CN107675163A - The method that the pure zinc of Mg alloy surface/Zinc alloy coated is prepared based on cold spray technique - Google Patents
The method that the pure zinc of Mg alloy surface/Zinc alloy coated is prepared based on cold spray technique Download PDFInfo
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- CN107675163A CN107675163A CN201711124802.3A CN201711124802A CN107675163A CN 107675163 A CN107675163 A CN 107675163A CN 201711124802 A CN201711124802 A CN 201711124802A CN 107675163 A CN107675163 A CN 107675163A
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
- C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/087—Coating with metal alloys or metal elements only
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Abstract
The present invention relates to metal material processing technical field, there is provided a kind of method that the pure zinc of Mg alloy surface/Zinc alloy coated is prepared based on cold spray technique, grinding process, Chemical cleaning is carried out to magnesium/magnesium alloy substrate；Appropriate technological parameter is set, pure zinc/Zinc alloy powder is sprayed to the depositional plane of the substrate, obtains pure zinc/Zinc alloy coated.The present invention is based on efficiently quick cold spraying coat preparing technology, successfully pure zinc/Zinc alloy coated is prepared in Mg alloy surface, resulting materials have good mechanical property and decay resistance, and bioactivity is well and cellular affinity is excellent, by modulation process parameter the i.e. achievable material of pure zinc/Zinc alloy coated of magnesium alloy surface spraying different-thickness controlled degradation；The technology can also be applied to the surfacecti proteon of industrial magnesium alloys;Method simple practical, have a extensive future.
Description
Technical field
The present invention relates to metal material processing technical field, more particularly to one kind prepares magnesium alloy table based on cold spray technique
The method of the pure zinc in face/Zinc alloy coated.
Background technology
In the last few years, magnesium alloy achieved on the application development of industrial circle and bio-medical material huge enters
Step.Industrially because magnesium alloy density is low, specific strength is high, and thermal conductivity ability is excellent while has dimensionally stable, processing characteristics
The features such as good, is all widely used in fields such as Aero-Space, automobile, electronics, defence and militaries；It is sharp in technical field of biological material
The characteristic easily corroded in human body with metal materials such as magnesium alloys, realizes that metal implant is gradually degraded to finally in vivo
The clinical medicine target of disappearance.Magnesium alloy realizes biodegradation, and Mg because corrosion potential is low in human body2+It is that human body contains
The cation of flow control two, the source of a variety of enzymes participate in metabolism, can safely absorbed, and magnesium alloy mechanical property is closer to bone group
Knit, while cost is relatively low, suitable for the research and extension of bio-medical material.
Magnesium and magnesium alloy are with the obvious advantage, have a high potential, but corrosion resistance difference hinders its further development and application.Magnesium
It is the very active metal of chemical property, electronegativity is very strong, and corrosion resisting property is poor, has great limitation in commercial Application,
It also can not meet length of service needed for implant because degradation speed is too fast in human body simultaneously, and exist along with magnesium alloy
Internal fast degradation, a large amount of hydrogen aggregations, not only bad for the healing of bone tissue, can also trigger the production of inflammation and rimhole
It is raw.
The method of enhancing corrosion resistance of magnesium alloy mainly has two classes：First, improving the corrosion resistance of magnesium alloy itself, lead to
Crossing improves the microstructure of magnesium alloy, studies new alloy to realize；Second, by be surface-treated and it is modified make magnesium alloy substrate with
External environment completely cuts off, and slows down its corrosion rate.And it is surface-treated simultaneously also easily real as etch-proof important method efficiency high
It is existing.In the method for various Magnesiumalloy surface modifyings, including industrially application is relatively wide but is not suitable for giving birth to for chemical plating and plating
Thing medical field；Chemically transformed film technique complex pretreatment in bio-medical research, it is desirable to higher；Anodic oxidation and differential arc oxidation
Technology is difficult to the matrix for tackling complex topography and the subsequent treatment for needing sealing of hole；The cost of gas phase deposition technology prepares coating compared with
Height, processing time length, efficiency are low；Other surfaces treatment technology such as laser treatment easily makes matrix that oxidation and damage, thermal jet occur
Painting technology coating compactness is not high and high temperature to matrix, there is also fire damage, ion implantation technique complexity effective depth are limited.And
Cold spraying has original advantage as new coating production, its low-temperature spray, it is anti-oxidation, formed coating quality it is high,
The advantages of controllability is strong is highly suitable as a kind of new technology of Magnesiumalloy surface modifying, and the characteristic of especially low temperature depositing more makes
Obtain cold spray technique has extensive prospect in the preparation of biological coating.
In the selection of sprayed on material, it should be based on suitably slowing down magnesium alloy degradation rate, meet certain commercial Application, simultaneously
Bio-medical direction is extended to, the characteristics of this requires sprayed on material also to need biodegradation, possesses biocompatibility and nontoxic
The advantages such as side effect.In addition to bio-inert material, biomedical material research also focuses on the fields such as ferroalloy and kirsite, and two
The corrosion resistance of person is higher compared to magnesium alloy, but temperature needed for spraying ferrous alloy is higher, magnesium matrix can be caused on the contrary necessarily
The deterioration of degree.And spray pure zinc/kirsite and be then easily achieved, Zn elements are also one of micro elements needed by human, are participated in more
Kind of enzyme reaction, and maintain the stability of many macromolecular structures and function, human skeleton is grown, cardiovascular health it is equal
Play irreplaceable effect.Pure Zn is used as the trial of vascular stent material, it was demonstrated that its biomaterial application value,
So it can safely be implanted into human body as the surface modifying material of magnesium alloy.
The content of the invention
The purpose of the present invention is exactly overcome the deficiencies in the prior art, there is provided one kind prepares magnesium alloy based on cold spray technique
The method of the pure zinc in surface/Zinc alloy coated, had both ensured that coating and substrate binding ability were excellent, was improving corrosion resistance of magnesium alloy
Meanwhile can be by adjusting the features such as original material realizes composite biocompatibility and no biotoxicity, and can pass through
Regulation spraying parameter realizes the degrading and regulating of coating；The technology can also be applied to the surfacecti proteon of industrial magnesium alloys.
A kind of method that the pure zinc of Mg alloy surface/Zinc alloy coated is prepared based on cold spray technique of the present invention, is closed to magnesium/magnesium
Gold base carries out grinding process, Chemical cleaning；Pure zinc/Zinc alloy powder is sprayed to the depositional plane of the substrate, obtain pure zinc/
It is Zinc alloy coated.
Further, specifically comprise the following steps：
Step 1: processing substrate：Magnesium/magnesium alloy substrate is worked into required size, and grinding process is carried out to depositional plane, is removed
The oxide layer of the depositional plane, and carry out Chemical cleaning；
Step 2: powder prepares：Pure zinc/Zinc alloy powder is loaded into cold spray apparatus powder feeder；
Step 3: substrate is fixed：By substrate installation on the table, it is placed under Spray gun for cold spray；Optional spray gun is not
It is dynamic, movable workbench；Or workbench is motionless, one of spray gun movement two ways completes spraying；
Step 4: spraying substrate：Corresponding technological parameter is set, sprayed, obtains pure zinc/Zinc alloy coated.
Further, the magnesium/magnesium alloy substrate includes pure magnesium series, AS (Mg-Al-Si) series, AE (Mg-Al-RE)
Series, AM (Mg-Al-Mn) series.
Further, the magnesium/magnesium alloy substrate is binary Magnesium Alloys, ternary magnesium alloy system or complex magnesium alloy system；
The binary Magnesium Alloys include Mg-Ca, Mg-Zn, Mg-Sr, Mg-Si, Mg-Li, Mg-Mn, Mg-RE；
The ternary magnesium alloy system includes Mg-Y-Zn, Mg-Gd-Y-Zn, Mg-Gd-Y-Zr alloy system, Mg-Zn-Ca；
The complex magnesium alloy system includes Mg-Zn-Ca-X；Wherein X is Mn, Sn, Sr or RE.
Further, the pure zinc/kirsite is pure zinc, binary kirsite system, ternary kirsite system or polynary kirsite
System；
The binary kirsite system includes Zn-Mg, Zn-Ca, Zn-Mn, Zn-Sr；
The ternary kirsite system includes Zn-Mg-Ca, Zn-Ca-Sr, Zn-Mg-Sr, Zn-Mg-Y；
The polynary kirsite system includes Zn-Mg-Ca-X, and wherein X is Mn, Sn, Sr, RE.
Further, the thickness of the magnesium/magnesium alloy substrate, pure zinc/Zinc alloy coated, according to the corrosion speed of material in itself
Rate and the actually required degradation rate of medical device determine.
Further, in step 1, described polishing is manual grinding, and roughness is the thick of gained after 400# sand paper is polished
Rugosity；The substrate after polishing is cleaned using absolute ethyl alcohol, and dried up with cold wind.
Further, in step 2, the pure zinc/Zinc alloy powder granularity is 5 μm -100 μm.
Further, in step 4, spraying temperature is 50-550 DEG C, gas pressure 0.5-4MPa, spray gun translational speed
For 100-500mm/min, spray distance 10-30mm, working gas is nitrogen.
Further, when methods described is used for bio-medical material, the magnesium/magnesium alloy substrate is serial using pure magnesium,
Mg-Ca, or Mg-Zn-Ca；Pure zinc/the kirsite is using pure zinc series, Zn-Mg, or Zn-Mg-Ca.
Beneficial effects of the present invention are：Based on efficient quickly cold spraying coat preparing technology, successfully in magnesium alloy table
Face is prepared for pure zinc/Zinc alloy coated, and resulting materials have good mechanical property and decay resistance, and bioactivity is good
Good and cellular affinity is excellent, by modulation process parameter magnesium alloy surface spraying different-thickness pure zinc/Zinc alloy coated
The controlled degradation of material can be achieved；Method simple practical, have a extensive future.
Brief description of the drawings
Fig. 1 show the microstructure morphology of the spelter coating combination interface prepared in embodiment 1 on AZ31 magnesium substrates（Electronic Speculum
Photo）.
Fig. 2 show the spelter coating prepared in embodiment 1 on AZ31 magnesium substrates with magnesium alloy substrate, pure zine plate in analogue body
In liquid（SBF）Corrosion polarization curve.
Fig. 3 show the microstructure morphology of the spelter coating combination interface prepared in embodiment 2 on AZ91 magnesium substrates（Electronic Speculum
Photo）.
Fig. 4 show the spelter coating prepared in embodiment 2 on AZ91 magnesium substrates with magnesium alloy substrate, pure zine plate in analogue body
In liquid（SBF）Corrosion polarization curve.
Embodiment
The specific embodiment of the invention is described in detail below in conjunction with specific accompanying drawing.It should be noted that in following embodiments
The combination of the technical characteristic or technical characteristic of description is not construed as isolated, and they can be mutually combined so as to reach
To superior technique effect.In the accompanying drawing of following embodiments, identical label that each accompanying drawing occurs represent identical feature or
Person's part, it can be applied in different embodiments.
Embodiment 1：
The pure spelter coating of cold spraying, is concretely comprised the following steps on AZ31 magnesium alloy substrates：
1st, the use of roughness is 400# sand paper by institute by the machined sample into 50mm × 50mm × 10mm of AZ31 magnesium alloy plates
The roughness of gained after the face polishing that need to be sprayed, polishing direction is unlimited, removes surface oxide layer, is fought each other using absolute ethyl alcohol
Sheet material after mill is cleaned, and is dried up with cold wind；
2nd, the use of granularity is the pure zinc powder of -200 purposes, is slowly fitted into cold spraying dust feeder by funnel；
3rd, it is 300mm/min to set the cold spray apparatus spray gun speed of service and running orbit, spray gun speed, and spraying profile is " S "
Type；
4th, substrate is fixed：Magnesium substrate is fixed on sprayed panel by fixture, is placed under Spray gun for cold spray；
5th, substrate is sprayed：Corresponding spraying parameter is set, is sprayed, pure spelter coating is prepared on AZ31 substrates, is sprayed
It is 300 DEG C, gas pressure 3MPa, spray distance 20mm to apply temperature, and acceleration gas is high pressure nitrogen.
The pure spelter coating prepared by cold spray technique on AZ31 magnesium alloy substrates, the microstructure morphology at its interface is such as
Shown in Fig. 1, pure spelter coating dense uniform, interface cohesion is good, zero defect crackle.It is laggard to preparing pure spelter coating on AZ31 magnesium alloys
Row bond strength is tested, and is as a result 13.6MPa, has certain interfacial bonding strength, and the microhardness of cold spray zinc layers is
40.8HV.Fig. 2 be prepared on AZ31 magnesium substrates after pure spelter coating with pure magnesium plate, the corrosion polarization curve of pure zine plate.With AZ31 phases
Than the corrosion potential of material is suitable with pure zinc after the pure spelter coating of AZ31 magnesium alloy plate cold sprayings, and resistance to corrosion is remarkably reinforced.
Embodiment 2：
The pure spelter coating of cold spraying, is concretely comprised the following steps on AZ91 magnesium alloy substrates：
1st, will for 400# sand paper using roughness by the machined sample into 50mm × 50mm × 10mm of AZ91 magnesium alloy substrates
The roughness of gained after the face polishing of required spraying, polishing direction is unlimited, removes surface oxide layer, uses absolute ethyl alcohol pair
Sheet material after polishing is cleaned, and is dried up with cold wind；
2nd, the use of granularity is the pure zinc powder of -200 purposes, is slowly fitted into cold spraying dust feeder by funnel；
3rd, it is 350mm/min to set the cold spray apparatus spray gun speed of service and running orbit, spray gun speed, and spraying profile is " S "
Type；
4th, substrate is fixed：Magnesium substrate is fixed on sprayed panel by fixture, is placed under Spray gun for cold spray；
5th, substrate is sprayed：Corresponding spraying parameter is set, is sprayed, pure zinc is prepared on AZ91 magnesium alloy substrates and is applied
Layer, spraying temperature are 260 DEG C, gas pressure 2MPa, spray distance 15mm, and acceleration gas is high pressure nitrogen.
Microstructure morphology such as Fig. 3 institutes at interface after pure zinc are prepared on AZ91 magnesium alloy substrates by cold spray technique
Show, pure spelter coating dense uniform, interface cohesion is good, zero defect crackle.To being surveyed after the pure spelter coating of AZ91 magnesium alloy substrate cold sprayings
It is 8.9MPa to measure its interface bond strength, is well combined, and the microhardness value of cold spray zinc layers is 38.8HV.Fig. 4 is AZ91 magnesium-baseds
Prepared on plate after pure spelter coating with pure magnesium plate, the corrosion polarization curve of pure zine plate.Compared with AZ91, AZ91 magnesium alloy plate cold sprayings
The corrosion potential of material is suitable with pure zinc after pure spelter coating, and the resistance to corrosion of coating is remarkably reinforced.
Although having been presented for several embodiments of the present invention herein, it will be appreciated by those of skill in the art that
Without departing from the spirit of the invention, the embodiments herein can be changed.Above-described embodiment be it is exemplary, no
Restriction that should be using the embodiments herein as interest field of the present invention.
Claims (10)
- A kind of 1. method that the pure zinc of Mg alloy surface/Zinc alloy coated is prepared based on cold spray technique, it is characterised in that to magnesium/ Magnesium alloy substrate carries out grinding process, Chemical cleaning；Pure zinc/Zinc alloy powder is sprayed to the depositional plane of the substrate, obtained Pure zinc/Zinc alloy coated.
- 2. the method as described in claim 1, it is characterised in that specifically comprise the following steps：Step 1: processing substrate：Magnesium/magnesium alloy substrate is worked into required size, and grinding process is carried out to depositional plane, is removed The oxide layer of the depositional plane, and carry out Chemical cleaning；Step 2: powder prepares：Pure zinc/Zinc alloy powder is loaded into cold spray apparatus powder feeder；Step 3: substrate is fixed：By substrate installation on the table, it is placed under Spray gun for cold spray；Optional spray gun is not It is dynamic, movable workbench；Or workbench is motionless, one of spray gun movement two ways completes spraying；Step 4: spraying substrate：Corresponding technological parameter is set, sprayed, obtains pure zinc/Zinc alloy coated.
- 3. method as claimed in claim 1 or 2, it is characterised in that the magnesium/magnesium alloy substrate includes pure magnesium series, AS (Mg-Al-Si) it is serial, AE (Mg-Al-RE) series, AM (Mg-Al-Mn) series.
- 4. method as claimed in claim 1 or 2, it is characterised in that the magnesium/magnesium alloy substrate is binary Magnesium Alloys, three First Magnesium Alloys or complex magnesium alloy system；The binary Magnesium Alloys include Mg-Ca, Mg-Zn, Mg-Sr, Mg-Si, Mg-Li, Mg-Mn, Mg-RE；The ternary magnesium alloy system includes Mg-Y-Zn, Mg-Gd-Y-Zn, Mg-Gd-Y-Zr alloy system, Mg-Zn-Ca；The complex magnesium alloy system includes Mg-Zn-Ca-X；Wherein X is Mn, Sn, Sr or RE.
- 5. method as claimed in claim 1 or 2, it is characterised in that the pure zinc/kirsite be pure zinc, binary kirsite system, Ternary kirsite system or polynary kirsite system；The binary kirsite system includes Zn-Mg, Zn-Ca, Zn-Mn, Zn-Sr；The ternary kirsite system includes Zn-Mg-Ca, Zn-Ca-Sr, Zn-Mg-Sr, Zn-Mg-Y；The polynary kirsite system includes Zn-Mg-Ca-X, and wherein X is Mn, Sn, Sr, RE.
- 6. method as claimed in claim 1 or 2, it is characterised in that the magnesium/magnesium alloy substrate, pure zinc/Zinc alloy coated Thickness, determined according to the actually required degradation rate of material corrosion rate in itself and medical device.
- 7. method as claimed in claim 2, it is characterised in that in step 1, described polishing is manual grinding, and roughness is The roughness of gained after the polishing of 400# sand paper；The substrate after polishing is cleaned using absolute ethyl alcohol, and dried up with cold wind.
- 8. method as claimed in claim 2, it is characterised in that in step 2, the pure zinc/Zinc alloy powder granularity be 5 μm- 100μm。
- 9. method as claimed in claim 2, it is characterised in that in step 4, spraying temperature is 50-550 DEG C, gas pressure For 0.5-4MPa, spray gun translational speed is 100-500mm/min, and spray distance 10-30mm, working gas is nitrogen.
- 10. method as claimed in claim 1 or 2, it is characterised in that described when methods described is used for bio-medical material Magnesium/magnesium alloy substrate is using pure magnesium series, Mg-Ca, or Mg-Zn-Ca；Pure zinc/the kirsite is serial using pure zinc, Zn-Mg, Or Zn-Mg-Ca.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108581392A (en) * | 2018-05-18 | 2018-09-28 | 中国兵器科学研究院宁波分院 | A kind of preparation method and application of biological medical degradable magnesium alloy surface thin crystal composite layer |
| CN110607526A (en) * | 2019-09-06 | 2019-12-24 | 中国兵器科学研究院宁波分院 | Method for preparing nickel-based wide-temperature-range self-lubricating coating with nano structure by cold spraying |
| CN115181874A (en) * | 2022-08-04 | 2022-10-14 | 北京科技大学 | Method for generating carbonate protective layer on surface of zinc alloy and application thereof |
| CN115747573A (en) * | 2022-12-08 | 2023-03-07 | 季华实验室 | Cold spray zinc alloy powder, coating and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108581392A (en) * | 2018-05-18 | 2018-09-28 | 中国兵器科学研究院宁波分院 | A kind of preparation method and application of biological medical degradable magnesium alloy surface thin crystal composite layer |
| CN110607526A (en) * | 2019-09-06 | 2019-12-24 | 中国兵器科学研究院宁波分院 | Method for preparing nickel-based wide-temperature-range self-lubricating coating with nano structure by cold spraying |
| CN110607526B (en) * | 2019-09-06 | 2022-07-05 | 中国兵器科学研究院宁波分院 | Method for preparing nickel-based wide-temperature-range self-lubricating coating with nano structure by cold spraying |
| CN115181874A (en) * | 2022-08-04 | 2022-10-14 | 北京科技大学 | Method for generating carbonate protective layer on surface of zinc alloy and application thereof |
| CN115747573A (en) * | 2022-12-08 | 2023-03-07 | 季华实验室 | Cold spray zinc alloy powder, coating and preparation method thereof |
| CN115747573B (en) * | 2022-12-08 | 2024-02-13 | 季华实验室 | Cold spraying zinc alloy powder, coating and preparation method thereof |
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Application publication date: 20180209 |