CN107119269A - The acid coated method of the winestone with corrosion protection effect is built in magnesium based metal - Google Patents

The acid coated method of the winestone with corrosion protection effect is built in magnesium based metal Download PDF

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CN107119269A
CN107119269A CN201710249052.6A CN201710249052A CN107119269A CN 107119269 A CN107119269 A CN 107119269A CN 201710249052 A CN201710249052 A CN 201710249052A CN 107119269 A CN107119269 A CN 107119269A
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magnesium
metal
winestone
corrosion protection
corrosion
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CN107119269B (en
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万国江
李薇
陈英奇
张文泰
黄楠
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Southwest Jiaotong University
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Southwest Jiaotong University
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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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/02—Inorganic materials
    • A61L31/022—Metals or alloys
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08—Materials for coatings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Vascular Medicine (AREA)
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  • Animal Behavior & Ethology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Epidemiology (AREA)
  • Heart & Thoracic Surgery (AREA)
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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention discloses planting in the acid coated method of winestone of the magnesium based metal structure with corrosion protection effect, its step is：A, polishing, pickle are cleaned by ultrasonic；B, the magnesium immersion metal for obtaining A steps, in 3mol/L NaOH solution, under the water bath for being placed in 50 70 DEG C, to place 11 14h, carrying out alkali activating pretreatment, are then rinsed well rear, dry in concentration；C, the tartaric acid solution for preparing 5 25g/L, pH to 59 is adjusted with 1mol/L NaOH；D, the magnesium immersion metal for obtaining B steps are walked in C in configured tartaric acid solution, under the water bath for being placed in 30 80 DEG C, are placed 3 12h, are further taken out magnesium metal and rinsed well with deionized water, are dried in vacuo；It is acid coated the winestone with corrosion protection effect successfully to be built in magnesium based metal.It is modified to magnesium based metal using this method, more effectively to magnesium corrosion of metal speed, magnesium metal can be made as biological medical degradable material in use, the treatment of its corrosion degradation and organism recovers cycle match by control corrosion rate environment.

Description

The acid coated method of the winestone with corrosion protection effect is built in magnesium based metal
Technical field
The present invention relates to mg-based material surface modifying method, there is a kind of more particularly to built in magnesium based metal corrosion to protect The acid coated surface modifying method of winestone of shield effect.
Background technology
Magnesium is as one of most abundant element of content in the earth's crust, because its density is small, intensity is high, wearability is strong, ductility With the mechanical property such as toughness is higher, turn into the metal material of very attractive after 20 end of the centurys.Wherein, in bio-medical material In material field, magnesium metal relies near its excellent mechanical property, modulus of elasticity and people's bone photo, degradability and biocompatibility is good It is good, be implanted into material as most potential biodegradable, have especially in terms of bone implant material, angiocarpy bracket material compared with Big application prospect.
But be due to magnesium chemical property it is active, magnesium and magnesium alloy under arms during easily by environment institute corrosion failure, Too fast corrosion rate and serious local corrosion can be caused to be implanted into mechanical property of materials premature failure, and great wind is brought to operation Danger.Therefore the too fast corrosion rate of magnesium alloy limits magnesium and magnesium alloy as the application of biological medical degradable material, and it is rotten The control problem for losing speed is urgent problem to be solved.
The content of the invention
Have the winestone of corrosion protection effect acid coated it is an object of the invention to provide a kind of built in magnesium based metal Method, it is modified to magnesium based metal using this method, can more effectively control corrosion rate environment to magnesium corrosion of metal speed Rate, makes magnesium and magnesium alloy as biological medical degradable material in use, the treatment of its corrosion degradation and organism recovers the cycle Matching, and its good biocompatibility.
The present invention realizes its purpose the technical scheme adopted is that there is a kind of built in magnesium based metal corrosion protection to make The acid coated method of winestone, its step is：
A, magnesium metal is polished through silicon carbide paper after be put into pickle be cleaned by ultrasonic one minute, then take out magnesium metal be used in combination Deionized water rinsing is clean；Mg (NO containing 150g/L in pickle3)2, 22g/L HNO3With 300g/L ethanol；
B, the magnesium immersion metal for obtaining A steps are placed in 50-70 DEG C of water-bath in the NaOH solution that concentration is 3mol/L Under environment, 11-14h is placed, alkali activating pretreatment is carried out, after then taking out magnesium metal and being rinsed well with deionized water, dried；
C, the tartaric acid solution for preparing 5-25g/L, pH to 5-9 is adjusted with 1mol/L NaOH；
D, the magnesium immersion metal for obtaining B steps are walked in C in configured tartaric acid solution, are placed in 30-80 DEG C of water-bath Under environment, 3-12h is placed, magnesium metal is further taken out and is rinsed well with deionized water, be dried in vacuo；I.e. in magnesium based metal success Build the winestone with corrosion protection effect acid coated.
The present invention mechanism be：
B steps carry out alkali activating pretreatment to magnesium metal, and one layer of Mg (OH) is formed on the surface of magnesium2Chemical conversion layer, make Magnesium surface is rich in more hydroxyls (- OH)；The hydroxyl (- OH) of magnesium surface in D steps with the carboxylic groups of tartaric acid molecules (- COOH chemical graft) is carried out, so that the surface that tartaric acid molecules are fixed on into material forms one layer of tartaric acid film.In addition, wine Stone acid has chelation, winestone as a kind of carboxylic acid type metal ion chelation agent to most of divalence or trivalent metal ion The divalence magnesium ion that acid molecule is escaped by the magnesium based metal captured from destroyed, magnesium ion is escaped in magnesium metal base basal surface Position form chelate products, so as to prevent the further generation of corrosion, and the entrance of the extraneous corrosive ion of barrier.Thus institute The surface of formation will play a part of control corrosion rate speed, protection base material in corrosive atmosphere.
Compared with prior art, the beneficial effects of the invention are as follows：
First, alkali activating pretreatment is first passed through, one layer of Mg (OH) is formed on the surface of magnesium2Chemical conversion layer, make magnesium surface Rich in more hydroxyls (- OH), hydroxyl (- OH) carries out chemical graft with the carboxylic group (- COOH) of tartaric acid molecules again, so that The surface that tartaric acid molecules are fixed on into material forms one layer of tartaric acid film, meanwhile, using the effect of chelated metal ions, The divalence magnesium ion that rapid capture is escaped from the magnesium based metal of destroyed in film forming procedure, magnesium is escaped in magnesium metal base basal surface The position of ion forms chelate products so that coating is finer and close, on barrier magnesium metal base bottom the further effusion of magnesium ion and The entrance of extraneous tartaric acid molecules corrosive ion, so as to effectively reduce the avtive spot of material surface, slows down the generation of corrosion. Pass through the regulation and control of tartaric acid molecules deposited concentration, you can the acid coated thickness of control winestone and compactness, so as to efficiently control Corrosive atmosphere makes magnesium and magnesium alloy as biological medical degradable material in use, it corrodes to magnesium corrosion of metal speed Degraded and the treatment of organism recover cycle match.
2nd, tartaric acid is a kind of carboxylic acid, is present in various plants, wide material sources, is also main organic in grape wine One of acid.Simultaneously because it has optical activity and good biocompatibility, it once be used to induce different in biomaterial surface Biomolecule absorption, using tartaric acid to magnesium metal carry out surface modification, its corrosion resistance can not only be improved, also promoted The raising of its biocompatibility.
Brief description of the drawings
Fig. 1 be in embodiment 1 magnesium sheet is polished and be cleaned by ultrasonic it is clean after scanning electron microscope (SEM) photograph.
Fig. 2 is the scanning electron microscope (SEM) photograph of the obtained thing of embodiment 1.
Fig. 3 is nyquist diagram of the obtained thing (Mg-TA) with magnesium (Mg) of embodiment 1.
Fig. 4 is the enlarged diagram of Blocked portion in Fig. 3.
TA in Fig. 1-4 represents tartaric acid.
Embodiment
Embodiment 1
A kind of to build the acid coated method of the winestone with corrosion protection effect in pure magnesium surface, its step is：
A, pure magnesium is polished through silicon carbide paper after be put into the Mg (NO containing 150g/L3)2, 22g/L HNO3With 300g/L second In the pickle of alcohol, it is cleaned by ultrasonic one minute, then takes out pure magnesium and rinsed well with deionized water；
B, the pure magnesium for obtaining A steps are immersed in 3mol/L NaOH solutions, under the water bath for being placed in 60 DEG C, are placed 12h, carries out alkali activating pretreatment, then takes out pure magnesium and is rinsed well and dried repeatedly with deionized water；
C, the tartaric acid solution for preparing 5g/L, pH value of solution is adjusted to 5 with 1mol/L NaOH；
D, the pure magnesium for obtaining B steps are immersed in C and walked in configured tartaric acid solution, are placed in 60 DEG C of water bath Under, 12h is placed, pure magnesium is then taken out and is rinsed well repeatedly with deionized water, is dried in vacuo；Successfully built in pure magnesium surface The winestone acted on corrosion protection is acid coated.
Fig. 1 be in embodiment 1 pure magnesium is polished and be cleaned by ultrasonic it is clean after scanning electron microscope (SEM) photograph, Fig. 2 is to implement The scanning electron microscope (SEM) photograph for the obtained thing that D is walked in example 1.It is modified by the example method surface it can be seen from Fig. 1,2, in pure magnesium-based Basal surface forms the chelate products layer of substantial amounts of tartaric acid and magnesium ion, has effectively obstructed pure magnesium-based bottom and extraneous corrosivity ring The contact in border.
Fig. 3 is nyquist diagram of the obtained thing (Mg-TA) with magnesium (Mg) of embodiment 1.Fig. 4 is Blocked portion in Fig. 3 Enlarged diagram.This example is by the modified obtained sample in surface it can be seen from Fig. 3,4, and its impedance value is upper compared with pure magnesium Two orders of magnitude are risen, corrosion rate is effectively controlled, and decay resistance is significantly improved.
Embodiment 2
A kind of to build the acid coated method of the winestone with corrosion protection effect in Mg alloy surface, its step is：
A, magnesium alloy is polished through silicon carbide paper after be put into the Mg (NO containing 150g/L3)2, 22g/L HNO3And 300g/L In the pickle of ethanol, it is cleaned by ultrasonic one minute, then takes out magnesium alloy and rinsed well with deionized water；
B, the magnesium alloy for obtaining A steps are immersed in 3mol/L NaOH solutions, under the water bath for being placed in 50 DEG C, are put 11h is put, alkali activating pretreatment is carried out, magnesium alloy is then taken out and is rinsed well and dried repeatedly with deionized water；
C, the tartaric acid solution for preparing 15g/L, pH value of solution is adjusted to 7 with 1mol/L NaOH；
D, the magnesium alloy for obtaining B steps are immersed in C and walked in configured tartaric acid solution, are placed in 30 DEG C of water bath Under, 6h is placed, magnesium alloy is then taken out and is rinsed well repeatedly with deionized water, is dried in vacuo；I.e. in Mg alloy surface success Build the winestone with corrosion protection effect acid coated.
Embodiment 3
A kind of pure magnesium surface builds nanometer dressing structure and the method for coating functional molecular, and its step is：
A, pure magnesium is polished through silicon carbide paper after be put into the Mg (NO containing 150g/L3)2, 22g/L HNO3With 300g/L second In the pickle of alcohol, it is cleaned by ultrasonic one minute, then takes out pure magnesium and rinsed well with deionized water；
B, the pure magnesium for obtaining A steps are immersed in 3mol/L NaOH solutions, under the water bath for being placed in 70 DEG C, are placed 14h, carries out alkali activating pretreatment, then takes out pure magnesium and is rinsed well and dried repeatedly with deionized water；
C, the tartaric acid solution for preparing 25g/L, pH value of solution is adjusted to 9 with 1mol/L NaOH；
D, the pure magnesium for obtaining B steps are immersed in C and walked in configured tartaric acid solution, are placed in 80 DEG C of water bath Under, 3h is placed, pure magnesium is then taken out and is rinsed well repeatedly with deionized water, is dried in vacuo；Successfully built in pure magnesium surface The winestone acted on corrosion protection is acid coated.

Claims (2)

1. a kind of build the acid coated method of the winestone with corrosion protection effect in magnesium based metal, its step is：
A, magnesium metal is polished through silicon carbide paper after be put into pickle be cleaned by ultrasonic one minute, then take out magnesium metal and spend from Sub- water is rinsed well；Mg (NO containing 150g/L in pickle3)2, 22g/L HNO3With 300g/L ethanol；
B, the magnesium immersion metal for obtaining A steps are placed in 50-70 DEG C of water bath in the NaOH solution that concentration is 3mol/L Under, 11-14h is placed, alkali activating pretreatment is carried out, after then taking out magnesium metal and being rinsed well with deionized water, dried；
C, the tartaric acid solution for preparing 5-25g/L, pH to 5-9 is adjusted with 1mol/L NaOH；
D, the magnesium immersion metal for obtaining B steps are walked in C in configured tartaric acid solution, are placed in 30-80 DEG C of water bath Under, 3-12h is placed, magnesium metal is further taken out and is rinsed well with deionized water, is dried in vacuo；Successfully built in magnesium based metal The winestone acted on corrosion protection is acid coated.
2. a kind of side acid coated in winestone of the magnesium based metal structure with corrosion protection effect according to claim 1 Method, it is characterised in that described magnesium metal is pure magnesium or magnesium alloy.
CN201710249052.6A 2017-04-17 2017-04-17 In the method that magnesium based metal building has the winestone of corrosion protection effect acid coated Active CN107119269B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877697A (en) * 2020-12-21 2021-06-01 重庆大学 Surface porous magnesium alloy and preparation method thereof
CN113171755A (en) * 2021-04-28 2021-07-27 安徽工业大学 Nickel-chelated magnetic nano-particle, preparation method and application for separating and purifying histidine-tagged protein

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Publication number Priority date Publication date Assignee Title
JP2011074490A (en) * 2009-09-07 2011-04-14 Ofutekku Kk Surface treatment method of magnesium and magnesium alloy for imparting brightness/decorating property, high corrosion resistance and functionality
CN103614718A (en) * 2013-10-30 2014-03-05 西南交通大学 Method for obtaining bio-functionalized coating with low corrosion speed on pure magnesium surface
CN105331977A (en) * 2015-09-28 2016-02-17 西南交通大学 Method for constructing nanometer containing structure on surface of magnesium metal and coating functional molecules
CN106011815A (en) * 2016-06-07 2016-10-12 西南交通大学 Preparation method for hybrid composite coating used for magnesium-based biological material surface medication

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011074490A (en) * 2009-09-07 2011-04-14 Ofutekku Kk Surface treatment method of magnesium and magnesium alloy for imparting brightness/decorating property, high corrosion resistance and functionality
CN103614718A (en) * 2013-10-30 2014-03-05 西南交通大学 Method for obtaining bio-functionalized coating with low corrosion speed on pure magnesium surface
CN105331977A (en) * 2015-09-28 2016-02-17 西南交通大学 Method for constructing nanometer containing structure on surface of magnesium metal and coating functional molecules
CN106011815A (en) * 2016-06-07 2016-10-12 西南交通大学 Preparation method for hybrid composite coating used for magnesium-based biological material surface medication

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877697A (en) * 2020-12-21 2021-06-01 重庆大学 Surface porous magnesium alloy and preparation method thereof
CN113171755A (en) * 2021-04-28 2021-07-27 安徽工业大学 Nickel-chelated magnetic nano-particle, preparation method and application for separating and purifying histidine-tagged protein

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