CN104073868A - Electrochemical treatment method suitable for magnesium alloy interventional device and auxiliary equipment - Google Patents
Electrochemical treatment method suitable for magnesium alloy interventional device and auxiliary equipment Download PDFInfo
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- CN104073868A CN104073868A CN201410271817.2A CN201410271817A CN104073868A CN 104073868 A CN104073868 A CN 104073868A CN 201410271817 A CN201410271817 A CN 201410271817A CN 104073868 A CN104073868 A CN 104073868A
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Abstract
The invention relates to an electrochemical treatment method suitable for a magnesium alloy interventional device. The electrochemical treatment method comprises surface pretreatment and electrochemical polishing, wherein the pretreatment comprises the sub-steps: ultrasonically cleaning the magnesium alloy interventional device in a pretreatment aqueous solution at the temperature of 40-70 DEG C for 5-30 minutes, and ultrasonically cleaning in absolute ethyl alcohol for 5-20 minutes, wherein 1L of pretreatment aqueous solution comprises the following components: 5-50g of sodium phosphate, 5-40g of sodium hydroxide, 10-100g of sodium silicate and the balance of distilled water. According to the pretreatment aqueous solution, the electrochemical polishing solution has high biocompatibility, the surface treatment effect is good, and the pretreatment aqueous solution is suitable for most of magnesium alloy interventional devices. Moreover, the related auxiliary equipment clamping mode is unique and convenient, the product can be uniformly polished, multiple samples of different types can be simultaneously clamped, and the method is suitable for electrochemical polishing of the meshed, rod-shaped, tubular, plate-shaped and other-shaped magnesium alloy interventional devices.
Description
technical field
The invention belongs to bio-medical material technical field, be specifically related to a kind of electrochemical process for treating and utility appliance that is applicable to magnesium alloy intervention apparatus.
Background technology
Magnesium is one of major element of needed by human, in human body, to occupy the metallic element of the 4th, mainly be distributed in a series of metabolic processes of participation in cell, and the standard equilibrium potential of magnesium is negative (2.37V), very easily corrosion degraded in human body environment, therefore magnesium and magnesium alloy have the inherent advantage of development Biodegradable material, are suitable for preparing degradable embedded material.
In recent years, magnesium alloy materials has been subject to people's special concern, a kind of revolutionary medical metal material of being known as, and the investigator of multiple countries has successively carried out a large amount of bases and research for application and development, has obtained the positive achievement attracting people's attention.At present, magnesium alloy is very rapid as the research and development of medicine equipment, and along " from external in body, from animal to human body ", track gradually deeply substantially in its development.Biotronik company of Germany has developed the Absorbale magnesium alloy intravascular stent product taking WE43 as main component, and relevant clinical trial has been carried out in the worldwide international clinical trial of the Ba Ge base that takes the lead in, carry out the CE of European Union certification, be expected in clinical treatment, obtain in the near future widespread use.
But, if the surface treatment of magnesium alloy intervention apparatus is bad, will have influence on medicine carrying and the implantation of medicine equipment.Especially in the early stage of the magnesium alloy intervention apparatus course of processing, may occur that tubing, sheet material and silk material surface irregularity are smooth, in the laser cutting of tubing, sheet material and the welding process of silk material, there will be burr and product to splash and surface oxidation, these badly influence the surface quality of magnesium alloy intervention apparatus.Therefore necessary post-processed is carried out in magnesium alloy intervention apparatus surface.Be limited to the special shape of magnesium alloy intervention apparatus, mechanical polishing cannot play a role, and electrochemical etching technique and the relevant device of therefore developing a kind of easy, practical magnesium alloy intervention apparatus are very important.
In electrochemical etching, coating and the medicine loading procedure of magnesium alloy intervention apparatus, for ensureing that magnesium alloy intervention apparatus obtains full and uniform surface treatment, how clamping and rotating is the difficult problem that another one need to solve, therefore, develop a kind of simple and easy to do magnesium alloy intervention apparatus electrochemical etching utility appliance also necessary.
Current, relevant discussion about the electropolishing technology of magnesium alloy intervention apparatus is less, the Chen Qing of Faersheng-Peiersi Material Sciene-Technology Co., Ltd., Jiangyin City good fortune, Sha Gui Cheongju disclose a kind of preparation for processing of biodegradable magnesium alloy intravascular stent, but in its polishing fluid, contain harmful material, and carry out under non-normal temperature.The Zhang Xiaobo of Shanghai Communications University, Yuan Guangyin etc. disclose the electrochemical polishing method of degradable magnesium alloy vascular inner rack, the method health environment-friendly, but its polish results is unstable, and complicated operation.Relevant discussion about the electropolishing utility appliance of magnesium alloy intervention apparatus does not almost have, and this equipment has again very large meaning in actual production process.Therefore, in the urgent need to a kind of polishing technology of green high-efficient more and simple and easy to do utility appliance.
Summary of the invention
For overcoming prior art deficiency, the object of the invention is to provide a kind of electrochemical process for treating and utility appliance that is applicable to magnesium alloy intervention apparatus, and the method and operation of equipment are easy, and polishing effect is good.
For achieving the above object, the present invention adopts following technical scheme:
A kind of electrochemical process for treating that is applicable to magnesium alloy intervention apparatus, comprise surface preparation and electropolishing, described pre-treatment is: by magnesium alloy intervention apparatus in pretreated water solution in 40-70 DEG C of ultrasonic cleaning 5-30min, and then be placed in dehydrated alcohol ultrasonic cleaning 5-20min; The solution composition of 1L pretreated water is: sodium phosphate 5-50g, and sodium hydroxide 5-40g, water glass 10-100g, surplus is distilled water.The power of supersonic cleaning machine can be selected 20-60Hz.
Concrete, described magnesium alloy is magnesium zinc system, magnalium system or magnesium Rare Earth magnesium alloy.In the present invention, phosphoric acid is selected the solution (analytical pure) of mass content >=85%.
Described electropolishing is: the magnesium alloy intervention apparatus of surface preparation is clamped and is placed in electrolytic solution, carry out at normal temperatures electropolishing; Cathode material is ring mesh stainless steel electrode, and polishing voltage is 10-20V, and polishing electric current is 0.10-0.20A, and electrode distance is 60-100mm, and polishing time is 1-5min.
Described electrolytic solution is made up of phosphoric acid, citric acid, glycerol and dehydrated alcohol; The component proportions of 1L electrolytic solution is: phosphatase 11 00-500ml, and citric acid 2-8g, glycerol 10-100ml, surplus is dehydrated alcohol.
Be applicable to the utility appliance of above-mentioned magnesium alloy intervention apparatus electrochemical process for treating, this utility appliance comprises transmission mechanism and clamping device, the planet circular system that described transmission mechanism is made up of sun wheel, planetary set and ring gear, planetary set is between sun wheel and ring gear, and motor drives sun wheel rotation.Planetary set rotation and revolution.The diameter of sun wheel is 20-200mm, and sun wheel is with planetary diameter than being 1-20, and sun wheel rotating speed is 5-15 rev/min.Clamping device is connected with the planet pin in transmission mechanism.
Described clamping device comprises pipe connecting and the cylindrical tube that centre is thick, two ends are thin being fixedly connected with pipe connecting; The column construction of similar ellipse, ellipse short shaft radius is 3-10mm, major axis is 15-40mm, clamping internal diameter 0.5-10mm.Mainly be the cancellated intervention apparatus of hollow cylindrical in order to clamping, as intravascular stent etc.
Described clamping device comprises pipe connecting and the inverted U fixture being fixedly connected with pipe connecting, and a side inwall of this inverted U fixture is provided with prominent cone and groove, and the opposite side position corresponding with prominent cone and groove is respectively equipped with trip bolt.It is 5-40mm that inverted U presss from both sides ambilateral spacing.The intervention apparatus of the different structures such as main, screw tabular in order to clamp.
Described clamping device comprises pipe connecting and the arc fixture being fixedly connected with pipe connecting, two semicircles that this arc fixture is partly cut open by stainless steel tube form (diameter 5-20mm, wall thickness 2-5mm), upper end is provided with binding thread and nut, mainly, tubulose isostructural intervention apparatus bar-shaped in order to clamp.
Compared to the prior art, beneficial effect of the present invention:
Adopt the inventive method and equipment, can obtain surface quality good, smooth finish is high, and surface roughness Ra (interferometric method) is about the magnesium alloy intervention apparatus of 0.002-0.008 μ m.The pretreated water solution of selecting in the present invention, electrolytic polishing liquid has good biocompatibility, and surface treatment effect is better, is applicable to most of magnesium alloy intervention apparatus.And the relevant original convenience of utility appliance method of clamping, can ensure the uniform polish of product can clamp multiple different types of samples simultaneously, be applicable to netted, bar-shaped, tubulose, the electrochemical etching of the tabular intervention apparatus that waits different shape.In addition, the inventive method and device operability are strong, and cost is low, easy, effective.Intervention apparatus surface quality after treatment is better and bright.
Brief description of the drawings
Fig. 1 is the structural representation of utility appliance of the present invention;
Fig. 2 is the structural representation of transmission mechanism in Fig. 1;
Fig. 3 is a kind of structural representation of clamping device in utility appliance of the present invention, is the cancellated intervention apparatus of hollow cylindrical in order to clamping;
Fig. 4 is a kind of structural representation of clamping device in utility appliance of the present invention, is the intervention apparatus of tabular or bolt structure in order to clamping;
Fig. 5 is a kind of structural representation of clamping device in utility appliance of the present invention, is the intervention apparatus of bar-shaped or tubular structure in order to clamping.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further, but protection scope of the present invention is not limited to this.
embodiment 1: to the electropolishing of magnesium zinc yttrium neodymium alloy intravascular stent
A kind of electrochemical process for treating that is applicable to magnesium alloy intervention apparatus, comprise surface preparation and electropolishing, described pre-treatment is: by magnesium zinc yttrium neodymium alloy intravascular stent in pretreated water solution in 50 DEG C of ultrasonic cleaning 15min, and then be placed in dehydrated alcohol ultrasonic cleaning 10min; The solution composition of 1L pretreated water is: sodium phosphate 30g, and sodium hydroxide 20g, water glass 80g, surplus is distilled water.The power selection 50Hz of supersonic cleaning machine.Described electropolishing is: the magnesium zinc yttrium neodymium alloy intravascular stent of surface preparation is clamped and is placed in electrolytic solution, carry out at normal temperatures electropolishing; Cathode material is ring mesh stainless steel electrode, and polishing voltage is 15V, and polishing electric current is 0.10A, and electrode distance is 80mm, and polishing time is 3min.Described electrolytic solution is made up of phosphoric acid, citric acid, glycerol and dehydrated alcohol; The component proportions of 1L electrolytic solution is: phosphoric acid 300ml, and citric acid 6g, glycerol 50ml, surplus is dehydrated alcohol.
As shown in Figures 1 to 3, a kind of utility appliance that is applicable to above-mentioned magnesium zinc yttrium neodymium alloy intravascular stent electrochemical process for treating, this utility appliance comprises transmission mechanism 1 and clamping device, the planet circular system that described transmission mechanism is made up of sun wheel 7, planetary set 8 and ring gear 9, planetary set 8 is between sun wheel 7 and ring gear 9, and motor drives sun wheel 7 rotations.Planetary set 8 rotations and revolution.The diameter of sun wheel 7 is 100mm, and sun wheel 7 is 10 with planetary diameter ratio, and the rotating speed of sun wheel 7 is 10 revs/min.Described clamping device comprises the column construction of pipe connecting 2 and the similar ellipse of cylindrical tube 3(that centre is thick, two ends are thin being fixedly connected with pipe connecting 2, and ellipse short shaft radius is 5mm, and major axis is 30mm, clamping internal diameter 5mm).Mainly be the cancellated intravascular stent 4 of hollow cylindrical in order to clamping.The pipe connecting 2 of clamping device is pegged graft with the planetary axle in transmission mechanism 1, and the quantity of clamping device is identical with planetary quantity, the clamping device of pegging graft on each planetary axle.As shown in FIG., this utility appliance can be processed six intravascular stents simultaneously.
While using this utility appliance to carry out electropolishing, first cathode material 6 is put into the electrolyzer 5 that fills electrolytic solution, then assemble transmission mechanism 1 and clamping device, there is the clamping device of intervention apparatus to stretch in electrolyzer 5 clamping, and be positioned at the inside of ring mesh stainless steel cathode, adjust corresponding polishing condition, can start polishing.After polishing finishes, take out rapidly intervention apparatus and be again placed in dehydrated alcohol room temperature ultrasonic cleaning 5min.
Cut open the zinc yttrium neodymium alloy intravascular stent surface roughness Ra 0.0031 μ m after light.
embodiment 2: to the electropolishing of magnesium zinc calcium hone lamella or nail
A kind of electrochemical process for treating that is applicable to magnesium alloy intervention apparatus, comprise surface preparation and electropolishing, described pre-treatment is: by magnesium zinc calcium hone lamella or nail in pretreated water solution in 60 DEG C of ultrasonic cleaning 10min, and then be placed in dehydrated alcohol ultrasonic cleaning 10min; The solution composition of 1L pretreated water is: sodium phosphate 20g, and sodium hydroxide 30g, water glass 60g, surplus is distilled water.The power selection 50Hz of supersonic cleaning machine.Described electropolishing is: the magnesium zinc calcium hone lamella of surface preparation or nail are clamped and be placed in electrolytic solution, carry out at normal temperatures electropolishing; Cathode material is ring mesh stainless steel electrode, and polishing voltage is 10V, and polishing electric current is 0.20A, and electrode distance is 70mm, and polishing time is 5min.Described electrolytic solution is made up of phosphoric acid, citric acid, glycerol and dehydrated alcohol; The component proportions of 1L electrolytic solution is: phosphatase 11 50ml, and citric acid 8g, glycerol 30ml, surplus is dehydrated alcohol.
A utility appliance that is applicable to above-mentioned magnesium zinc calcium hone lamella or nail electrochemical process for treating, this utility appliance comprises transmission mechanism and clamping device, described transmission mechanism can be with reference to embodiment 1.Described clamping device (as shown in Figure 4) comprises pipe connecting 2 and the inverted U fixture 10 being fixedly connected with pipe connecting 2, one side inwall of this inverted U fixture 10 is provided with prominent cone 11 and groove 12, and the opposite side position corresponding with prominent cone 11 and groove 12 is respectively equipped with the first trip bolt 13 and the second trip bolt 14.It is 20mm that inverted U presss from both sides ambilateral spacing.
In the time that intervention apparatus is magnesium zinc calcium hone lamella, hone lamella is vertically placed in inverted U fixture, according to the thickness of hone lamella, suitably adjust and tighten the first trip bolt 13, withstand hone lamella by the tip of prominent cone 11 and the first trip bolt 13, make hone lamella not move and not slide.In the time that intervention apparatus is magnesium zinc calcium nail, by nail horizontal positioned, groove 12 is withstood in one end, and the other end is suitably tightened the second trip bolt 14, makes nail not move and not slide by groove 12 and the second trip bolt 14.
Cut open magnesium zinc calcium hone lamella or nail surface roughness Ra 0.0044 μ m after light.
embodiment 3: to the electropolishing of AZ31 alloy wire
A kind of electrochemical process for treating that is applicable to magnesium alloy intervention apparatus, comprise surface preparation and electropolishing, described pre-treatment is: by AZ31 alloy wire in pretreated water solution in 70 DEG C of ultrasonic cleaning 5min, and then be placed in dehydrated alcohol ultrasonic cleaning 15min; The solution composition of 1L pretreated water is: sodium phosphate 45g, and sodium hydroxide 10g, water glass 30g, surplus is distilled water.The power selection 50Hz of supersonic cleaning machine.Described electropolishing is: the AZ31 alloy wire of surface preparation is clamped and is placed in electrolytic solution, carry out at normal temperatures electropolishing; Cathode material is ring mesh stainless steel electrode, and polishing voltage is 20V, and polishing electric current is 0.10A, and electrode distance is 60mm, and polishing time is 3min.Described electrolytic solution is made up of phosphoric acid, citric acid, glycerol and dehydrated alcohol; The component proportions of 1L electrolytic solution is: phosphatase 24 00ml, and citric acid 3g, glycerol 80ml, surplus is dehydrated alcohol.
A utility appliance that is applicable to above-mentioned AZ31 alloy wire electrochemical process for treating, this utility appliance comprises transmission mechanism 1 and clamping device, described transmission mechanism can be with reference to embodiment 1.Described clamping device (as shown in Figure 5) comprises pipe connecting 2 and the arc fixture being fixedly connected with pipe connecting 2, this arc fixture is two semicircle 16(diameter 10mm that stainless steel tube is partly cut open, wall thickness 3mm), upper end is provided with binding thread and nut 15, mainly, tubulose isostructural intervention apparatus bar-shaped in order to clamp.
AZ31 alloy wire is inserted in arc fixture, then turn binding thread and the nut 15 of upper end, and then clamping device is assembled on transmission mechanism 1.
Cut open the AZ31 alloy wire surface roughness Ra 0.0067 μ m after light.
The above is only part embodiment of the present invention, for those skilled in the art, under the premise without departing from the principles of the invention, can also make some improvement and replacement, and these improvement and replacement also should be considered as protection scope of the present invention.
Claims (8)
1. one kind is applicable to the electrochemical process for treating of magnesium alloy intervention apparatus, comprise surface preparation and electropolishing, it is characterized in that, described pre-treatment is: by magnesium alloy intervention apparatus in pretreated water solution in 40-70 DEG C of ultrasonic cleaning 5-30min, and then be placed in dehydrated alcohol ultrasonic cleaning 5-20min; The solution composition of 1L pretreated water is: sodium phosphate 5-50g, and sodium hydroxide 5-40g, water glass 10-100g, surplus is distilled water.
2. the electrochemical process for treating that is applicable to as claimed in claim 1 magnesium alloy intervention apparatus, is characterized in that, described magnesium alloy is magnesium zinc system, magnalium system or magnesium Rare Earth magnesium alloy.
3. the electrochemical process for treating that is applicable to as claimed in claim 1 magnesium alloy intervention apparatus, is characterized in that, described electropolishing is: the magnesium alloy intervention apparatus of surface preparation is clamped and is placed in electrolytic solution, carry out at normal temperatures electropolishing; Cathode material is ring mesh stainless steel electrode, and polishing voltage is 10-20V, and polishing electric current is 0.10-0.20A, and electrode distance is 60-100mm, and polishing time is 1-5min.
4. the electrochemical process for treating that is applicable to as claimed in claim 3 magnesium alloy intervention apparatus, is characterized in that, described electrolytic solution is made up of phosphoric acid, citric acid, glycerol and dehydrated alcohol; The component proportions of 1L electrolytic solution is: phosphatase 11 00-500ml, and citric acid 2-8g, glycerol 10-100ml, surplus is dehydrated alcohol.
5. be applicable to the utility appliance of the arbitrary described magnesium alloy intervention apparatus electrochemical process for treating of claim 1 to 4, it is characterized in that, this utility appliance comprises transmission mechanism and clamping device, the planet circular system that described transmission mechanism is made up of sun wheel, planetary set and ring gear, planetary set is between sun wheel and ring gear; The diameter of sun wheel is 20-200mm, and sun wheel is 1-20 with planetary diameter ratio.
6. the utility appliance that is applicable to as claimed in claim 5 magnesium alloy intervention apparatus electrochemical process for treating, is characterized in that, described clamping device comprises pipe connecting and the cylindrical tube that centre is thick, two ends are thin being fixedly connected with pipe connecting.
7. be applicable to as claimed in claim 5 the utility appliance of magnesium alloy intervention apparatus electrochemical process for treating, it is characterized in that, described clamping device comprises pipe connecting and the inverted U fixture being fixedly connected with pipe connecting, one side inwall of this inverted U fixture is provided with prominent cone and groove, and the opposite side position corresponding with prominent cone and groove is respectively equipped with trip bolt.
8. be applicable to as claimed in claim 5 the utility appliance of magnesium alloy intervention apparatus electrochemical process for treating, it is characterized in that, described clamping device comprises pipe connecting and the arc fixture being fixedly connected with pipe connecting, two semicircles that this arc fixture is partly cut open by stainless steel tube form, and upper end is provided with binding thread and nut.
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| CN105483814A (en) * | 2016-01-13 | 2016-04-13 | 上海交通大学 | Electrolytic polishing liquid and polishing method for measuring residual stress of rare earth magnesium alloy through layer stripping method |
| CN105603500A (en) * | 2016-01-13 | 2016-05-25 | 上海轻合金精密成型国家工程研究中心有限公司 | Electrolytic polishing agent and electrolytic polishing method for pretreatment of magnesium alloy residual stress test |
| WO2017020832A1 (en) * | 2015-08-04 | 2017-02-09 | 河南通镁新材料科技有限公司 | Electrochemical polishing method for magnesium metal members |
| CN106544714A (en) * | 2016-10-21 | 2017-03-29 | 郑州大学 | A kind of preparation method of medical magnesium alloy surface coating |
| CN107313031A (en) * | 2017-06-28 | 2017-11-03 | 西安理工大学 | A kind of chemical nickel-plating method for surface for improving corrosion stability of magnesium alloy |
| CN111270240A (en) * | 2020-01-20 | 2020-06-12 | 东南大学泰州生物医药与医疗器械研究院 | Two-step polishing method of magnesium alloy intravascular stent and polishing solution thereof |
| CN112458529A (en) * | 2020-11-26 | 2021-03-09 | 贾昱 | Electrochemical polishing equipment for coronary intravascular stent |
| CN113106511A (en) * | 2021-03-20 | 2021-07-13 | 上海太同电镀有限公司 | Plated item belt cleaning device |
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| CN112458529A (en) * | 2020-11-26 | 2021-03-09 | 贾昱 | Electrochemical polishing equipment for coronary intravascular stent |
| CN113106511A (en) * | 2021-03-20 | 2021-07-13 | 上海太同电镀有限公司 | Plated item belt cleaning device |
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