acid is very easily water-soluble, and after ultrasonic cleaning, magnesium based metal is through EDS energy spectrum analysis, not containing chromium element, affects with using nothing for subsequent disposal.
Embodiment two: present embodiment and embodiment one unlike: described magnesium metal is magnalium, magnesium-zinc alloy, Mg-Zr alloys, magnesium-rare earth or magnesium calcium alloy.Other are identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: the electrolytic solution described by step 2 is silicate electrolyte or phosphoric acid salt electrolytic solution, and other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: the pH value of the chromic acid solution described in step 3 is 1.0 ~ 3.0.Other are identical with one of embodiment one to five.
Embodiment five: one of present embodiment and embodiment one to four unlike: the repeating step number of times described in step 5 can be secondary.Other are identical with one of embodiment one to four.
By following verification experimental verification beneficial effect of the present invention:
Test 1: this test is undertaken by following steps: one, by magnesium metallic substance with 240#, 600#, 1200# abrasive paper for metallograph is polished step by step to surface and is had metalluster, cut visual inspection is not obvious, then acetone and each ultrasonic cleaning 20min of dehydrated alcohol is at room temperature used successively, adopt washed with de-ionized water afterwards, 80 DEG C of loft drier are dried, and obtain pretreated magnesium metallic substance; Two, the magnesium metallic substance after processing step one is as anode, use stainless steel plate as negative electrode, (contained water glass 10g/L in phosphoric acid salt electrolytic solution, monocalcium phosphate 10g/L, sodium hydroxide 5g/L) temperature is 20 ~ 50 DEG C, operating frequency is 800Hz, dutycycle is 8%, under the condition of voltage 400V, micro-arc discharge 8min, obtains the magnesium metallic substance after micro-arc discharge oxidation; Three, at room temperature 60min is soaked in ultrasound environments to the magnesium metallic substance after the micro-arc discharge obtained in step 2 in the chromic acid solution of 150g/L; Four, use deionized water ultrasonic cleaning 20min, 80 DEG C of loft drier are dried, and complete the preparation of magnesium based metal micro-nano combined multi-stage Porous materials.
In this test, magnesium metallic substance is the wafer A Z31 magnesium alloy sample of Φ 30.This test obtain magnesium metal material surface one-level hole dimension at 5 ~ 8 μm, second hole size at 0.1 ~ 0.5 μm, the aperture degree of depth 3 ~ 9 μm.Scanning electron microscope pattern is shown in Fig. 3.
Test 2: this test is undertaken by following steps: one, by magnesium metallic substance with 240#, 600#, 1200# abrasive paper for metallograph is polished step by step to surface and is had metalluster, cut visual inspection is not obvious, then each ultrasonic cleaning 20min of acetone, dehydrated alcohol is at room temperature used successively, adopt washed with de-ionized water afterwards, 80 DEG C of loft drier are dried, and obtain pretreated magnesium metallic substance; Two, the magnesium metallic substance after processing step one is as anode, use stainless steel plate as negative electrode, (contained water glass 10g/L in phosphoric acid salt electrolytic solution, monocalcium phosphate 10g/L, sodium hydroxide 5g/L) temperature is 20 ~ 50 DEG C, operating frequency is 800Hz, dutycycle is 8%, under the condition of voltage 400V, micro-arc discharge 3min, obtains the magnesium metallic substance after micro-arc discharge; Three, under room temperature, 60min is soaked to the magnesium metallic substance after the micro-arc discharge obtained in step 2 in the chromic acid solution of 100g/L in ultrasound environments; Four, use deionized water ultrasonic cleaning 20min, 80 DEG C of loft drier are dried; Five, repeating step two, three, four, iterative process and step 2, three, four identical, complete the preparation of magnesium based metal micro-nano combined multi-stage Porous materials.
In this test, magnesium metallic substance is the wafer A Z31 magnesium alloy sample of Φ 30.The magnesium metal material surface one-level hole dimension that this test obtained before step 5 at 1 ~ 5 μm, second hole size at 0.05 ~ 0.5 μm, the aperture degree of depth 3 ~ 5 μm.The magnesium metal material surface obtained after step 5 contains 5 ~ 12 μm, 3 ~ 5 μm, 0.5 ~ 3 μm, and 0.05 ~ 0.5 μm is waited micro-nano hole.
Test 3: this test is undertaken by following steps: one, by magnesium metallic substance with 240#, 600#, 1200# abrasive paper for metallograph is polished step by step to surface and is had metalluster, cut visual inspection is not obvious, then each ultrasonic cleaning 20min of acetone, dehydrated alcohol is at room temperature used successively, adopt washed with de-ionized water afterwards, 80 DEG C of loft drier are dried, and obtain pretreated magnesium metallic substance; Two, the magnesium metallic substance after processing step one is as anode, use stainless steel plate as negative electrode, (contained water glass 10g/L in phosphoric acid salt electrolytic solution, monocalcium phosphate 10g/L, sodium hydroxide 5g/L) temperature is 20 ~ 50 DEG C, operating frequency is 800Hz, dutycycle is 8%, under the condition of voltage 500V, micro-arc discharge 20min, obtains the magnesium metallic substance after micro-arc discharge; Three, at room temperature 90min is soaked in ultrasound environments to the magnesium metallic substance after the micro-arc discharge obtained in step 2 in the chromic acid solution of 150g/L; Four, use deionized water ultrasonic cleaning 20min, 80 DEG C of loft drier are dried, and complete the preparation of magnesium based metal micro-nano combined multi-stage Porous materials.
In this test, magnesium metallic substance is the wafer A Z31 magnesium alloy sample of Φ 30.This test obtain magnesium metal material surface one-level hole dimension at 10 ~ 15 μm, second hole size at 0.1 ~ 2 μm, the aperture degree of depth 8 ~ 18 μm.
Claims (10)
1. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials etches preparation method, it is characterized in that described method is undertaken by following steps: one, polished step by step respectively with 240#, 600# and 1200# abrasive paper for metallograph by magnesium metallic substance, then acetone and each ultrasonic cleaning 5 ~ 20min of dehydrated alcohol is at room temperature used successively, adopt washed with de-ionized water afterwards, dry, obtain pretreated magnesium metallic substance; Two, the magnesium metallic substance after processing step one is as anode, use stainless steel plate as negative electrode, temperature is 20 ~ 50 DEG C in the electrolytic solution, operating frequency is 400 ~ 1200Hz, dutycycle is under the condition of 4 ~ 20%, differential arc oxidation process 2 ~ 10min, thus adopt micro-arc discharge mode to build hypertrophy micro-nano oxide compound micro-" convex " the body template going deep into magnesium matrix at magnesium metal and differential arc oxidation coating interface; Three, use chromic acid solution under ultrasonic wave added, remove differential arc oxidation coating and etch oxide compound micro-" convex " the body template going deep into magnesium matrix further, the position, hole copying " convex " body forms micro-nano hole; Wherein, the concentration of chromic acid solution is 100 ~ 300g/L, and at room temperature the ultrasonic wave added treatment time is 30 ~ 60min; Four, use deionized water ultrasonic cleaning 5 ~ 20min, dry 10 ~ 20min at 60 ~ 80 DEG C and obtain magnesium based metal micro-nano combined multi-stage Porous materials.
2. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 1 etches preparation method, it is characterized in that described method also comprises the steps: five, completes reaming to magnesium based metal and further multipolarity process for the magnesium based metal micro-nano combined multi-stage Porous materials repeating step two, three, four of completing steps two, step 3 and step 4, complete the preparation of magnesium based metal micro-nano combined multi-stage Porous materials.
3. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 1 and 2 etches preparation method, it is characterized in that described magnesium metal is magnalium, magnesium-zinc alloy, Mg-Zr alloys, magnesium-rare earth or magnesium calcium alloy.
4. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 1 and 2 etches preparation method, it is characterized in that the electrolytic solution described by step 2 is silicate electrolyte or phosphoric acid salt electrolytic solution.
5. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 1 and 2 etches preparation method, it is characterized in that the pH value of the chromic acid solution described in step 3 is 1.0 ~ 3.0.
6. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 2 etches preparation method, it is characterized in that the repeating step number of times described in step 5 is secondary.
7. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 1 etches preparation method, it is characterized in that, with acetone and each ultrasonic cleaning 20min of dehydrated alcohol in step one, after deionized water washings, 80 DEG C of loft drier are dried.
8. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 1 etches preparation method, and it is characterized in that in step 2 phosphoric acid salt electrolytic solution, containing water glass 10g/L, phosphoric acid calcium dihydrogen 10g/L, containing sodium hydroxide 5g/L.
9. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 1 etches preparation method, it is characterized in that the magnesium metallic substance after step 3 micro-arc discharge at room temperature soaks 60min in ultrasound environments in the chromic acid solution of 150g/L.
10. template-the 3D of magnesium based metal micro-nano combined multi-stage Porous materials according to claim 1 etches preparation method, it is characterized in that deionized water ultrasonic cleaning 20min in step 4, and 80 DEG C of loft drier are dried.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108930042A (en) * | 2018-07-13 | 2018-12-04 | 西安理工大学 | A kind of preparation method of Mg alloy surface super-hydrophobic film |
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