CN101698116A - Method for preparing biodegradable magnesium or magnesium alloy and tricalcium phosphate composite material - Google Patents
Method for preparing biodegradable magnesium or magnesium alloy and tricalcium phosphate composite material Download PDFInfo
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Abstract
The invention discloses a method for preparing a biodegradable magnesium or magnesium alloy and tricalcium phosphate composite material, which comprises the following steps: (1) preparing a porous tricalcium phosphate blank, which is to prepare a porous tricalcium phosphate blank by using an organic foam impregnation method; and (2) permeating magnesium or a magnesium alloy, which is to permeate magnesium or a magnesium alloy into the porous tricalcium phosphate blank by using a fusant permeation method to preparing the magnesium or magnesium alloy and tricalcium phosphate composite material. The method has the advantages that: the prepared composite material has high degree of communication as well as well-guaranteed osteoinductive performance and biodegradability and can be used as material for hard tissue replacement and bone repair, completely degrade after being transplanted into a body for a certain time period and induce the formation of new bones; the production process is simple and does not need special equipment and production cost is low; and the method is suitable to prepare biodegradable composite materials with different properties.
Description
Technical field
The present invention relates to the preparation method of biodegradable composite, be specifically related to the preparation method of biodegradable magnesium or magnesium alloy and tricalcium phosphate composite material.
Background technology
Magnesium is one of macroelement of needed by human, and everyone the daily requirement amount of being grown up surpasses 350mg; It participates in a series of metabolic processes in the body, comprises the formation of osteocyte, the healing of accelerated bone damage, or the like.Make hard tissue implanting material with magnesium or magnesium alloy, can not consider the toxicity of its trace metal ion pair cell, and the elastic modelling quantity lower (about 45GPa) that closes of magnesium or magnesium; Therefore, utilize magnesium or magnesium to run jointly to send out problems such as stress shielding that inert metal material implants such as rustless steel that metal implant material can solve present wide clinical application, titanium alloy, cochrome exist, harmful element stripping.In addition, magnesium or magnesium close has the advantages that to corrode degraded in physiological environment, behind implant into body, be degraded and absorbed or discharge, take out thereby need not to carry out second operation, for degradable metallic hard tissue substitute material has been showed a tempting prospect along with the self-healing of human body.Yet, studies show that at present the corrosion in human body environment (the about 7.4-7.6 of pH, high chlorine) of available magnesium alloy is too fast, produce excessive hydrogen and high pH value easily in the part, thereby influence the biocompatibility and the mechanical property of material.This shows that the degradation speed of control magnesium alloy is a primary goal of improving the magnesium alloy performance, its method mainly contains alloying, compoundization and surface modification.
Tricalcium phosphate (TCP) composition is similar to osseous tissue, has excellent biological compatibility, easily biodegradation absorbs, has osteoinductive and have no side effect, and is regarded as good bone alternate material.Experiment and clinical practice also show in numerous animal bodies: this material non-toxic, no local irritation, unlikely haemolysis or blood coagulation, not mutagenesis or canceration.But its fatigue strength is low, and fragility is big, and anti-folding and shock resistance far can not satisfy the requirement of high load capacity artificial bone.
To have the magnesium of good biocompatibility or magnesium alloy and tricalcium phosphate and be prepared into composite, can utilize the advantage of the two, and satisfy bone and induce requirement with controllable biodegradable.At present, the someone adopts mixing, compacting, the sintering technology of prior powder metallurgy to prepare magnesium/tricalcium phosphate, magnesium/hydroxylapatite biology degrading composite (Chinese patent, publication number CN101524558A, CN101524559A, CN101347639A).But, the prior powder metallurgy method of employing, when sintering, severe oxidation takes place in pulverous raw material easily, thereby influences the performance of its performance.
Summary of the invention
The preparation method that the purpose of this invention is to provide a kind of biodegradable magnesium or magnesium alloy and tricalcium phosphate composite material, this method can avoid raw material that the highly oxidized phenomenon takes place when sintering easily, can more effectively guarantee the biocompatibility of tricalcium phosphate, bring into play the osteoinductive of tricalcium phosphate better, and technology is simple and easy to do, and production cost is lower.
The preparation method of biodegradable magnesium of the present invention or magnesium alloy and tricalcium phosphate composite material, its step is as follows:
(1) preparation porous tricalcium phosphate base substrate: adopt the foam impregnation legal system to be equipped with the porous tricalcium phosphate base substrate;
A, pretreatment polyurethane sponge earlier with the polyurethane sponge excision forming, are soaked in it percentage by weight again and are in 30%～40% the NaOH solution, soak 2～4h down at 60 ℃, then, clean with clear water, dry standby;
B, preparation polyvinyl alcohol (PVA) solution, with polyvinyl alcohol and deionized water by in 1: 10 ratio of the mass ratio adding dissolution kettle, warming while stirring to 95 ℃, and be incubated to PVA and be dissolved in fully in the deionized water, obtaining concentration is the PVA solution of 0.1g/ml;
C, preparation tricalcium phosphate slurry are that the PVA solution of 0.1g/ml mixes in ceramic pot with tricalcium phosphate powder and concentration, and both ratios are to add 50～70g tricalcium phosphate powder in the PVA solution of every 100ml; Press 1/5th of PVA liquor capacity again and add dehydrated alcohol in ceramic pot, to eliminate foam; Then, add Ceramic Balls and make abrasive body, by Ceramic Balls: the adding of 10: 1 ratio of the mass ratio of tricalcium phosphate powder ball milling 3-8 hour, makes the tricalcium phosphate slurry of mix homogeneously;
D, soaking paste calcining are immersed pretreated polyurethane sponge in the tricalcium phosphate slurry, soak after 24 hours, taking-up also squeezes out unnecessary slurry, carries out dried again, then, be placed in the tube furnace,, make the porous tricalcium phosphate base substrate 1150 ℃ of calcinings 4～6 hours;
E, measure porosity, measure the size of porous tricalcium phosphate base substrate earlier with micrometer, and calculate its volume V, on balance, claim its weight M again with this
1, be calculated as follows out porosity θ at last:
In the formula, V is the porous tricalcium phosphate volume, ρ
1Solid density 3.18g/cm for tricalcium phosphate
3
(2) infiltrate magnesium or magnesium alloy: adopt the melt infiltration method that magnesium or magnesium alloy are penetrated in the porous tricalcium phosphate base substrate, its method is:
A, according to the porosity of porous tricalcium phosphate base substrate with intend the magnesium of infiltration or the densimeter of magnesium alloy is calculated the weight of required magnesium or magnesium alloy, in order to make the composite of high compaction, actually should get excessive 10～20% blocky magnesium or magnesium alloy, therefore, infiltration with magnesium or magnesium alloy weight M2 computing formula is:
M
2＝V×θ×ρ
2×(1.1～1.2) (2)
In the formula, V is the porous tricalcium phosphate volume; θ is a porosity; ρ
2The density under infiltrating temperature for magnesium or magnesium alloy during Practical Calculation, can directly be got the density 1.74g/cm of pure magnesium under the room temperature
3
B, the porous tricalcium phosphate base substrate is placed corundum crucible, and magnesium or magnesium alloy piece are placed on the top of porous tricalcium phosphate base substrate, cover with coverture (composition sees Table 1);
Table 1 test coverture composition (weight %)
C, the corundum crucible that will fill porous tricalcium phosphate base substrate and magnesium or magnesium alloy briquet place the tubular type atmosphere furnace; feed high-purity argon gas (purity 99.999%) protection; be heated to 700～800 ℃; insulation infiltration 1-8 hour fully penetrates in the hole of porous tricalcium phosphate base substrate, then magnesium metal or magnesium alloy; cut off the electricity supply but keep the ventilation; cool to the furnace below 100 ℃, close argon and come out of the stove, promptly make magnesium or magnesium alloy and tricalcium phosphate composite material.
The present invention adopts the melt infiltration method to realize the compound of pure magnesium or magnesium alloy and tricalcium phosphate, promptly by in the interconnected pore of porous tricalcium phosphate, infiltrating magnesium or magnesium alloy, guaranteed magnesium and tricalcium phosphate interconnection separately, the biological degradability and the osteoinductive of material are coordinated better, so the composite prepared of this law more help the replacement of osseous tissue.The present invention is by the percentage composition of magnesium or magnesium alloy and tricalcium phosphate in the porosity control composite of adjusting porous tricalcium phosphate, the purpose that reaches the control material degradation rate and obtain suitable mechanical property.The composite that adopts prepared of the present invention to go out, deleterious interfacial reaction does not take place with tricalcium phosphate in magnesium metal or magnesium alloy, and the interface bond strength between magnesium or magnesium alloy and the tricalcium phosphate is higher.The tricalcium phosphate of the present invention's preparation strengthens magnesium base composite material can satisfy the requirement of medical application fields such as bone tissue engineering scaffold, bone internal fixation securing member to material comprehensive mechanical property and biology performance better, is particularly suitable for the replacement and the reparation of osseous tissue.
Beneficial effect of the present invention: tricalcium phosphate and magnesium (magnesium alloy) all have good degree of communication in the composite that makes, osteoinductive energy and degradation property have good assurance, can be used as the material that sclerous tissues replaces or bone is repaired, implant the back certain hour after, can degrade fully, and induce the formation of new bone; Production technology is fairly simple, does not need special installation, has the low advantage of production cost; Be applicable to magnesium and multiple magnesium alloy in the porous tricalcium phosphate sintered body infiltration with the biological degradable composite material of preparation different performance.
The specific embodiment
Embodiment one: prepare biodegradable magnesium and tricalcium phosphate composite material, its step is as follows:
(1) preparation porous tricalcium phosphate base substrate: adopt the foam impregnation legal system to be equipped with the porous tricalcium phosphate base substrate;
A, pretreatment polyurethane sponge earlier cut into polyurethane sponge the type body of 2cm * 2cm * 1cm, it are soaked in percentage by weight again and are in 35% the NaOH solution, soak 2h down at 60 ℃, then, clean with clear water, dry standby;
B, preparation polyvinyl alcohol (PVA) solution, earlier with polyvinyl alcohol: deionized water adds in the dissolution kettle in 1: 10 ratio of quality, warming while stirring to 95 ℃, and be incubated to polyvinyl alcohol and be dissolved in fully in the deionized water, obtaining concentration is the PVA solution of 0.1g/ml;
C, preparation tricalcium phosphate slurry are that the PVA solution of 0.1g/ml mixes in ceramic pot with tricalcium phosphate powder and concentration, and both ratios are adding 50g tricalcium phosphate powder in the poly-vinyl alcohol solution of 100ml; / 5th (20ml) that press the poly-vinyl alcohol solution volume again add dehydrated alcohol in ceramic pot, to eliminate foam; Then, add Ceramic Balls and make abrasive body, by Ceramic Balls: the adding of 10: 1 ratio of the mass ratio of tricalcium phosphate powder, ball milling 3 hours makes the tricalcium phosphate slurry;
D, soaking paste calcining, pretreated polyurethane sponge is immersed in the tricalcium phosphate slurry, soak after 24 hours, take out and squeeze out unnecessary slurry, carry out dried again, then, be placed in the tube furnace, 1150 ℃ of calcinings 4 hours, make porous tricalcium phosphate base substrate with the three-dimensional pore space structure of connection;
E, measure porosity, measure the size (2cm * 2cm * 1cm), and be 4cm of porous body earlier with micrometer with this volume V that calculates sample
3, on balance, claim to such an extent that the mass M of porous tricalcium phosphate base substrate is 1.78g again, as follows
Calculate porosity θ=86%.
(2) infiltrate magnesium: adopt the melt infiltration method that pure magnesium (purity 〉=99.95%) is penetrated in the porous tricalcium phosphate base substrate, its method is:
A, calculate the quality of required magnesium according to the porosity of porous tricalcium phosphate base substrate and the densimeter of intending the magnesium of infiltration, and in order to make the composite of high compaction, take by weighing excessive 20% block pure magnesium, therefore, the weight M of required pure magnesium is calculated as follows by formula (2):
M＝4cm
3×86％×1.74g/cm
3×1.2≈7.2g
B; the porous tricalcium phosphate base substrate is placed corundum crucible; and the pure MAG block of 7.2g is placed the top of porous tricalcium phosphate base substrate; cover with coverture (composition sees Table 1); place the tubular type atmosphere furnace; feed high-purity argon gas (purity 99.999%) protection; be heated to 700 ℃; insulation infiltration 1 hour; magnesium metal is fully penetrated in the hole of porous tricalcium phosphate base substrate; then, cut off the electricity supply but keep the ventilation, cool to the furnace below 100 ℃; close argon and come out of the stove, obtain relative density (real density/solid density) and be magnesium/tricalcium phosphate composite material of 98.4%.
Place chemical composition and the essentially identical simulated body fluid of human body fluid (composition sees Table 2) immersion after 30 days this magnesium/tricalcium phosphate composite material, detect and find that material surface has the deposition of hydroxyapatite.
Table 2 experiment simulated body fluid proportioning (g/L)
Embodiment two: prepare biodegradable magnesium calcium alloy and tricalcium phosphate composite material, its step is as follows:
(1) preparing porosity by embodiment one same procedure is 86% porous tricalcium phosphate base substrate;
(2) infiltrate the Mg-1.0Ca alloy: adopt the melt infiltration method that Mg-1.0Ca alloy (be that the Ca percentage by weight is about 1.0%, all the other are the alloy of Mg) is penetrated in the porous tricalcium phosphate base substrate, its method is:
A, calculate the quality of required alloy according to the porosity of porous tricalcium phosphate base substrate and the densimeter of intending the Mg-1.0Ca alloy of infiltration, and in order to make the composite of high compaction, should take by weighing excessive 10% Mg-1.0Ca alloy, therefore, the weight M of required Mg-1.0Ca alloy is calculated as follows by formula (2):
M＝4cm
3×86％×1.74g/cm
3×1.1≈6.6g
B; the porous tricalcium phosphate base substrate is placed corundum crucible; and the Mg-1.0Ca alloy 6.6g that weighs up is placed the top of porous tricalcium phosphate base substrate; cover with coverture (composition sees Table 1); place the tubular type atmosphere furnace; feed high-purity argon gas (purity 99.999%) protection; be heated to 730 ℃; insulation infiltration 2 hours; the Mg-1.0Ca alloy is fully penetrated in the hole of porous tricalcium phosphate base substrate; then, cut off the electricity supply but keep the ventilation, cool to the furnace below 100 ℃; close argon and come out of the stove, obtain relative density (real density/solid density) and be Mg-1.0Ca alloy/tricalcium phosphate composite material of 98.5%.
Place chemical composition and the essentially identical simulated body fluid of human body fluid (composition sees Table 2) immersion after 30 days this Mg-1.0Ca alloy/tricalcium phosphate composite material, detect and find that material surface has the deposition of hydroxyapatite.
Embodiment three: prepare biodegradable Mg-Zn-Mn alloy and tricalcium phosphate composite material, its step is as follows:
(1) preparation porous tricalcium phosphate base substrate: adopt the foam impregnation legal system to be equipped with the porous tricalcium phosphate base substrate;
A, pretreatment polyurethane sponge, different with embodiment one is: polyurethane sponge is Φ 50 * 20mm
3The type body, in percentage by weight is 35% NaOH solution, be 3h 60 ℃ of following soak times;
B, press embodiment one same procedure preparation polyvinyl alcohol (PVA) solution;
C, preparation tricalcium phosphate slurry, different with embodiment one is: the mixed proportion of tricalcium phosphate powder and PVA solution is for adding the 70g tricalcium phosphate powder in the PVA of 100ml solution, add the 20ml dehydrated alcohol again, mix, make tricalcium phosphate slurry with better flowability through ball milling;
D, preparation porous tricalcium phosphate base substrate, different with embodiment one is: the porous body sintering schedule is 1150 ℃ of calcinings 5 hours, makes to have the porous tricalcium phosphate base substrate that is communicated with three-dimensional pore space structure;
The porosity of e, mensuration porous tricalcium phosphate base substrate is measured porous body size (Φ 50 * 20mm with micrometer earlier
3), and be about 40cm with this volume V that calculates sample
3, on balance, claim to such an extent that the mass M of sample is 33g again, calculate porosity θ=74% by formula (1).
(2) infiltrate the Mg-6.0Zn-1.0Mn alloy: adopt the melt infiltration method that Mg-6.0Zn-1.0Mn alloy (be that the Zn percentage by weight is about 6.0%, Mn is about 1.0%, and all the other are the alloy of Mg) is penetrated in the porous tricalcium phosphate base substrate, its method is:
A, in order to make the composite of high compaction, should take by weighing excessive 10% Mg-6.0Zn-1.0Mn alloy, therefore, required alloy mass M is calculated as follows by formula (2):
M＝40cm
3×74％×1.74g/cm
3×1.1≈57g
B; the porous tricalcium phosphate base substrate is placed corundum crucible; the Mg-6.0Zn-1.0Mn alloy 57g that weighs up is placed the top of porous tricalcium phosphate base substrate; cover with coverture (composition sees Table 1); place the tubular type atmosphere furnace; feed high-purity argon gas (purity 99.999%) protection; be heated to 730 ℃; insulation infiltration 6 hours; the Mg-6.0Zn-1.0Mn alloy is fully penetrated in the hole of porous tricalcium phosphate base substrate; cut off the electricity supply then but keep the ventilation; cool to the furnace below 100 ℃, close argon and come out of the stove, obtain relative density (real density/solid density) and be Mg-6.0Zn-1.0Mn alloy/tricalcium phosphate composite material of 98.5%.
Place chemical composition and the essentially identical simulated body fluid of human body fluid (composition sees Table 2) immersion after 30 days this Mg-6.0Zn-1.0Mn alloy/tricalcium phosphate composite material, detect and find that material surface has the deposition of hydroxyapatite.
Embodiment four: prepare biodegradable magnesium calcium alloy and tricalcium phosphate composite material, its step is as follows:
(1) preparation porous tricalcium phosphate base substrate: adopt the foam impregnation legal system to be equipped with the porous tricalcium phosphate base substrate;
A, pretreatment polyurethane sponge, different with embodiment one is: polyurethane sponge is the type body of 5cm * 5cm * 2cm, in percentage by weight is 35% NaOH solution, is 4h 60 ℃ of following soak times;
B, press embodiment one same procedure preparation polyvinyl alcohol (PVA) solution;
C, prepare the tricalcium phosphate slurry by embodiment one same procedure;
D, preparation porous tricalcium phosphate base substrate, different with embodiment one is: the porous body sintering schedule is 1150 ℃ of calcinings 6 hours, makes to have the porous tricalcium phosphate base substrate that is communicated with three-dimensional pore space structure;
E, measure the porosity of porous tricalcium phosphate base substrate, measure porous body size (5cm * 5cm * 2cm), and be 50cm with micrometer earlier with this volume V that calculates sample
3, on balance, claim to such an extent that the mass M of sample is 35g again, calculate porosity θ=78% by formula (1).
(2) infiltrate the Mg-1.0Ca alloy: adopt the melt infiltration method that Mg-1.0Ca alloy (be that the Ca percentage by weight is about 1.0%, all the other are the alloy of Mg) is penetrated in the porous tricalcium phosphate base substrate, its method is:
A, calculate the quality of required alloy according to the porosity of porous tricalcium phosphate base substrate and the densimeter of intending the Mg-1.0Ca alloy of infiltration, and in order to make the composite of high compaction, should take by weighing excessive 15% Mg-1.0Ca alloy, therefore, required alloy mass M is calculated as follows by formula (2):
M＝50cm
3×78％×1.74g/cm
3×1.15≈78g
B; the porous tricalcium phosphate base substrate is placed corundum crucible; the Mg-1.0Ca alloy 78g that weighs up is placed the top of porous tricalcium phosphate base substrate; cover with coverture (composition sees Table 1); place the tubular type atmosphere furnace; feed high-purity argon gas (purity 99.999%) protection; be heated to 730 ℃; insulation infiltration 4 hours; the Mg-1.0Ca alloy is fully penetrated in the hole of porous tricalcium phosphate base substrate; then, cut off the electricity supply but keep the ventilation, cool to the furnace below 100 ℃; close argon and come out of the stove, obtain relative density (real density/solid density) and be Mg-1.0Ca alloy/tricalcium phosphate composite material of 96.7%.
Place chemical composition and the essentially identical simulated body fluid of human body fluid (composition sees Table 2) immersion after 30 days this Mg-1.0Ca alloy/tricalcium phosphate composite material, detect and find that material surface has the deposition of hydroxyapatite.
Embodiment five: prepare biodegradable Mg-2.0Zn-1.0Ca alloy and tricalcium phosphate composite material, its step is as follows:
(1) prepares the porous tricalcium phosphate base substrate by embodiment four same procedure;
(2) infiltrate the Mg-2.0Zn-1.0Ca alloy: adopt the melt infiltration method that Mg-2.0Zn-1.0Ca alloy (be that the Zn percentage by weight is about 2.0%, Ca is about 1.0%, and all the other are the alloy of Mg) is penetrated in the porous tricalcium phosphate base substrate, its method is:
A, calculate the quality of required alloy according to the porosity of porous tricalcium phosphate base substrate and the densimeter of intending the Mg-2.0Zn-1.0Ca alloy of infiltration, and in order to make the composite of high compaction, take by weighing excessive 15% block Mg-2.0Zn-1.0Ca alloy, therefore, required alloy mass M is calculated as follows by formula (2):
M＝50cm
3×78％×1.74g/cm
3×1.15≈78g
B; the porous tricalcium phosphate base substrate is placed corundum crucible; the Mg-2.0Zn-1.0Ca alloy 78g that weighs up is placed the top of porous tricalcium phosphate base substrate; cover with coverture (composition sees Table 1); place the tubular type atmosphere furnace; feed high-purity argon gas (purity 99.999%) protection; be heated to 760 ℃; insulation infiltration 8 hours; the Mg-2.0Zn-1.0Ca alloy is fully penetrated in the hole of porous tricalcium phosphate base substrate; then, cut off the electricity supply but keep the ventilation, cool to the furnace below 100 ℃; close argon and come out of the stove, obtain relative density (real density/solid density) and be Mg-2.0Zn-1.0Ca alloy/tricalcium phosphate composite material of 97.8%.
Place chemical composition and the essentially identical simulated body fluid of human body fluid (composition sees Table 2) immersion after 30 days this Mg-2.0Zn-1.0Ca alloy/tricalcium phosphate composite material, detect and find that material surface has the deposition of hydroxyapatite.
Conclusion: the magnesium/tricalcium phosphate composite material of infiltrating method preparation provided by the invention has advantages such as technology is simple, material density is high, good biocompatibility, can induce the deposition of natural bone mineralogical composition hydroxyapatite in the simulation physiological environment.
Claims (3)
1. the preparation method of biodegradable magnesium or magnesium alloy and tricalcium phosphate composite material, its step is as follows:
(1) preparation porous tricalcium phosphate base substrate: adopt the foam impregnation legal system to be equipped with the porous tricalcium phosphate base substrate;
A, pretreatment polyurethane sponge earlier with the polyurethane sponge excision forming, are soaked in it percentage by weight again and are in 30%～40% the NaOH solution, soak 2～4h down at 60 ℃, then, clean with clear water, dry standby;
B, preparation polyvinyl alcohol (PVA) solution, with polyvinyl alcohol and deionized water by in 1: 10 ratio of the mass ratio adding dissolution kettle, warming while stirring to 95 ℃, and be incubated to PVA and be dissolved in fully in the deionized water, obtaining concentration is the PVA solution of 0.1g/ml;
C, preparation tricalcium phosphate slurry are that the PVA solution of 0.1g/ml mixes in ceramic pot with tricalcium phosphate powder and concentration, and both ratios are to add 50～70g tricalcium phosphate powder in the PVA solution of every 100ml; Press 1/5th of PVA liquor capacity again and add dehydrated alcohol in ceramic pot; Then, add Ceramic Balls and make abrasive body, ball milling 3-8 hour, make the tricalcium phosphate slurry of mix homogeneously;
D, soaking paste calcining are immersed pretreated polyurethane sponge in the tricalcium phosphate slurry, soak after 24 hours, taking-up also squeezes out unnecessary slurry, carries out dried again, then, be placed in the tube furnace,, make the porous tricalcium phosphate base substrate 1150 ℃ of calcinings 4～6 hours;
E, measure porosity, measure the size of porous tricalcium phosphate base substrate earlier with micrometer, and calculate its volume V, on balance, claim its weight M again with this
1, be calculated as follows out porosity θ at last:
In the formula, V is the porous tricalcium phosphate volume, ρ
1Solid density 3.18g/cm for tricalcium phosphate
3
(2) infiltrate magnesium or magnesium alloy: adopt the melt infiltration method that magnesium or magnesium alloy are penetrated in the porous tricalcium phosphate base substrate, its method is:
A, according to the porosity of porous tricalcium phosphate base substrate with intend the magnesium of infiltration or the densimeter of magnesium alloy is calculated the weight of required magnesium or magnesium alloy, infiltration is with magnesium or magnesium alloy weight M
2Computing formula is:
M
2＝V×θ×ρ
2×(1.1～1.2) (2)
In the formula, V is the porous tricalcium phosphate volume; θ is a porosity; ρ
2The density under infiltrating temperature for magnesium or magnesium alloy during Practical Calculation, can directly be got the density 1.74g/cm of pure magnesium under the room temperature
3
B, the porous tricalcium phosphate base substrate is placed corundum crucible, and magnesium or magnesium alloy piece are placed on the top of porous tricalcium phosphate base substrate, cover with coverture;
C, the corundum crucible that will fill porous tricalcium phosphate base substrate and magnesium or magnesium alloy briquet place the tubular type atmosphere furnace; the protection of feeding high-purity argon gas; be heated to 700～800 ℃; insulation infiltration 1-8 hour fully penetrates in the hole of porous tricalcium phosphate base substrate, then magnesium metal or magnesium alloy; cut off the electricity supply but keep the ventilation; cool to the furnace below 100 ℃, close argon and come out of the stove, promptly make magnesium or magnesium alloy and tricalcium phosphate composite material.
2. the preparation method of biodegradable magnesium according to claim 1 or magnesium alloy and tricalcium phosphate composite material is characterized in that the Ceramic Balls of adding: the mass ratio of tricalcium phosphate powder is 10: 1 in the step of preparation tricalcium phosphate slurry.
3. the preparation method of biodegradable magnesium according to claim 1 or magnesium alloy and tricalcium phosphate composite material is characterized in that the coverture model of using is RJ-2 in the step of infiltrating magnesium or magnesium alloy, and the percentage by weight of composition is: 45% MgCl
2, 37% KCl, 8% NaCl, 4% CaF
2, 6% BaCl
2
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| CN102634716A (en) * | 2012-04-28 | 2012-08-15 | 中南大学 | Preparation method of magnesium-zinc-tricalcium phosphate composite material by powder hot pressed sintering |
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| CN101524558B (en) * | 2009-03-11 | 2013-02-27 | 重庆大学 | Biodegradable hydroxylapatite-magnesium and calcium metallic matrix composite |
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| CN102560310A (en) * | 2012-02-16 | 2012-07-11 | 常州大学 | Hot dip plating Zn-Al-Si-Mg alloy plating and hot dip plating method thereof |
| CN102560310B (en) * | 2012-02-16 | 2013-12-18 | 常州大学 | Hot dip plating Zn-Al-Si-Mg alloy plating and hot dip plating method thereof |
| CN102634716A (en) * | 2012-04-28 | 2012-08-15 | 中南大学 | Preparation method of magnesium-zinc-tricalcium phosphate composite material by powder hot pressed sintering |
| CN102634716B (en) * | 2012-04-28 | 2013-08-07 | 中南大学 | Preparation method of magnesium-zinc-tricalcium phosphate composite material by powder hot pressed sintering |
| CN103170011A (en) * | 2013-04-10 | 2013-06-26 | 浙江大学 | In situ-coated biological ceramic artificial magnesium bone and preparation method thereof |
| CN104147638A (en) * | 2014-07-18 | 2014-11-19 | 中国科学院金属研究所 | Three-dimensional connective porous artificial bone scaffold as well as preparation method and application thereof |
| CN104147638B (en) * | 2014-07-18 | 2016-05-04 | 中国科学院金属研究所 | A kind of three-dimensional connected porous artificial bone scaffold and its preparation method and application |
| CN108057133A (en) * | 2018-01-24 | 2018-05-22 | 山东建筑大学 | A kind of preparation method of the compound bone material of renewable magnesium-based |
| CN109020701A (en) * | 2018-09-11 | 2018-12-18 | 浙江世佳科技有限公司 | A kind of high-performance bio bacterial manure |
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