CN102973342A - Preparation method of degradable magnesium alloy interventional stent - Google Patents
Preparation method of degradable magnesium alloy interventional stent Download PDFInfo
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- CN102973342A CN102973342A CN2012105437044A CN201210543704A CN102973342A CN 102973342 A CN102973342 A CN 102973342A CN 2012105437044 A CN2012105437044 A CN 2012105437044A CN 201210543704 A CN201210543704 A CN 201210543704A CN 102973342 A CN102973342 A CN 102973342A
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Abstract
The invention discloses a preparation method of a degradable magnesium alloy interventional stent, and the method comprises the following steps of A, selecting a magnesium alloy capillary tube; B, forming through a laser engraving way; C, removing slag; D, primary sand blasting, and vacuum drying after the ultrasonic washing for 3min to 10min in weak-acid washing agent after the sand blasting treatment; E, heat treatment: the heat treatment is carried by adopting a vacuum furnace or a heat treatment furnace under the argon protection, the heat treatment time is 5min to 20min, and the heat treatment temperature is 200DEG C to 400DEG C; F, secondary sand blasting and vacuum drying after the ultrasonic washing of 3min to 10min in weak-acid washing agent after the secondary sand blasting treatment; and G, electrolysis polishing. The method is simple in steps, reasonable in design, convenient to realize, good in application effect and capable of effectively preventing the oxidation of the stent in the machining process; and moreover, the prepared interventional stent is high in dimensional precision, high in surface smoothness and excellent in mechanical property.
Description
Technical field
The present invention relates to the human organ interventional therapys such as a kind of blood vessel, the bile duct preparation method of intervention support, especially relate to a kind of preparation method of degradable magnesium alloy intervention support.
Background technology
The blood vessel intervention support is applied to the treatment of the undesirable or damaged blood vessels of percutaneous transluminal angioplasty effect at first, and repairs the compound damage that bypass is put up a bridge and caused.Compare with simple PTCA, the acute occlusion that causes behind the intravascular stent implant into body and the incidence rate of restenosis obviously reduce.Because support contacts with blood for a long time, the blood compatibility of material and the quality of biomechanical property will directly affect clinical application effect.
At present, be applied to the clinical support overwhelming majority and be made of metal, comprised 316L rustless steel, titanium alloy, cobalt-base alloys, tantalum-base alloy, magnesium alloy etc.The most mechanical property of metallic stent material is better, but As time goes on, metal material is aging, corrosion gradually, discharges metal ion in body fluid, may produce harmful effect to body.In addition, support is subject to the effect of body internal stress in vivo for a long time, after using in the long period, fatigue fracture may occur.Thereby current research and development trend are the degradable intervention supports of research.
Low and the specific strength of the density of magnesium alloy, specific stiffness are high, particularly have good biocompatibility, elastic modelling quantity low, can progressively degrade and by the effective characteristics such as absorption of human body in vivo, in recent years, increasing magnesium alloy materials is used to exploitation and the application of Srgery grafting apparatus (such as blade plate, bone screw etc.) and internal medicine intervention apparatus (such as products such as endovascular stents).Generally contain magnesium more than 90% as the magnesium alloy of intravascular stent, mechanical property is suitable with the 316L rustless steel, be unique a kind of biodegradation absorption metallic stent material of doing, can be absorbed in about about two months behind its implant into body that the Mg ion pair human body that discharges has no side effect.
Owing to can be absorbed by blood dissolves, magnesium alloy bracket can carry out repeatedly interventional therapy at same vascular lesion position, and not having the overlapping problem of bringing of support, this has positive effect to improving the lesion vessels compliance, can adopt noninvasive test to follow up a case by regular visits to after the more important thing is Stent.2004, the magnesium alloy coronary artery bracket was used for first human clinical's experiment and has obtained success.Recently, have again a kind of new magnesium alloy biodegradable stent to be developed, its composition is Mg-3A1-1Re, studies show that it is safely and effectively.
As a kind of absorbable metal support, magnesium alloy bracket has the potentiality as New-support, and catabolite is nontoxic, is an important directions of metal rack development.But magnesium alloy plasticity at room temperature is very poor, in the processing preparation process oxidation occurs very easily, so dark, the polish of the high-end product of magnesium alloy have become the restriction magnesium alloy at the bottleneck of the high-tech areas such as biomedical engineering application with development.
Early stage intravascular stent partly forms with the B alloy wire braiding, and particularly the support of TiNi B alloy wire making all is woven into mostly.Afterwards; support precision and the mechanical property of clinical discovery braiding are relatively poor; the processed finished products rate is low, so developed the laser-engraving technique of tubing, adopts the structure of thin footpath thin-wall Mg alloy tubing laser engraving support more stable; not yielding; radial support power is stronger, and working (machining) efficiency is higher, and can effectively control with gas protection the oxidation of surface of the work in the course of processing; the figure of processing changes easily, and then can reduce the cost of manufacture of support.Magnesium alloy is very active, and the surface is atmospheric oxidn easily, and the easy corrosion dissolving of most polar solvents such as water, for the post processing of magnesium alloy bracket has brought very large difficulty.Therefore, be necessary to develop processing and the post-processing technology of biodegradable magnesium alloy intravascular stent.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned deficiency of the prior art, a kind of preparation method of degradable magnesium alloy intervention support is provided, its method step is simple, reasonable in design, realization is convenient and result of use is good, can effectively avoid support that oxidation occurs in the course of processing, and the dimensional accuracy of prepared intervention support is high, surface smoothness is high and good mechanical performance.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of degradable magnesium alloy intervention support is characterized in that the method may further comprise the steps:
Step 1, magnesium alloy capillary tube are selected: selected magnesium alloy capillary tube is external diameter Φ 1.5mm～Φ 19mm, wall thickness 0.2mm～1mm, the magnesium alloy seamless pipe of length 20mm～100mm and linearity≤1mm/m; The material of described magnesium alloy seamless pipe is can biodegradable medical magnesium alloy material;
Step 2, laser engraving molding: the intervention support pattern that will design in advance first also drawn required engraving molding imports laser engraving machine; Afterwards, under inert gas shielding, adopt described laser engraving machine that selected described magnesium alloy capillary tube in the step 1 is carried out the precision engraving, and make the intervention support through the molding of precision engraving;
The laser output power of described laser engraving machine is 20W～50W, and laser output frequency is 1500Hz～9000Hz, and the pulsewidth of institute's Output of laser is 0.1ms～0.5ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the described magnesium alloy distance that is etched between the surface capillaceous is 2mm～3mm, and cutting speed is 70mm/min～150mm/min;
Step 3, the processing of removing slag: with described in the step 2 through the intervention support of precision engraving molding, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry;
Step 4, a blasting treatment, its processing procedure is as follows:
Step 401, blasting treatment: adopt sandblasting machine that the intervention support that removes slag in the step 3 after processing is carried out blasting treatment, the sand grains that adopts during blasting treatment is formed by bead and the mixing of white corundum pearl, and the percentage by volume of bead is 10%～30% in the described sand grains; The granularity of described bead and white corundum pearl is-180 orders;
Step 402, ultrasonic cleaning: with the intervention support after the blasting treatment in the step 401, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry;
Step 5, heat treatment: adopt vacuum drying oven or adopt heat-treatment furnace under argon shield, the intervention support behind the vacuum drying in the step 402 is heat-treated, heat treatment time is 5min～20min, and heat treatment temperature is 200 ℃～400 ℃;
Step 6, secondary blasting treatment, its processing procedure is as follows:
Step 601, blasting treatment: the intervention support after adopting sandblasting machine to heat treatment in the step 5 carries out blasting treatment, the sand grains that adopts during blasting treatment is formed by bead and the mixing of white corundum pearl, and the percentage by volume of bead is 10%～30% in the described sand grains; The granularity of described bead and white corundum pearl is-180 orders;
Step 602, ultrasonic cleaning: with the intervention support after the blasting treatment in the step 601, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry;
Step 7, electrobrightening are processed, and its processing procedure is as follows:
Step 701, electrobrightening are processed:, carry out electrobrightening take aluminium bar as negative electrode and process as anode with the intervention support behind the vacuum drying in the step 602; And when carrying out the electrobrightening processing, electrolysis temperature is-25 ℃～20 ℃, and decomposition voltage is that voltage is 8V～15V DC voltage, and electrolysis time is 30s～2min; The electrolyte that adopts is uniformly mixed to form by phosphoric acid and organic solvent, and the volume ratio of phosphoric acid is 10%～20% in the described electrolyte;
Step 702, ultrasonic cleaning: with the intervention support after the electrobrightening processing in the step 701, it is dry to put into dehydrated alcohol ultrasonic cleaning 3min～10min final vacuum.
The preparation method of above-mentioned a kind of degradable magnesium alloy intervention support is characterized in that: the material of medical magnesium alloy described in the step 1 is AZ31 magnesium alloy or WE43 magnesium alloy.
The preparation method of above-mentioned a kind of degradable magnesium alloy intervention support is characterized in that: the noble gas described in the step 2 is argon or nitrogen.
The preparation method of above-mentioned a kind of degradable magnesium alloy intervention support, it is characterized in that: being weakly acidic abluent described in step 3, step 402 and the step 602, is that ((ratio of 70～75) ︰ (10～20) evenly mixes 20～10) ︰ by nitric acid, dehydrated alcohol and water according to volume ratio.
The preparation method of above-mentioned a kind of degradable magnesium alloy intervention support is characterized in that: the granularity of bead described in step 401 and the step 601 and white corundum pearl is-180 orders～+ 250 orders.
The preparation method of above-mentioned a kind of degradable magnesium alloy intervention support is characterized in that: organic solvent described in the step 701 is methanol and/or ethanol.
The preparation method of above-mentioned a kind of degradable magnesium alloy intervention support is characterized in that: organic solvent described in the step 701 is preferably the mixed solvent that is evenly mixed by methanol and ethanol, and the percent by volume of methanol is 50%～80% in the described electrolyte.
The preparation method of above-mentioned a kind of degradable magnesium alloy intervention support, it is characterized in that: when carrying out blasting treatment in the step 401, the sandblast distance is 25cm～30cm, and the sandblast angle is 30 °～45 °, blasting pressure is 0.4MPa ± 0.02Mpa, and the sandblast time is 40s～55s; When carrying out blasting treatment in the step 601, the sandblast distance is 35cm～40cm, and the sandblast angle is 30 °～45 °, and blasting pressure is 0.4MPa ± 0.02Mpa, and the sandblast time is 20s～35s.
The preparation method of above-mentioned a kind of degradable magnesium alloy intervention support is characterized in that: when carrying out blasting treatment in the step 401, blasting pressure is preferably 0.4MPa, and the sandblast time is preferably 50s; When carrying out blasting treatment in the step 601, blasting pressure is preferably 0.4MPa, and the sandblast time is preferably 30s.
The present invention compared with prior art has the following advantages:
1, the preparation method step is simple, realization is convenient and machining accuracy is high, can obtain the high magnesium alloy intervention support of dimensional accuracy.
2, the required processing pattern for preparing endovascular stent is convenient to global design, control is accurate among the easy change of designed pattern and the preparation technology, precision is high, and selected raw material is thin footpath good biocompatibility and biodegradable thin-wall Mg alloy seamless metal tubing.
3, preparation method is reasonable in design, and its preparation process mainly may further comprise the steps: one, the magnesium alloy capillary tubes is selected; Two, under the inert gas shielding, by laser engraving machine magnesium alloy pipe is carried out the precision engraving; Three, in mixed solution, carry out ultrasonic cleaning, remove residue, not only easy to clean and remove slag effective; Four, machined burrs and oxide skin are removed in a blasting treatment; Five, heat treatment: eliminate the stress that magnesium alloy materials inside and the laser engraving course of processing produce; Six, secondary blasting treatment, the surface strength of increase support; Seven, electrobrightening is processed, and removes oxide layer, reduces the rack surface roughness value, improves anticoagulation function, just obtains the degradable intervention support this moment.
4, in the processing preparation, the matrix of intervention support guarantees not oxidized, so that the surperficial aftertreatment technology of intervention support matrix is simple.
5, according to the different size of used thin footpath thin-wall Mg alloy tubing, reasonably select the machined parameters of laser engraving machine, make the endovascular stent surface quality that cuts out better, dimensional accuracy is higher, and mechanical property is better.
6, because magnesium alloy is very active; its surface is easily by atmospheric oxidn; thereby the easy corrosion dissolving of most polar solvents such as itself and water; therefore adopt the organic solvent of weak acid that support is carried out surface treatment; and rationally adjust ratio and the processing time of solution in the solvent according to the different size of laser engraving molding after-poppet, can reach better treatment effect.
7, result of use is good, and prepared intervention support craft precision is high, and the pattern of required processing changes easily and controls accurately, and in the processing preparation, the support matrix also can guarantee not oxidized.Thereby the present invention can avoid support that oxidation occurs in the course of processing, obtains the good degradable magnesium alloy intervention support of dimensional accuracy height, surface strength height and mechanical property.
8, the scope of application is extensive, the subsequent treatment process on intervention support surface after its magnesium alloy laser engraving precise forming capillaceous and the engraving molding, not only can be used for clinical middle treatment angiostenosis and preparation that can biodegradable magnesium alloy blood vessel inner bracket, can be used for equally the preparation that all kinds of blood vessels of human body such as arteria coronaria, intracranial vessel and non-blood vessel are got involved inner support.
In sum, the inventive method step is simple, reasonable in design, realization is convenient and result of use is good, can effectively avoid support that oxidation occurs in the course of processing, and the dimensional accuracy of prepared intervention support is high, surface strength is high and good mechanical performance.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the FB(flow block) of preparation method of the present invention.
The specific embodiment
As shown in Figure 1 a kind of preparation method of degradable magnesium alloy intervention support, may further comprise the steps:
Step 1, magnesium alloy capillary tube are selected: selected magnesium alloy capillary tube is the magnesium alloy seamless pipe of external diameter Φ 1.5mm～Φ 19mm, wall thickness 0.2mm～1mm, length 20mm～100mm and linearity≤1mm/m; The material of described magnesium alloy seamless pipe is can biodegradable medical magnesium alloy material.
Step 2, laser engraving molding: the intervention support pattern that will design in advance first also drawn required engraving molding imports laser engraving machine; Afterwards, under inert gas shielding, adopt described laser engraving machine that selected described magnesium alloy capillary tube in the step 1 is carried out the precision engraving, and make the intervention support through the molding of precision engraving.
The laser output power of described laser engraving machine is 20W～50W, and laser output frequency is 1500Hz～9000Hz, and the pulsewidth of institute's Output of laser is 0.1ms～0.5ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the described magnesium alloy distance that is etched between the surface capillaceous is 2mm～3mm, and cutting speed is 70mm/min～150mm/min.
Described pattern on the intervention support of precision engraving molding is for being in twos the pipe network structure that mirror symmetry figure forms by a plurality of, and the single mesh on the described pipe network structure be circle, ellipse, rhombus or swallow-tail form.
Step 3, the processing of removing slag: with described in the step 2 through the intervention support of precision engraving molding, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry.
Step 4, a blasting treatment, its processing procedure is as follows:
Step 401, blasting treatment: adopt sandblasting machine that the intervention support that removes slag in the step 3 after processing is carried out blasting treatment, the sand grains that adopts during blasting treatment is formed by bead and the mixing of white corundum pearl, and the percentage by volume of bead is 10%～30% in the described sand grains; The granularity of described bead and white corundum pearl is-180 orders.
Step 402, ultrasonic cleaning: with the intervention support after the blasting treatment in the step 401, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry.
Step 5, heat treatment: adopt vacuum drying oven or adopt heat-treatment furnace under argon shield, the intervention support behind the vacuum drying in the step 402 is heat-treated, heat treatment time is 5min～20min, and heat treatment temperature is 200 ℃～400 ℃.
Step 6, secondary blasting treatment, its processing procedure is as follows:
Step 601, blasting treatment: the intervention support after adopting sandblasting machine to heat treatment in the step 5 carries out blasting treatment, the sand grains that adopts during blasting treatment is formed by bead and the mixing of white corundum pearl, and the percentage by volume of bead is 10%～30% in the described sand grains; The granularity of described bead and white corundum pearl is-180 orders.
Step 602, ultrasonic cleaning: with the intervention support after the blasting treatment in the step 601, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry.
Step 7, electrobrightening are processed, and its processing procedure is as follows:
Step 701, electrobrightening are processed:, carry out electrobrightening take aluminium bar as negative electrode and process as anode with the intervention support behind the vacuum drying in the step 602; And when carrying out the electrobrightening processing, electrolysis temperature is-25 ℃～20 ℃, and decomposition voltage is that voltage is 8V～15V DC voltage, and electrolysis time is 30s～2min; The electrolyte that adopts is uniformly mixed to form by phosphoric acid and organic solvent, and the volume ratio of phosphoric acid is 10%～20% in the described electrolyte.
Step 702, ultrasonic cleaning: with the intervention support after the electrobrightening processing in the step 701, it is dry to put into dehydrated alcohol ultrasonic cleaning 3min～10min final vacuum.
In the actual fabrication process, being weakly acidic abluent described in step 3, step 402 and the step 602, is that ((ratio of 70～75) ︰ (10～20) evenly mixes 20～10) ︰ by nitric acid, dehydrated alcohol and water according to volume ratio.During concrete the cleaning, also can adopt the weak acid pickling agent of other type.
When carrying out blasting treatment in the step 401, the sandblast distance is 25cm～30cm, and the sandblast angle is 30 °～45 °, and blasting pressure is 0.4MPa ± 0.02Mpa, and the sandblast time is 40s～55s; When carrying out blasting treatment in the step 601, the sandblast distance is 35cm～40cm, and the sandblast angle is 30 °～45 °, and blasting pressure is 0.4MPa ± 0.02Mpa, and the sandblast time is 20s～35s.
The actual electrobrightening that carries out is when processing, and organic solvent described in the step 701 is methanol and/or ethanol, also can adopt the organic solvent of other type.
Embodiment 1
In the present embodiment, the preparation method of the degradable magnesium alloy intervention support that adopts may further comprise the steps:
Step 1, magnesium alloy capillary tube are selected: selected magnesium alloy capillary tube is the magnesium alloy seamless pipe of external diameter 2mm, wall thickness 0.2mm, length 30mm and linearity 1mm/m; The material of described magnesium alloy seamless pipe is the AZ31 magnesium alloy materials.
Step 2, laser engraving molding: the intervention support pattern that will design in advance first also drawn required engraving molding imports laser engraving machine; Afterwards, under inert gas shielding, adopt described laser engraving machine that selected described magnesium alloy capillary tube in the step 1 is carried out the precision engraving, and make the intervention support through the molding of precision engraving.
In the present embodiment, described noble gas is argon.
The laser output power of described laser engraving machine is 25W, and laser output frequency is 1500Hz, and the pulsewidth of institute's Output of laser is 0.1ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the described magnesium alloy distance that is etched between the surface capillaceous is 2mm, and cutting speed is 70mm/min.
Step 3, the processing of removing slag: with described in the step 2 through the intervention support of precision engraving molding, put into that to be weakly acidic abluent ultrasonic cleaning 3min final vacuum dry.
Step 4, a blasting treatment, its processing procedure is as follows:
Step 401, blasting treatment: adopt sandblasting machine that the intervention support that removes slag in the step 3 after processing is carried out blasting treatment, the sand grains that adopts during blasting treatment is formed by bead and the mixing of white corundum pearl, and the percentage by volume of bead is 10% in the described sand grains; The granularity of described bead and white corundum pearl is-180 orders～+ 250 orders.
Actual when carrying out blasting treatment, the granularity of described bead and white corundum pearl is all crossed 180 mesh sieves and just can.
In this step, when carrying out blasting treatment, the sandblast distance is 25cm, and the sandblast angle is 30 °, and blasting pressure is 0.4MPa, and the sandblast time is 50s.
Step 402, ultrasonic cleaning: with the intervention support after the blasting treatment in the step 401, put into that to be weakly acidic abluent ultrasonic cleaning 3min final vacuum dry.
Step 5, heat treatment: the intervention support after adopting vacuum drying oven to vacuum drying in the step 402 carries out vacuum heat, and heat treatment time is 20min, and heat treatment temperature is 200 ℃.
Step 6, secondary blasting treatment, its processing procedure is as follows:
Step 601, blasting treatment: the intervention support after adopting sandblasting machine to heat treatment in the step 5 carries out blasting treatment, and the sand grains that adopts during blasting treatment is formed by bead and the mixing of white corundum pearl, and the percentage by volume of bead is 10% in the described sand grains; The granularity of described bead and white corundum pearl is-180 orders～+ 250 orders.
In this step, when carrying out blasting treatment, the sandblast distance is 35cm, and the sandblast angle is 30 °, and blasting pressure is 0.4MPa, and the sandblast time is 30s.
Step 602, ultrasonic cleaning: with the intervention support after the blasting treatment in the step 601, put into that to be weakly acidic abluent ultrasonic cleaning 3min final vacuum dry.
Step 7, electrobrightening are processed, and its processing procedure is as follows:
Step 701, electrobrightening are processed:, carry out electrobrightening take aluminium bar as negative electrode and process as anode with the intervention support behind the vacuum drying in the step 602; And when carrying out the electrobrightening processing, electrolysis temperature is-25 ℃, and decomposition voltage is that voltage is the 8V DC voltage, and electrolysis time is 30s.The electrolyte that adopts is uniformly mixed to form by phosphoric acid and organic solvent, and the volume ratio of phosphoric acid is 10% in the described electrolyte.The mixed solvent of described organic solvent for evenly being mixed by methanol and ethanol, and the percent by volume of methanol is 60% in the described electrolyte.
Step 702, ultrasonic cleaning: with the intervention support after the electrobrightening processing in the step 701, it is dry to put into dehydrated alcohol ultrasonic cleaning 3min final vacuum.
In the present embodiment, the weakly acidic abluent that is that adopts in step 3, step 402 and the step 602 is that the ratio of 20 ︰, 70 ︰ 10 evenly mixes by nitric acid, dehydrated alcohol and water according to volume ratio, and the water that wherein adopts is deionized water.
Embodiment 2
In the present embodiment, as different from Example 1: selected magnesium alloy capillary tube is that external diameter Φ 19mm, wall thickness 1mm, length 100mm and linearity are the magnesium alloy seamless pipe of 1mm/m in the step 1; The material of described magnesium alloy seamless pipe is the WE43 magnesium alloy materials; When carrying out laser engraving in the step 2, the laser output power of described laser engraving machine is 50W, and laser output frequency is 9000Hz, and the pulsewidth of institute's Output of laser is 0.5ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the distance that is etched between the surface are 3mm, and cutting speed is 150mm/min; When carrying out blasting treatment in the step 401, the sandblast distance is 30cm, and the sandblast angle is 45 °, and blasting pressure is 0.38MPa, and the sandblast time is 55s; When heat-treating in the step 5, adopt vacuum drying oven or adopt heat-treatment furnace to heat-treat under argon shield, heat treatment time is 20min, and heat treatment temperature is 400 ℃; When carrying out blasting treatment in the step 601, the sandblast distance is 40cm, and the sandblast angle is 45 °, and blasting pressure is 0.38MPa, and the sandblast time is 35s; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 30% in step 401 and the step 601; The weakly acidic abluent that is that adopts in step 3, step 402 and the step 602 is that the ratio of 15 ︰, 75 ︰ 10 evenly mixes by nitric acid, dehydrated alcohol and water according to volume ratio, the water that wherein adopts is deionized water, and the ultrasonic cleaning time is 10min; When carrying out the electrobrightening processing in the step 701, electrolysis temperature is 20 ℃, and decomposition voltage is that voltage is the 15V DC voltage, and electrolysis time is 2min.The volume ratio of the phosphoric acid in the electrolyte that adopts is 15%, the mixed solvent of described organic solvent for evenly being mixed by methanol and ethanol, and the percent by volume of methanol is 50% in the described electrolyte; In the step 702, the ultrasonic cleaning time is 10min.
In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
Embodiment 3
In the present embodiment, as different from Example 1: selected magnesium alloy capillary tube is that external diameter Φ 10mm, wall thickness 0.5mm, length 50mm and linearity are the magnesium alloy seamless pipe of 1mm/m in the step 1; The material of described magnesium alloy seamless pipe is AZ 31 magnesium alloy materials; When carrying out laser engraving in the step 2, carry out under nitrogen protection, and the laser output power of described laser engraving machine is 40W that laser output frequency is 7000Hz, the pulsewidth of institute's Output of laser is 0.4ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the distance that is etched between the surface are 3mm, and cutting speed is 100mm/min; When carrying out blasting treatment in the step 401, the sandblast distance is 28cm, and the sandblast angle is 35 °, and blasting pressure is 0.42MPa, and the sandblast time is 40s; When heat-treating in the step 5, adopt vacuum drying oven or adopt heat-treatment furnace to heat-treat under argon shield, heat treatment time is 10min, and heat treatment temperature is 300 ℃; When carrying out blasting treatment in the step 601, the sandblast distance is 38cm, and the sandblast angle is 35 °, and blasting pressure is 0.42MPa, and the sandblast time is 20s; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 15% in the step 401; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 20% in the step 601; The weakly acidic abluent that is that adopts in step 3, step 402 and the step 602 is that the ratio of 15 ︰, 75 ︰ 10 evenly mixes by nitric acid, dehydrated alcohol and water according to volume ratio, the ultrasonic cleaning time is 6min in step 3 and the step 602, and the ultrasonic cleaning time is 7min in the step 402; When carrying out the electrobrightening processing in the step 701, electrolysis temperature is 0 ℃, and decomposition voltage is that voltage is the 10V DC voltage, and electrolysis time is 30s; The volume ratio of the phosphoric acid in the electrolyte that adopts is 15%, the mixed solvent of described organic solvent for evenly being mixed by methanol and ethanol, and the percent by volume of methanol is 70% in the described electrolyte; In the step 702, the ultrasonic cleaning time is 4min.
In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
Embodiment 4
In the present embodiment, as different from Example 1: selected magnesium alloy capillary tube is that external diameter Φ 10mm, wall thickness 0.4mm, length 30mm and linearity are the magnesium alloy seamless pipe of 1mm/m in the step 1; The material of described magnesium alloy seamless pipe is the WE43 magnesium alloy materials; When carrying out laser engraving in the step 2, carry out under argon shield, and the laser output power of described laser engraving machine is 35W that laser output frequency is 5000Hz, the pulsewidth of institute's Output of laser is 0.3ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the distance that is etched between the surface are 2mm, and cutting speed is 90mm/min; When carrying out blasting treatment in the step 401, the sandblast distance is 26cm, and the sandblast angle is 38 °, and blasting pressure is 0.4MPa, and the sandblast time is 45s; When heat-treating in the step 5, adopt vacuum drying oven or adopt heat-treatment furnace to heat-treat under argon shield, heat treatment time is 20min, and heat treatment temperature is 400 ℃; When carrying out blasting treatment in the step 601, the sandblast distance is 36cm, and the sandblast angle is 38 °, and blasting pressure is 0.4MPa, and the sandblast time is 25s; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 30% in the step 401; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 25% in the step 601; The weakly acidic abluent that is that adopts in step 3, step 402 and the step 602 is that the ratio of 15 ︰, 75 ︰ 10 evenly mixes by nitric acid, dehydrated alcohol and water according to volume ratio, the ultrasonic cleaning time is 5min in step 3 and the step 402, and the ultrasonic cleaning time is 4min in the step 602; When carrying out the electrobrightening processing in the step 701, electrolysis temperature is-20 ℃, and decomposition voltage is that voltage is the 10V DC voltage, and electrolysis time is 30s; The volume ratio of the phosphoric acid in the electrolyte that adopts is 15%, the mixed solvent of described organic solvent for evenly being mixed by methanol and ethanol, and the percent by volume of methanol is 80% in the described electrolyte; In the step 702, the ultrasonic cleaning time is 3min, and the abluent that also can adopt other and magnesium not to react carries out ultrasonic cleaning.
In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
Embodiment 5
In the present embodiment, as different from Example 1: selected magnesium alloy capillary tube is that external diameter Φ 10mm, wall thickness 0.4mm, length 40mm and linearity are the magnesium alloy seamless pipe of 1mm/m in the step 1; The material of described magnesium alloy seamless pipe is AZ 31 magnesium alloy materials; When carrying out laser engraving in the step 2, carry out under nitrogen protection, and the laser output power of described laser engraving machine is 35W that laser output frequency is 6000Hz, the pulsewidth of institute's Output of laser is 0.2ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the distance that is etched between the surface are 2mm, and cutting speed is 100mm/min; When heat-treating in the step 5, adopt vacuum drying oven or adopt heat-treatment furnace to heat-treat under argon shield, heat treatment time is 10min, and heat treatment temperature is 300 ℃; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 20% in the step 401; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 10% in the step 601; The weakly acidic abluent that is that adopts in step 3, step 402 and the step 602 is that the ratio of 10 ︰, 70 ︰ 20 evenly mixes by nitric acid, dehydrated alcohol and water according to volume ratio, the ultrasonic cleaning time is 5min in step 3 and the step 602, and the ultrasonic cleaning time is 4min in the step 402; When carrying out the electrobrightening processing in the step 701, electrolysis temperature is-10 ℃, and decomposition voltage is that voltage is the 10V DC voltage, and electrolysis time is 50s; The volume ratio of the phosphoric acid in the electrolyte that adopts is 13%, the mixed solvent of described organic solvent for evenly being mixed by methanol and ethanol, and the percent by volume of methanol is 80% in the described electrolyte; In the step 702, the ultrasonic cleaning time is 4min, and the abluent that also can adopt other and magnesium not to react carries out ultrasonic cleaning.
In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
Embodiment 6
In the present embodiment, as different from Example 1: selected magnesium alloy capillary tube is that external diameter Φ 12mm, wall thickness 0.6mm, length 60mm and linearity are the magnesium alloy seamless pipe of 1mm/m in the step 1; The material of described magnesium alloy seamless pipe is the AZ31 magnesium alloy materials; When carrying out laser engraving in the step 2, carry out under nitrogen protection, and the laser output power of described laser engraving machine is 20W that laser output frequency is 1700Hz, the pulsewidth of institute's Output of laser is 0.2ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the distance that is etched between the surface are 2.5mm, and cutting speed is 120mm/min; When heat-treating in the step 5, adopt vacuum drying oven or adopt heat-treatment furnace to heat-treat under argon shield, heat treatment time is 5min, and heat treatment temperature is 300 ℃; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 25% in the step 401; During blasting treatment, the percentage by volume of the bead in the sand grains that adopts is 15% in the step 601; The weakly acidic abluent that is that adopts in step 3, step 402 and the step 602 is that the ratio of 12 ︰, 72 ︰ 16 evenly mixes by nitric acid, dehydrated alcohol and water according to volume ratio; When carrying out the electrobrightening processing in the step 701, electrolysis temperature is 10 ℃, and decomposition voltage is that voltage is the 12V DC voltage, and electrolysis time is 90s; The volume ratio of the phosphoric acid in the electrolyte that adopts is 18%, the mixed solvent of described organic solvent for evenly being mixed by methanol and ethanol, and the percent by volume of methanol is 62% in the described electrolyte.
In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
Embodiment 7
In the present embodiment, as different from Example 1: selected magnesium alloy capillary tube is that external diameter Φ 1.5mm, wall thickness 0.3mm, length 20mm and linearity are the magnesium alloy seamless pipe of 1mm/m in the step 1; The material of described magnesium alloy seamless pipe is the AZ31 magnesium alloy materials; When carrying out laser engraving in the step 2, carry out under nitrogen protection, and the laser output power of described laser engraving machine is 22W that laser output frequency is 2000Hz, the pulsewidth of institute's Output of laser is 0.2ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the distance that is etched between the surface are 2.5mm, and cutting speed is 85mm/min; When heat-treating in the step 5, adopt vacuum drying oven or adopt heat-treatment furnace to heat-treat under argon shield, heat treatment time is 15min, and heat treatment temperature is 350 ℃; The weakly acidic abluent that is that adopts in step 3, step 402 and the step 602 is that the ratio of 18 ︰, 75 ︰ 7 evenly mixes by nitric acid, dehydrated alcohol and water according to volume ratio; When carrying out the electrobrightening processing in the step 701, electrolysis temperature is 15 ℃, and decomposition voltage is that voltage is the 10V DC voltage, and electrolysis time is 70s; The volume ratio of the phosphoric acid in the electrolyte that adopts is 20%, the mixed solvent of described organic solvent for evenly being mixed by methanol and ethanol, and the percent by volume of methanol is 75% in the described electrolyte.
In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
Embodiment 8
In the present embodiment, as different from Example 1: selected magnesium alloy capillary tube is that external diameter Φ 16mm, wall thickness 0.8mm, length 85mm and linearity are the magnesium alloy seamless pipe of 1mm/m in the step 1; The material of described magnesium alloy seamless pipe is the AZ31 magnesium alloy materials; When carrying out laser engraving in the step 2, carry out under nitrogen protection, and the laser output power of described laser engraving machine is 45W that laser output frequency is 8000Hz, the pulsewidth of institute's Output of laser is 0.2ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the distance that is etched between the surface are 2.5mm, and cutting speed is 90mm/min; When heat-treating in the step 5, adopt vacuum drying oven or adopt heat-treatment furnace to heat-treat under argon shield, heat treatment time is 10min, and heat treatment temperature is 350 ℃; The weakly acidic abluent that is that adopts in step 3, step 402 and the step 602 is that the ratio of 16 ︰, 72 ︰ 12 evenly mixes by nitric acid, dehydrated alcohol and water according to volume ratio; When carrying out the electrobrightening processing in the step 701, electrolysis temperature is 10 ℃, and decomposition voltage is that voltage is the 12V DC voltage, and electrolysis time is 90s; The volume ratio of the phosphoric acid in the electrolyte that adopts is 18%, and described organic solvent is methanol.
In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
Embodiment 9
In the present embodiment, as different from Example 1: selected magnesium alloy capillary tube is that external diameter Φ 18mm, wall thickness 0.9mm, length 90mm and linearity are the magnesium alloy seamless pipe of 1mm/m in the step 1; The material of described magnesium alloy seamless pipe is the AZ31 magnesium alloy materials; When carrying out laser engraving in the step 2, carry out under nitrogen protection, and the laser output power of described laser engraving machine is 45W that laser output frequency is 3000Hz, the pulsewidth of institute's Output of laser is 0.2ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the distance that is etched between the surface are 2.5mm, and cutting speed is 80mm/min; When heat-treating in the step 5, adopt vacuum drying oven or adopt heat-treatment furnace to heat-treat under argon shield, heat treatment time is 15min, and heat treatment temperature is 250 ℃; When carrying out the electrobrightening processing in the step 701, electrolysis temperature is-5 ℃, and decomposition voltage is that voltage is the 9V DC voltage, and electrolysis time is 40s; The volume ratio of the phosphoric acid in the electrolyte that adopts is 15%, and described organic solvent is ethanol.
In the present embodiment, all the other method steps are all identical with embodiment 1 with technological parameter.
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, every any simple modification, change and equivalent structure of above embodiment being done according to the technology of the present invention essence changes, and all still belongs in the protection domain of technical solution of the present invention.
Claims (9)
1. the preparation method of a degradable magnesium alloy intervention support is characterized in that the method may further comprise the steps:
Step 1, magnesium alloy capillary tube are selected: selected magnesium alloy capillary tube is external diameter Ф 1.5mm～Ф 19mm, wall thickness 0.2mm～1mm, the magnesium alloy seamless pipe of length 20mm～100mm and linearity≤1mm/m; The material of described magnesium alloy seamless pipe is can biodegradable medical magnesium alloy material;
Step 2, laser engraving molding: the intervention support pattern that will design in advance first also drawn required engraving molding imports laser engraving machine; Afterwards, under inert gas shielding, adopt described laser engraving machine that selected described magnesium alloy capillary tube in the step 1 is carried out the precision engraving, and make the intervention support through the molding of precision engraving;
The laser output power of described laser engraving machine is 20W～50W, and laser output frequency is 1500Hz～9000Hz, and the pulsewidth of institute's Output of laser is 0.1ms～0.5ms; And when carrying out laser engraving, the Laser emission mouth of described laser engraving machine and the described magnesium alloy distance that is etched between the surface capillaceous is 2mm～3mm, and cutting speed is 70mm/min～150mm/min;
Step 3, the processing of removing slag: with described in the step 2 through the intervention support of precision engraving molding, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry;
Step 4, a blasting treatment, its processing procedure is as follows:
Step 401, blasting treatment: adopt sandblasting machine that the intervention support that removes slag in the step 3 after processing is carried out blasting treatment, the sand grains that adopts during blasting treatment is formed by bead and the mixing of white corundum pearl, and the percentage by volume of bead is 10%～30% in the described sand grains; The granularity of described bead and white corundum pearl is-180 orders;
Step 402, ultrasonic cleaning: with the intervention support after the blasting treatment in the step 401, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry;
Step 5, heat treatment: adopt vacuum drying oven or adopt heat-treatment furnace under argon shield, the intervention support behind the vacuum drying in the step 402 is heat-treated, heat treatment time is 5min～20min, and heat treatment temperature is 200 ℃～400 ℃;
Step 6, secondary blasting treatment, its processing procedure is as follows:
Step 601, blasting treatment: the intervention support after adopting sandblasting machine to heat treatment in the step 5 carries out blasting treatment, the sand grains that adopts during blasting treatment is formed by bead and the mixing of white corundum pearl, and the percentage by volume of bead is 10%～30% in the described sand grains; The granularity of described bead and white corundum pearl is-180 orders;
Step 602, ultrasonic cleaning: with the intervention support after the blasting treatment in the step 601, put into that to be weakly acidic abluent ultrasonic cleaning 3min～10min final vacuum dry;
Step 7, electrobrightening are processed, and its processing procedure is as follows:
Step 701, electrobrightening are processed:, carry out electrobrightening take aluminium bar as negative electrode and process as anode with the intervention support behind the vacuum drying in the step 602; And when carrying out the electrobrightening processing, electrolysis temperature is-25 ℃～20 ℃, and decomposition voltage is that voltage is 8V～15V DC voltage, and electrolysis time is 30s～2min; The electrolyte that adopts is uniformly mixed to form by phosphoric acid and organic solvent, and the volume ratio of phosphoric acid is 10%～20% in the described electrolyte;
Step 702, ultrasonic cleaning: with the intervention support after the electrobrightening processing in the step 701, it is dry to put into dehydrated alcohol ultrasonic cleaning 3min～10min final vacuum.
2. according to the preparation method of a kind of degradable magnesium alloy intervention support claimed in claim 1, it is characterized in that: the material of medical magnesium alloy described in the step 1 is AZ31 magnesium alloy or WE43 magnesium alloy.
3. according to the preparation method of claim 1 or 2 described a kind of degradable magnesium alloy intervention supports, it is characterized in that: the noble gas described in the step 2 is argon or nitrogen.
4. according to the preparation method of claim 1 or 2 described a kind of degradable magnesium alloy intervention supports, it is characterized in that: being weakly acidic abluent described in step 3, step 402 and the step 602, is that ((ratio of 70～75) ︰ (10～20) evenly mixes 20～10) ︰ by nitric acid, dehydrated alcohol and water according to volume ratio.
5. according to the preparation method of claim 1 or 2 described a kind of degradable magnesium alloy intervention supports, it is characterized in that: the granularity of bead described in step 401 and the step 601 and white corundum pearl is-180 orders～+ 250 orders.
6. according to the preparation method of claim 1 or 2 described a kind of degradable magnesium alloy intervention supports, it is characterized in that: organic solvent described in the step 701 is methanol and/or ethanol.
7. according to the preparation method of a kind of degradable magnesium alloy intervention support claimed in claim 6, it is characterized in that: organic solvent described in the step 701 is preferably the mixed solvent that is evenly mixed by methanol and ethanol, and the percent by volume of methanol is 50%～80% in the described electrolyte.
8. according to the preparation method of claim 1 or 2 described a kind of degradable magnesium alloy intervention supports, it is characterized in that: when carrying out blasting treatment in the step 401, the sandblast distance is 25cm～30cm, the sandblast angle is 30 °～45 °, blasting pressure is 0.4MPa ± 0.02Mpa, and the sandblast time is 40s～55s; When carrying out blasting treatment in the step 601, the sandblast distance is 35cm～40cm, and the sandblast angle is 30 °～45 °, and blasting pressure is 0.4MPa ± 0.02Mpa, and the sandblast time is 20s～35s.
9. according to the preparation method of a kind of degradable magnesium alloy intervention support claimed in claim 8, it is characterized in that: when carrying out blasting treatment in the step 401, blasting pressure is preferably 0.4MPa, and the sandblast time is preferably 50s; When carrying out blasting treatment in the step 601, blasting pressure is preferably 0.4MPa, and the sandblast time is preferably 30s.
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