CN110343922A - A kind of magnesium tin alloy and its preparation method and application that human body is degradable - Google Patents
A kind of magnesium tin alloy and its preparation method and application that human body is degradable Download PDFInfo
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- CN110343922A CN110343922A CN201910749871.6A CN201910749871A CN110343922A CN 110343922 A CN110343922 A CN 110343922A CN 201910749871 A CN201910749871 A CN 201910749871A CN 110343922 A CN110343922 A CN 110343922A
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- 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
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- 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
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- 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
- A61L31/148—Materials at least partially resorbable by the body
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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- Heart & Thoracic Surgery (AREA)
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Abstract
The invention discloses a kind of magnesium tin alloys and its preparation method and application that human body is degradable; biodegradable magnesium tin alloy is made by using gravity casting method; refining crystal grain by Equal-channel Angular Pressing (ECAE) technique enhances stress corrosion intensity; a protective film is being formed in alloy surface by later period alkali process again, magnesium tin alloy is prepared.The degradation rate of magnesium tin alloy of the present invention in human body is slow, and the product after degradation is harmless, can reduce the discomfort generated to human body.
Description
Technical field
The invention belongs to medical embedded material technical fields, and in particular to a kind of magnesium tin alloy that human body is degradable and its system
Preparation Method and application.
Background technique
Magnesium alloy has the characteristics that light weight, specific strength are high, higher than rigidity, thermal conductivity is good, ELECTROMAGNETIC OBSCURANT ability is strong,
One of the most abundant light metal alloy of reserves on the earth, processing cost is low, be easily recycled, pollute it is low.The purposes of magnesium is very wide
It is general, in terms of being usually used in auto industry, aerospace industry and 3C industry, and application aspect is cured raw, magnesium also has very big dive
Power, because its have and human body bone similar in density and modulus of elasticity, and it is excellent to have bio-compatibility, biodegradability etc.
Point, and its ingredient of degrading can stimulate bone cell activity, be suitably applied on short-term implant, such as bone inner embedded body, bone group
Weaver's engineering support, angiocarpy bracket etc., and may replace the stainless steel, cochrome and titanium alloy of current clinical use, avoid two
Secondary operation is to pain caused by patient.
However, the shortcomings that magnesium alloy, is, and it is poor rich in corrosion resistance in the solution for having chloride environment in blood plasma or body fluid, it drops
It is too fast to solve rate, causes implant surface liberation of hydrogen speed too fast, body abnormality is caused to react.The magnesium alloy of later period research and development has good
Good mechanics and corrosion resistance, but aluminium be to human body it is virose, will cause neurological disease, such as dementia, alzheimer
Disease etc..
Summary of the invention
In view of the problems of the existing technology, it is an object of that present invention to provide a kind of slow, harmless magnesium of degrading
Tin alloy, the alloy are made biodegradable magnesium tin alloy using gravity casting method, pass through Equal-channel Angular Pressing (ECAE)
Technique, which refines crystal grain, enhances stress corrosion intensity, forms a protective film in alloy surface by later period alkali process, effectively reduces
Degradation rate in human body, and the product after degradation is harmless, can reduce the discomfort generated to human body.
The present invention is realized especially by following technical scheme:
A kind of magnesium tin alloy that human body is degradable, the magnesium tin alloy are made of pure magnesium and pure tin, the magnesium and tin
Mass ratio be 17~20:1.
The preparation method of the degradable magnesium tin alloy of above-mentioned human body, comprising the following steps:
1) pure magnesium and pure tin are weighed according to quantity, in SF6Melting is carried out in environment, after 710~750 DEG C keep the temperature 10~15 minutes
It is cast；
2) homogenizing annealing processing is carried out in process of setting in liquid alloy；
3) extruding after obtained sample being placed in the equal channel angular extrusion die channel of preheating；
4) it by specimen surface grinding, polishing through squeezing, is immersed in after continuing 72~80 hours in NaOH or KOH solution and dries
It is dry.
Further, casting grinding tool need to preheat in advance in step (1), and preheating temperature is 180~220 DEG C.
Further, annealing conditions described in step (2) are as follows: kept the temperature at 470~500 DEG C 8~10 hours it is cold with furnace again
But to room temperature.
Further, the preheating temperature of equal channel angular extrusion die described in step (3) is 300~350 DEG C.
Further, extrusion speed described in step (3) is 0.5~2mm/min.
Further, the temperature of NaOH described in step (4) or KOH solution is 75~85 DEG C, and pH value is 9~9.5.
In another aspect of this invention, the magnesium tin alloy is as preparing answering in degradable medical apparatus material
With.
The invention has the benefit that
1) the magnesium tin alloy preparation cost in the present invention is low, and degradation rate is slow, and it is too fast not will lead to liberation of hydrogen, causes human body
It is uncomfortable.
2) tin element in the magnesium tin alloy in the present invention is the element contained in human body, harmless.
3) the magnesium tin alloy in the present invention is after Equal-channel Angular Pressing and alkali process, body pendular ring with higher
Stress corrosion resistant ability in border.
Detailed description of the invention
Fig. 1 is the alloy for preparing in the embodiment of the present invention 4 product component after stress corrosion；
Fig. 2 is the SEM pattern of the alloy prepared in the embodiment of the present invention 3；
Fig. 3 is the SEM pattern of the alloy prepared in the embodiment of the present invention 4；
Fig. 4 is the stress corrosion cracking (SCC) depth curve comparison diagram of alloy of the present invention.
Specific embodiment
Below in conjunction with specific embodiment of the present invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
(1) alloy melting and gravitational casting
In stainless steel crucible, it is put into the pure magnesium and pure tin (purity is all larger than 99.98%) that weight percent is 20:1, is
Alloy oxidation in fusion process is prevented, passes first into SF6 protective gas to completely cut off air, reuses resistance-type heating furnace to alloy
Alloy melting is carried out, keep the temperature 15 minutes at 710 DEG C and is poured into warmed-up 180 DEG C of mold after being sufficiently stirred, with gravity casting
Method is cast, and is cooled to room temperature in air.Ingot casting cutting cuboid is finally subjected to ECAE in case of the later period using sawing machine.
(2) homogeneous makes annealing treatment
Liquid alloy is easy to produce segregation in process of setting causes alloying component to be unevenly distributed.At homogenizing annealing
For reason to improve, Homogenization Treatments condition is to keep the temperature 10 hours at 470 DEG C to cool to room temperature with the furnace again.
(3) ECAE Equal-channel Angular Pressing
BC type is in the equal channel angular extrusion die internal channel path used.It is wrapped up using Furtulon high temperature adhesive tape and squeezes examination
Sample reduces friction.Extrusion die is heated up to 300 DEG C.Extruded sample and formed punch are put into channel and preheated 20 minutes.It utilizes
Universal testing machine is squeezed, extrusion speed 0.5mm/min.The sample squeezed out is ground, and next extruding can be reduced
The resistance of passage.It repeats to squeeze 2 times altogether.
(4) alkali process
The sample that previous step is squeezed, is cut into sheet through diamond cutter, and surface grinding, polishing and after drying are impregnated
Drying is taken out after continuing 80 hours in 75 DEG C of temperature, the NaOH solution that pH value is 9.5.
Embodiment 2
(1) alloy melting and gravitational casting
In stainless steel crucible, it is put into the pure magnesium and pure tin (purity is all larger than 99.98%) that weight percent is 17:1, is
Alloy oxidation in fusion process is prevented, passes first into SF6 protective gas to completely cut off air, reuses resistance-type heating furnace to alloy
Alloy melting is carried out, keep the temperature 10 minutes at 750 DEG C and is poured into warmed-up 220 DEG C of mold after being sufficiently stirred, with gravity casting
Method is cast, and is cooled to room temperature in air.Ingot casting cutting cuboid is finally subjected to ECAE in case of the later period using sawing machine.
(2) homogeneous makes annealing treatment
Liquid alloy is easy to produce segregation in process of setting causes alloying component to be unevenly distributed.At homogenizing annealing
For reason to improve, Homogenization Treatments condition is to keep the temperature 8 hours at 500 DEG C to cool to room temperature with the furnace again.
(3) ECAE Equal-channel Angular Pressing
BC type is in the equal channel angular extrusion die internal channel path used.It is wrapped up using Furtulon high temperature adhesive tape and squeezes examination
Sample reduces friction.Extrusion die is heated up to 350 DEG C.Extruded sample and formed punch are put into channel and preheated 10 minutes.It utilizes
Universal testing machine is squeezed, extrusion speed 1mm/min.The sample squeezed out is ground, and next extruding road can be reduced
Secondary resistance.It repeats to squeeze 3 times altogether.
(4) alkali process
The sample that previous step is squeezed, is cut into sheet through diamond cutter, and surface grinding, polishing and after drying are impregnated
Drying is taken out after continuing 75 hours in 85 DEG C of temperature, the KOH solution that pH value is 9.
Embodiment 3
(1) alloy melting and gravitational casting
In stainless steel crucible, it is put into the pure magnesium and pure tin (purity is all larger than 99.98%) that weight percent is 19:1, is
Alloy oxidation in fusion process is prevented, passes first into SF6 protective gas to completely cut off air, reuses resistance-type heating furnace to alloy
Alloy melting is carried out, keep the temperature 12 minutes at 730 DEG C and is poured into warmed-up 200 DEG C of mold after being sufficiently stirred, with gravity casting
Method is cast, and is cooled to room temperature in air.Ingot casting cutting cuboid is finally subjected to ECAE in case of the later period using sawing machine.
(2) homogeneous makes annealing treatment
Liquid alloy is easy to produce segregation in process of setting causes alloying component to be unevenly distributed.At homogenizing annealing
For reason to improve, Homogenization Treatments condition is to keep the temperature 9 hours at 490 DEG C to cool to room temperature with the furnace again.
(3) ECAE Equal-channel Angular Pressing
BC type is in the equal channel angular extrusion die internal channel path used.It is wrapped up using Furtulon high temperature adhesive tape and squeezes examination
Sample reduces friction.Extrusion die is heated up to 330 DEG C.Extruded sample and formed punch are put into channel and preheated 16 minutes.It utilizes
Universal testing machine is squeezed, extrusion speed 2mm/min.The sample squeezed out is ground, and next extruding road can be reduced
Secondary resistance.It repeats to squeeze 4 times altogether.
(4) alkali process
The sample that previous step is squeezed, is cut into sheet through diamond cutter, and surface grinding, polishing and after drying are impregnated
Drying is taken out after continuing 72 hours in 80 DEG C of temperature, the NaOH solution that pH value is 9.5.
Embodiment 4
(1) alloy melting and gravitational casting
In stainless steel crucible, it is put into the pure magnesium and pure tin (purity is all larger than 99.98%) that weight percent is 19:1, is
Alloy oxidation in fusion process is prevented, passes first into SF6 protective gas to completely cut off air, reuses resistance-type heating furnace to alloy
Alloy melting is carried out, keep the temperature 10 minutes at 720 DEG C and is poured into warmed-up 200 DEG C of mold after being sufficiently stirred, with gravity casting
Method is cast, and is cooled to room temperature in air.Ingot casting cutting cuboid is finally subjected to ECAE in case of the later period using sawing machine.
(2) homogeneous makes annealing treatment
Liquid alloy is easy to produce segregation in process of setting causes alloying component to be unevenly distributed.At homogenizing annealing
For reason to improve, Homogenization Treatments condition is to keep the temperature 8 hours at 480 DEG C to cool to room temperature with the furnace again.
(3) ECAE Equal-channel Angular Pressing
BC type is in the equal channel angular extrusion die internal channel path used.It is wrapped up using Furtulon high temperature adhesive tape and squeezes examination
Sample reduces friction.Extrusion die is heated up to 300 DEG C.Extruded sample and formed punch are put into channel and preheated 10 minutes.It utilizes
Universal testing machine is squeezed, extrusion speed 2mm/min.The sample squeezed out is ground, and next extruding road can be reduced
Secondary resistance.It repeats to squeeze 5 times altogether.
(4) alkali process
The sample that previous step is squeezed, is cut into sheet through diamond cutter, and surface grinding, polishing and after drying are impregnated
Drying is taken out after continuing 72 hours in 80 DEG C of temperature, the NaOH solution that pH value is 9.5.
The analysis experiment of embodiment 5
Constituent analysis is carried out to product after the alloy corrosion in example IV using XRD-6000 type diffractometer, is using target
Cu, sweep speed are 5 °/s, and the angular range of measurement is 20 °~80 °, are compared using 5.0 software of Jade.Referring to Fig.1 may be used
See, it is harmless to generate product.
Three point bending test is carried out according to ASTM G39 standard, the bending stress of application is 100~120MPa, the power of application
Excessive not have to corrosion and crack, the power of application is too small to be difficult to observe corrosive effect in a short time.Na in simulated body fluid+、K+、
Mg2+、Ca2+、Cl-、HCO3 -、HPO4 2-、SO4 2-Ion concentration be respectively 142.0mM/L, 5.0mM/L, 1.5mM/L, 2.5mM/
L, 147.8mM/L, 4.2mM/L, 1.0mM/L, 0.5mM/L, pH 7.40, temperature are 37 DEG C.Electricity is scanned using JSM 6700F type
Sample section pattern after sem observation corrosion.
Referring to the scanning electron microscope shape appearance figure of Fig. 2 and Fig. 3, it is seen that after corrosion in 48 hours, three corrosion cracking of embodiment is larger,
Example IV is almost without corrosion cracking.
It is each alloy stress corrosion cracking depth referring to Fig. 4, it is seen that Equal-channel Angular Pressing and alkali process are conducive to subtract
Small corrosion rate.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understand without departing from the principles and spirit of the present invention can to these examples carry out it is a variety of variation, modification, replacement and
Modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of magnesium tin alloy that human body is degradable, which is characterized in that the magnesium tin alloy is made of pure magnesium and pure tin, described
Magnesium and tin mass ratio be 17~20:1.
2. the preparation method of degradable magnesium tin alloy described in claim 1, which comprises the following steps:
1) pure magnesium and pure tin are weighed according to quantity, in SF6Melting is carried out in environment, is carried out after keeping the temperature 10~15 minutes at 710~750 DEG C
Casting；
2) homogenizing annealing processing is carried out in process of setting in liquid alloy；
3) extruding after obtained sample being placed in the equal channel angular extrusion die channel of preheating；
4) it by specimen surface grinding, polishing through squeezing, is immersed in after continuing 72~80 hours in NaOH or KOH solution and dries.
3. preparation method according to claim 2, which is characterized in that casting grinding tool need to preheat in advance in step (1), preheat
Temperature is 180~220 DEG C.
4. preparation method according to claim 2, which is characterized in that annealing conditions described in step (2) are as follows: 470~
8~10 hours, which are kept the temperature, at 500 DEG C cools to room temperature with the furnace again.
5. preparation method according to claim 2, which is characterized in that Equal-channel Angular Pressing mould described in step (3)
The preheating temperature of tool is 300~350 DEG C.
6. preparation method according to claim 2, which is characterized in that extrusion speed described in step (3) be 0.5~
2mm/min。
7. preparation method according to claim 2, which is characterized in that the temperature of NaOH described in step (4) or KOH solution
Degree is 75~85 DEG C, and pH value is 9~9.5.
8. magnesium tin alloy described in claim 1 is as the application prepared in degradable medical apparatus material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910749871.6A CN110343922A (en) | 2019-08-14 | 2019-08-14 | A kind of magnesium tin alloy and its preparation method and application that human body is degradable |
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| CN201910749871.6A CN110343922A (en) | 2019-08-14 | 2019-08-14 | A kind of magnesium tin alloy and its preparation method and application that human body is degradable |
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Application publication date: 20191018 |