CN107119269B - In the method that magnesium based metal building has the winestone of corrosion protection effect acid coated - Google Patents

In the method that magnesium based metal building has the winestone of corrosion protection effect acid coated Download PDF

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CN107119269B
CN107119269B CN201710249052.6A CN201710249052A CN107119269B CN 107119269 B CN107119269 B CN 107119269B CN 201710249052 A CN201710249052 A CN 201710249052A CN 107119269 B CN107119269 B CN 107119269B
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magnesium
metal
winestone
protection effect
corrosion protection
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CN107119269A (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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    • 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)
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  • General Health & Medical Sciences (AREA)
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  • Heart & Thoracic Surgery (AREA)
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  • 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 the methods that kind has the winestone of corrosion protection effect acid coated in magnesium based metal building, the steps include: A, polishing, pickling solution ultrasonic cleaning；B, the magnesium immersion metal for walking A is placed under 50-70 DEG C of water bath in the NaOH solution that concentration is 3mol/L, places 11-14h, carries out alkali activating pretreatment, is then rinsed well rear, dry；C, the tartaric acid solution for preparing 5-25g/L adjusts pH to 5-9 with 1mol/L NaOH；D, the magnesium immersion metal for walking B is walked in C in configured tartaric acid solution, is placed under 30-80 DEG C of water bath, is placed 3-12h, is further taken out magnesium metal and rinsed well with deionized water, is dried in vacuo；It is acid coated that the winestone with corrosion protection effect is successfully constructed in magnesium based metal.It is modified to magnesium based metal using this method, more effectively magnesium metal can be made as biological medical degradable material in use, the treatment of its corrosion degradation and organism restores cycle match magnesium corrosion of metal rate by control corrosion rate environment.

Description

In the method that magnesium based metal building has the winestone of corrosion protection effect acid coated
Technical field
It is the present invention relates to mg-based material surface modifying method, in particular to a kind of in magnesium based metal building to there is corrosion to protect The acid coated surface modifying method of the winestone of shield effect.
Background technique
Magnesium is as one of the most abundant element of content in the earth's crust, since its density is small, intensity is high, wearability is strong, ductility With the mechanical properties such as toughness is higher, become very attractive metal material after at the end of the 20th century.Wherein, in bio-medical material In material field, magnesium metal is by its excellent mechanical property, elasticity modulus and people's bone is close, degradability and biocompatibility are good It is good, become most potential biodegradable implantation material, have especially in terms of bone implant material, angiocarpy bracket material compared with Big application prospect.
But since the chemical property of magnesium is active, magnesium and magnesium alloy during military service easily by environment institute corrosion failure, Too fast corrosion rate and serious local corrosion will cause implantation mechanical property of materials premature failure, bring great wind to operation Danger.Therefore the too fast corrosion rate of magnesium alloy limits the application of magnesium and magnesium alloy as biological medical degradable material, rotten The control problem of erosion rate is a problem to be solved.
Summary of the invention
Have the winestone of corrosion protection effect acid coated in magnesium based metal building the object of the present invention is to provide a kind of 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 restores the period Matching, and its good biocompatibility.
The present invention realizes its purpose the technical scheme adopted is that a kind of in magnesium based metal building there is corrosion protection to make The acid coated method of winestone, the steps include:
A, magnesium metal is put into pickling solution to be cleaned by ultrasonic one minute after silicon carbide paper is polished, magnesium metal is then taken out and is used in combination Deionized water is rinsed well；Mg (NO in pickling solution containing 150g/L3)2, 22g/L HNO3With 300g/L ethyl alcohol；
B, the magnesium immersion metal for walking A is placed in 50-70 DEG C of water-bath in the NaOH solution that concentration is 3mol/L Under environment, 11-14h is placed, carries out alkali activating pretreatment, then take out magnesium metal and is rinsed well with deionized water rear, dry；
C, the tartaric acid solution for preparing 5-25g/L adjusts pH to 5-9 with 1mol/L NaOH；
D, the magnesium immersion metal for walking B is walked in C in configured tartaric acid solution, is 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, is dried in vacuo；I.e. in magnesium based metal success Constructing has the winestone of corrosion protection effect acid coated.
Mechanism of the invention is:
B step carries out alkali activating pretreatment to magnesium metal, forms one layer of Mg (OH) on the surface of magnesium2Chemical conversion layer, make Magnesium surface is rich in more hydroxyls (- OH)；The hydroxyl (- OH) of magnesium surface in D step 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 material is formed 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 divalent or trivalent metal ion The divalent magnesium ion that acid molecule is escaped by capture from the magnesium based metal of destroyed escapes magnesium ion in magnesium metal base bottom surface Position form chelate products, to prevent the further occurrence of corrosion, and obstruct the entrance of extraneous corrosive ion.Thus institute The surface of formation will play the role of control corrosion rate rate, protection base material in corrosive environment.
Compared with prior art, the beneficial effects of the present invention are:
One, alkali activating pretreatment is first passed through, forms one layer of Mg (OH) 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, thus The surface that tartaric acid molecules are fixed on material is formed into one layer of tartaric acid film, meanwhile, using the effect of chelated metal ions, The divalent magnesium ion escaped from the magnesium based metal of destroyed is captured in film forming procedure rapidly, escapes magnesium in magnesium metal base bottom surface The position of ion forms chelate products so that coating is finer and close, obstruct on magnesium metal base bottom the further evolution of magnesium ion with The entrance of extraneous tartaric acid molecules corrosive ion slows down the generation of corrosion to effectively reduce the active site of material surface. By the regulation of tartaric acid molecules deposited concentration, i.e., the thickness and compactness of controllable tartaric acid coating, to efficiently control Corrosive environment makes magnesium and magnesium alloy as biological medical degradable material in use, it corrodes magnesium corrosion of metal rate Degradation and the treatment of organism restore cycle match.
Two, tartaric acid is a kind of carboxylic acid, is present in various plants, main organic in from a wealth of sources and grape wine One of acid.Simultaneously because it with optical activity and good biocompatibility, once be used to induce difference in biomaterial surface Biomolecule absorption, it is modified that surface carried out to magnesium metal using tartaric acid, its corrosion resistance can not only be improved, also promoted The raising of its biocompatibility.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph in embodiment 1 after being polished magnesium sheet and being cleaned by ultrasonic completely.
Fig. 2 is the scanning electron microscope (SEM) photograph of the obtained object of embodiment 1.
Fig. 3 is the obtained object (Mg-TA) of embodiment 1 and the nyquist diagram of magnesium (Mg).
Fig. 4 is the enlarged diagram of Blocked portion in Fig. 3.
TA in Fig. 1-4 indicates tartaric acid.
Specific embodiment
Embodiment 1
A method of have the winestone of corrosion protection effect acid coated in pure magnesium surface building, the steps include:
A, pure magnesium is put into the Mg (NO containing 150g/L after silicon carbide paper is polished3)2, 22g/L HNO3With 300g/L second In the pickling solution 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 walking A is immersed in 3mol/L NaOH solution, is placed under 60 DEG C of water bath, is placed 12h carries out alkali activating pretreatment, then takes out pure magnesium and and drying clean with deionized water repeated flushing；
C, the tartaric acid solution for preparing 5g/L adjusts pH value of solution to 5 with 1mol/L NaOH；
D, the pure magnesium for walking B is immersed in C and walks in configured tartaric acid solution, is placed in 60 DEG C of water bath Under, 12h is placed, pure magnesium and, vacuum drying clean with deionized water repeated flushing are then taken out；Successfully constructed in pure magnesium surface Winestone with corrosion protection effect is acid coated.
Fig. 1 is the scanning electron microscope (SEM) photograph in embodiment 1 after being polished pure magnesium and being cleaned by ultrasonic completely, and Fig. 2 is to implement The scanning electron microscope (SEM) photograph for the obtained object 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 Bottom surface forms the chelate products layer of a large amount of tartaric acid and magnesium ion, has effectively obstructed pure magnesium-based bottom and extraneous corrosivity ring The contact in border.
Fig. 3 is the obtained object (Mg-TA) of embodiment 1 and the nyquist diagram of magnesium (Mg).Fig. 4 is Blocked portion in Fig. 3 Enlarged diagram.For this example by the modified obtained sample in surface, impedance value is upper compared with pure magnesium it can be seen from Fig. 3,4 Two orders of magnitude are risen, corrosion rate is effectively controlled, and corrosion resistance significantly improves.
Embodiment 2
A method of have the winestone of corrosion protection effect acid coated in Mg alloy surface building, the steps include:
A, magnesium alloy is put into the Mg (NO containing 150g/L after silicon carbide paper is polished3)2, 22g/L HNO3And 300g/L In the pickling solution of ethyl alcohol, it is cleaned by ultrasonic one minute, then take out magnesium alloy and is rinsed well with deionized water；
B, the magnesium alloy for walking A is immersed in 3mol/L NaOH solution, is placed under 50 DEG C of water bath, is put 11h is set, alkali activating pretreatment is carried out, then takes out magnesium alloy and and drying clean with deionized water repeated flushing；
C, the tartaric acid solution for preparing 15g/L adjusts pH value of solution to 7 with 1mol/L NaOH；
D, the magnesium alloy for walking B is immersed in C and walks in configured tartaric acid solution, is placed in 30 DEG C of water bath Under, 6h is placed, magnesium alloy and, vacuum drying clean with deionized water repeated flushing are then taken out；I.e. in Mg alloy surface success Constructing has the winestone of corrosion protection effect acid coated.
Embodiment 3
A kind of method that pure magnesium surface constructs nanometer dressing structure and coats functional molecular, the steps include:
A, pure magnesium is put into the Mg (NO containing 150g/L after silicon carbide paper is polished3)2, 22g/L HNO3With 300g/L second In the pickling solution 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 walking A is immersed in 3mol/L NaOH solution, is placed under 70 DEG C of water bath, is placed 14h carries out alkali activating pretreatment, then takes out pure magnesium and and drying clean with deionized water repeated flushing；
C, the tartaric acid solution for preparing 25g/L adjusts pH value of solution to 9 with 1mol/L NaOH；
D, the pure magnesium for walking B is immersed in C and walks in configured tartaric acid solution, is placed in 80 DEG C of water bath Under, 3h is placed, pure magnesium and, vacuum drying clean with deionized water repeated flushing are then taken out；Successfully constructed in pure magnesium surface Winestone with corrosion protection effect is acid coated.

Claims (2)

1. a kind of method for having the winestone of corrosion protection effect acid coated in magnesium based metal building, the steps include:
A, magnesium metal is put into after silicon carbide paper is polished pickling solution be cleaned by ultrasonic one minute, then take out magnesium metal and spend from Sub- water is rinsed well；Mg (NO in pickling solution containing 150g/L3)2, 22g/L HNO3With 300g/L ethyl alcohol；
B, the magnesium immersion metal for walking A is 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, magnesium metal is then taken out and is rinsed well with deionized water rear, dry；
C, the tartaric acid solution for preparing 5-25g/L adjusts pH to 5-9 with 1mol/L NaOH；
D, the magnesium immersion metal for walking B is walked in C in configured tartaric acid solution, is 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 constructed in magnesium based metal Winestone with corrosion protection effect is acid coated.
2. according to claim 1 a kind of in the side that magnesium based metal building has the winestone of corrosion protection effect acid coated Method, which is characterized in that the 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 examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877697B (en) * 2020-12-21 2023-03-21 重庆大学 Surface porous magnesium alloy and preparation method thereof
CN113171755B (en) * 2021-04-28 2022-10-14 安徽工业大学 Nickel-chelated magnetic nano-particle, preparation method and application for separating and purifying histidine-tagged protein

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

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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