CN103436874B - A kind of Mg alloy surface submicron antimicrobial silver preparation method of granules - Google Patents
A kind of Mg alloy surface submicron antimicrobial silver preparation method of granules Download PDFInfo
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- CN103436874B CN103436874B CN201310299662.9A CN201310299662A CN103436874B CN 103436874 B CN103436874 B CN 103436874B CN 201310299662 A CN201310299662 A CN 201310299662A CN 103436874 B CN103436874 B CN 103436874B
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Abstract
The invention discloses a kind of Mg alloy surface submicron antimicrobial silver preparation method of granules, comprise deoiling step, water-washing step, preparation submicron antimicrobial silver particle step, water-washing step, alcohol washes step and dry step, the concrete grammar of described preparation submicron antimicrobial silver particle step is: silver ion solution is put into reaction vessel, simultaneously, by the unsettled top being positioned over silver ion solution of magnesium alloy sample after process, be heated to 150 DEG C ~ 300 DEG C and make silver ion solution boils, and after being incubated 15min ~ 90min, sample is taken out.Gas-solid reaction technology in the present invention's gaseous environment, effectively can to control between gas and solid surface concentration of silver ions in interface region, thus control the speed of growth of Mg alloy surface Argent grain, obtain the submicron Argent grain that size is tiny, while keeping magnesium alloy biodegradation character, improve the erosion resistance of magnesium alloy.
Description
Technical field
The present invention relates to a kind of submicron antimicrobial silver preparation method of granules, relate to a kind of Mg alloy surface submicron antimicrobial silver preparation method of granules more specifically, belong to field of metal surface treatment technology.
Background technology
Magnesium alloy is a kind of biodegradable metallic substance, has broad application prospects in the biological implant devices such as hone lamella, nail, intravascular stent.But, because corrosion stability of magnesium alloy is poor, caused producing local inflammation at implantation initial stage Chang Yin by fast erosion with the biological implant devices of magnesium alloy manufacture to react, therefore, the particle again the preparation of magnesium alloy biological devices surface does not change its biodegradation character while with certain antibacterial is significant.At present, improve magnesium alloy erosion resistance and often adopt the method for Mg alloy surface being carried out to modification, but the solidity to corrosion of the conventional modified magnesium alloy of method is still more weak, and modified layer does not have antibacterial, can not adapt to the needs of medical device product.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the shortcoming of prior art, provides one not affect biodegradation character, improves anticorrosive and Mg alloy surface submicron antimicrobial silver preparation method of granules that is anti-microbial property.
In order to solve above technical problem, the invention provides a kind of Mg alloy surface submicron antimicrobial silver preparation method of granules, comprise deoiling step, water-washing step, preparation submicron antimicrobial silver particle step, water-washing step, alcohol is washed step and is dried step, the concrete grammar of described preparation submicron antimicrobial silver particle step is: silver ion solution is put into reaction vessel, simultaneously, by the unsettled top being positioned over silver ion solution of magnesium alloy sample after process, be heated to 150 DEG C ~ 300 DEG C and make silver ion solution boils, and after being incubated 15min ~ 90min, sample is taken out.By controlling the concentration of silver ions in gas-solid interface district, the speed of growth of the Argent grain that effective control silver ion steam and Mg alloy surface magnesium chemical reaction are formed, thus obtain submicron antimicrobial silver particle at Mg alloy surface.
Being further defined to of technical solution of the present invention: the silver nitrate solution of described silver ion solution to be concentration be 5 grams per liter ~ 30 grams per liters.
Further: described magnesium alloy sample is Mg-Nd-Zn-Zr magnesium alloy sample or AZ91D magnesium alloy sample.Mg-Nd-Zn-Zr magnesium alloy and AZ91D magnesium alloy are the magnesium alloy that medical field is conventional, require high to erosion resistance, further, while keeping its biodegradation character, the difficult problem that its corrosion resistance nature is puzzlement those skilled in the art is always increased, unresolved.
Further: described reaction vessel is resistant to elevated temperatures Glass Containers, make temperature of reaction can remain on more than 150 DEG C, and, because the transparency of Glass Containers is high, be convenient to observing response situation.
Further: the method for described heating is for put into baking oven or electric furnace by reaction vessel, and switch on power heating, make heating means simple, and easy control temperature and soaking time accurately.
The invention has the beneficial effects as follows: a kind of Mg alloy surface submicron antimicrobial silver preparation method of granules disclosed by the invention, silver is utilized to be a kind of bactericidal disinfectant material that medical field is conventional, magnesium alloy biological devices surface uniform distributes the submicron Argent grain of certain area density, both the biodegradation character of magnesium alloy biological devices can not have been changed, magnesium alloy biological devices can also be given and at the implantation initial stage, there is certain anti-microbial effect, thus play the effect effectively reducing the local inflammation reaction probability that the implantation initial stage may occur; Meanwhile, the present invention adopts the gas-solid reaction technology in gaseous environment, effectively can to control between gas and solid surface concentration of silver ions in interface region, thus controls the speed of growth of Mg alloy surface Argent grain, obtains the submicron Argent grain that size is tiny; In addition, the present invention changes the concentration of Silver Nitrate in silver nitrate solution, temperature of reaction and time, the growth time of concentration of silver ions and Argent grain in interface region between controllable gas and Mg alloy surface, thus the size of regulation and control Mg alloy surface submicron antimicrobial silver particle and distribution area density.
Accompanying drawing explanation
Fig. 1 is Mg-Nd-Zn-Zr Mg alloy surface submicron Argent grain distribution pattern in embodiment 1;
Fig. 2 is Mg-Nd-Zn-Zr Mg alloy surface submicron Argent grain agglomerated masses pattern in embodiment 2;
Fig. 3 is AZ91D Mg alloy surface Argent grain energy spectrogram in embodiment 5.
Embodiment
embodiment 1
A kind of Mg alloy surface submicron antimicrobial silver preparation method of granules, comprise deoiling step, water-washing step, preparation submicron antimicrobial silver particle step, water-washing step, alcohol washes step and dry step, wherein, deoiling step, water-washing step, water-washing step, alcohol are washed step and are dried step and all adopts conventional method, primary object of the present invention improves preparation submicron antimicrobial silver particle step, therefore, the present embodiment is described in further detail for preparation submicron antimicrobial silver particle step.
First, resistant to elevated temperatures glass reaction container is put into together with the silver nitrate solution that Mg-Nd-Zn-Zr magnesium alloy sample and silver nitrate concentration through oil removing and washing is 20 grams per liters, further, the unsettled top being positioned over silver ion solution of the magnesium alloy sample after process, both do not contact.
Then, this reaction vessel is put into baking oven and to switch on power heating, start timing when temperature reaches 150 DEG C, after 150 DEG C of insulation 30min, sample is taken out, after washing, alcohol dry after washing, obtain the magnesium alloy that there is submicron antimicrobial silver particle on surface.
The scanning electronic microscope used for magnesium alloy prepared by aforesaid method is observed its surface topography and is shown, be uniform-distribution with the white particle of many submicron at specimen surface, as shown in Figure 1, energy spectrum analysis shows, these white particles are Argent grain.
embodiment 2
The operation steps of the present embodiment is as substantially identical in embodiment 1, is specially:
First, resistant to elevated temperatures glass reaction container is put into together with the silver nitrate solution that Mg-Nd-Zn-Zr magnesium alloy sample and silver nitrate concentration through oil removing and washing is 20 grams per liters, further, the unsettled top being positioned over silver ion solution of the magnesium alloy sample after process, both do not contact.
Then, this reaction vessel is put into baking oven and to switch on power heating, start timing when temperature reaches 150 DEG C, after 150 DEG C of insulation 90min, sample is taken out, after washing, alcohol dry after washing, obtain the magnesium alloy that there is submicron antimicrobial silver particle on surface.
The magnesium alloy scanning electronic microscope prepared by aforesaid method is observed its surface topography and is shown, magnesium alloy sample surface is made up of more equally distributed submicron white Argent grain and a small amount of Argent grain agglomerated masses, Argent grain size in Argent grain agglomerated masses is also submicron, as shown in Figure 2.
embodiment 3
The operation steps of the present embodiment is as substantially identical in embodiment 1, is specially:
First, resistant to elevated temperatures glass reaction container is put into together with the silver nitrate solution that Mg-Nd-Zn-Zr magnesium alloy sample and silver nitrate concentration through oil removing and washing is 30 grams per liters, further, the unsettled top being positioned over silver ion solution of the magnesium alloy sample after process, both do not contact.
Then, this reaction vessel is put into baking oven and to switch on power heating, start timing when temperature reaches 200 DEG C, after 200 DEG C of insulation 30min, sample is taken out, after washing, alcohol dry after washing, obtain the magnesium alloy that there is submicron antimicrobial silver particle on surface.
The scanning electronic microscope used for magnesium alloy prepared by aforesaid method is observed its surface topography and is shown, be uniform-distribution with the white particle of many submicron at specimen surface, energy spectrum analysis shows, these white particles are Argent grain.
embodiment 4
The operation steps of the present embodiment is as substantially identical in embodiment 1, is specially:
First, resistant to elevated temperatures glass reaction container is put into together with the silver nitrate solution that Mg-Nd-Zn-Zr magnesium alloy sample and silver nitrate concentration through oil removing and washing is 5 grams per liters, further, the unsettled top being positioned over silver ion solution of the magnesium alloy sample after process, both do not contact.
Then, this reaction vessel is put into baking oven and to switch on power heating, start timing when temperature reaches 300 DEG C, after 300 DEG C of insulation 15min, sample is taken out, after washing, alcohol dry after washing, obtain the magnesium alloy that there is submicron antimicrobial silver particle on surface.
The scanning electronic microscope used for magnesium alloy prepared by aforesaid method is observed its surface topography and is shown, be uniform-distribution with the white particle of many submicron at specimen surface, energy spectrum analysis shows, these white particles are Argent grain.
embodiment 5
The operation steps of the present embodiment is as substantially identical in embodiment 1, is specially:
First, resistant to elevated temperatures glass reaction container is put into together with the silver nitrate solution that AZ91D magnesium alloy sample and silver nitrate concentration through oil removing and washing is 10 grams per liters, further, the unsettled top being positioned over silver ion solution of the magnesium alloy sample after process, both do not contact.
Then, this reaction vessel is put into resistance furnace and to switch on power heating, start timing when temperature reaches 250 DEG C, after 250 DEG C of insulation 20min, sample is taken out, after washing, alcohol dry after washing, obtain the magnesium alloy that there is submicron antimicrobial silver particle on surface.
The scanning electronic microscope used for magnesium alloy prepared by aforesaid method is observed its surface topography and is shown, be uniform-distribution with the white particle of many submicron at specimen surface, energy spectrum analysis shows, these white particles are Argent grain, as shown in Figure 3.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (3)
1. a Mg alloy surface submicron antimicrobial silver preparation method of granules, comprise deoiling step, water-washing step, preparation submicron antimicrobial silver particle step, water-washing step, alcohol washes step and dry step, it is characterized in that, the concrete grammar of described preparation submicron antimicrobial silver particle step is: silver ion solution is put into reaction vessel, the silver nitrate solution of described silver ion solution to be concentration be 5 grams per liter ~ 30 grams per liters; Meanwhile, by the unsettled top being positioned over silver ion solution of magnesium alloy sample after process, reaction vessel is put into baking oven and to switch on power heating; Be heated to 150 DEG C ~ 300 DEG C and make silver ion solution boils, and after being incubated 15min ~ 90min, sample is taken out.
2. a kind of Mg alloy surface submicron antimicrobial silver preparation method of granules according to claim 1, is characterized in that: described magnesium alloy sample is Mg-Nd-Zn-Zr magnesium alloy sample or AZ91D magnesium alloy sample.
3. a kind of Mg alloy surface submicron antimicrobial silver preparation method of granules according to claim 1, is characterized in that: described reaction vessel is resistant to elevated temperatures Glass Containers.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109515A (en) * | 1994-12-30 | 1995-10-04 | 邵天敏 | Method for preparing aluminium and aluminium alloy surface coating |
| CN1793424A (en) * | 2005-12-30 | 2006-06-28 | 东北大学 | Process for silver caating on surface of magnesium and magnesium alloy |
| CN102703886A (en) * | 2012-06-20 | 2012-10-03 | 太原理工大学 | Method for preparing magnesium alloy super-hydrophobic surface |
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- 2013-07-16 CN CN201310299662.9A patent/CN103436874B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109515A (en) * | 1994-12-30 | 1995-10-04 | 邵天敏 | Method for preparing aluminium and aluminium alloy surface coating |
| CN1793424A (en) * | 2005-12-30 | 2006-06-28 | 东北大学 | Process for silver caating on surface of magnesium and magnesium alloy |
| CN102703886A (en) * | 2012-06-20 | 2012-10-03 | 太原理工大学 | Method for preparing magnesium alloy super-hydrophobic surface |
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Effective date of registration: 20180629 Address after: 212000 the north side of north two weft Road, Danyang Development Zone, Zhenjiang, Jiangsu. Patentee after: Jiangsu Kay Cci Capital Ltd Address before: 211167 Hong Jing Road, Jiangning District, Nanjing, Jiangsu Province, No. 1 Co-patentee before: Jiangsu Konsung Medical Equipment Co., Ltd. Patentee before: Nanjing Institute of Technology |
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